United States
Environmental Protection
Agency
Industrial Environmental Research
Laboratory
Research Triangle Park NC 2771 1
EPA-600/7-79-190
August 1979
Environmental
Assessment: Source Test
and Evaluation Report -
Lurgi (Kosovo) Medium-Btu
Gasification, Phase 1
Interagency
Energy/Environment
R&D Program Report
-------
-------
EPA-600/7-79-190
August 1979
Environmental Assessment: Source Test and
Evaluation Report - Lurgi (Kosovo) Medium-Btu
Gasification, Phase 1
by
K. J. Bombaugh, W. E. Corbett, and M. D. Matson
Radian Corporation
P.O. Box 9948
Austin, Texas 78766
Contract No. 68-02-2608
Task No. 57
Program Element No. EHE623A
EPA Project Officer: William J. Rhodes
Industrial Environmental Research Laboratory
Office of Energy, Minerals, and Industry
Research Triangle Park, NC 27711
Prepared for
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, DC 20460
-------
ABSTRACT
This report summarizes the current status of an on-
going, cooperative, environmental data acquisition program which
is being jointly sponsored by the U.S. Environmental Protection
Agency and the government of Yugoslavia. The subject of this
test program is a commercial-scale, medium-Ecu", Lurgi gasifica-
tion facility which is currently operating in the Kosovo region
of Yugoslavia.
The overall objective of the Kosovo test program is to
characterize potential environmental problems and control tech-
nology needs associated with the gasification of lignite coal in
a state-of-the-art Lurgi gasification plant. This program is
especially timely because it is providing the EPA with an oppor-
tunity to study firsthand, the environmental problems which are
likely to be encountered by future operators of U.S. gasification
facilities.
To date, the Phase I of a multiphase test program has
been completed. Phase I concentrated primarily on the character-
ization of major pollutants in the plant's gaseous emissions.
Some characterization of the plant's liquid and solid waste
streams and its by-products were also performed. A SAM/1A
analysis of the gaseous emissions indicated that the major pollu-
tants of concern are CO, benzene, H2S, mercaptans, and NH3.
Analysis of the Phenosolvan effluent indicated a high concentra-
tion of organics with a relatively low phenol concentration (170-
270 mg/Jl) . The gasifier section effluent was relatively low
in organics and had a nigh pH of 11-12 . Analysis of the by-
product streams indicated that the sulfur concentration of
"lights" (i.e., gasoline) was significantly higher than the
"heavies" (i.e., tar).
The next phase of this test program will emphasize
detailed characterization of trace organics and trace elements
in the plant's multimedia waste streams and evaluation of control
options of streams containing potentially harmful pollutants.
n.
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TABLE OF CONTENTS
Section Page
Abstract ii
Figures v
Tables - vi
Acknowledgements viii
1 .0 INTRODUCTION 1
1.1 SCOPE OF WORK ' 1
1 . 2 PROGRAM ORGANIZATION 2
1 .3 TEST SCHEDULE 4
1.4 REPORT ORGANIZATION 4
2.0 PLANT DESCRIPTION 6
2 .1 PROCESS OVERVIEW 6
2 . 2 FLEISSNER DRYING SECTION U
2 . 3 GASIFICATION SECTION 16
2.4 RECTISOL SECTION 19
2 .5 TAR/OIL SEPARATION SECTION 22
2 . 6 PHENOSOLVAN SECTION 23
2. 7 BY-PRODUCT STORAGE SECTION 26
2 . 8 AUXILIARIES 31
3.0 SAMPLING PROCEDURES 32
3 .1 FLOW MEASUREMENT PROCEDURES 34
3 . 2 PARTICULATES 36
-------
TABLE OF CONTENTS (Continued)
Section Page
3.3 GAS SAMPLING FOR WET CHEMICAL
ANALYSIS 37
3.4 GRAB GAS SAMPLES FOR GAS CHROMA-
TOGRAPHY 38
4.0 ANALYTICAL METHODOLOGY 40
4 .1 ANALYTICAL METHODS FOR GASES 40
4 .2 ANALYTICAL METHODS FOR WASTE WATERS 44
4 . 3 ANALYTICAL METHODS FOR SOLIDS 44
5.0 RESULTS AND RECOMMENDATIONS 45
5 .1 GASEOUS EMISSIONS 43
5.2 LIQUID EFFLUENTS, LIQUID BY-PRODUCTS
AND SOLID WASTES 57
5 . 3 MASS BALANCES 62
5.4 DISCUSSION OF RESULTS AND RECOMMENDA-
TIONS FOR FUTURE TESTING 64
REFERENCES 68
APPENDIX A: PHASE I DATA SUMMARY TABLES
FOR GASES A-1
APPENDIX B: PHASE I DATA SUMMARY TABLES -
LIQUIDS AND SOLIDS B-l
APPENDIX C: MASS BALANCE CALCULATIONS C-l
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FIGURES
Number Page
1-1 KOSOVO TEST PROGRAM PARTICIPATING ORGANIZA-
TIONS AND AREAS OF RESPONSIBILITY 3
2-1 KOSOVO GASIFICATION PLANT AND ITS RELATION-
SHIP TO SURROUNDING INDUSTRIES 7
2-2 OVERALL PLANT FLOW SCHEME - KOSOVO
GASIFICATION PLANT 8
2-3 SIMPLIFIED FLOW SCHEMATIC-KOSOVO
GASIFICATION PLANT 12
2-4 PROCESS FLOW DIAGRAM SHOWING SAMPLING POINTS
IN KOSOVO PLANT FLEISSNER DRYING SECTION 14
2-5 PROCESS FLOW DIAGRAM SHOWING SAMPLING POINTS
IN KOSOVO PLANT GASIFICATION SECTION 17
2-6 PROCESS FLOW DIAGRAM SHOWING SAMPLING POINTS
IN KOSOVO PLANT RECTISOL SECTION 20
2-7 PROCESS FLOW DIAGRAM SHOWING SAMPLING POINTS
IN KOSOVO PLANT TAR/OIL SEPARATION SECTION.... 24
2-8 PROCESS FLOW DIAGRAM SHOWING SAMPLING POINTS
IN KOSOVO PLANT PHENOSOLVAN SECTION 27
2-9 PROCESS FLOW DIAGRAM SHOWING SAMPLING POINTS
IN KOSOVO BY-PRODUCTS STORAGE AREA 29
3-1 TYPICAL SURGE TANK VENT PIPE ARRANGEMENT 35
3-2 FLOW MEASUREMENT APPROACH FOR HIGH
VELOCITY TANK VENTS 35
3-3 FLOW MEASUREMENT APPROACH FOR LOW VELOCITY
TANK VENT FLOWS 36
5-1 KOSOVO LIGNITE DATA GATHERED DURING
CAMPAIGN I 46
v
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TABLES
Number Page
1-1 KOSOVO TEST PROGRAM OBJECTIVES AND
SCHEDULE 5
2-1 KOSOVO PLANT DESIGN DATA (ASSUMES 5 OF 6
GASIFIERS IN SERVICE) 10
2-2 SIGNIFICANT KOSOVO PLANT FLEISSNER DRYING
SECTION PROCESS AND EMISSION STREAMS 15
2-3 SIGNIFICANT KOSOVO PLANT GASIFICATION
PROCESS AND EMISSION STREAMS 18
2-4 SIGNIFICANT KOSOVO PLANT RECTISOL SECTION
PROCESS AND EMISSION STREAMS 21
2-5 SIGNIFICANT KOSOVO PLANT TAR SEPARATION
SECTION PROCESS AND EMISSION STREAMS 25
2-6 SIGNIFICANT KOSOVO PLANT PHENOSOLVAN
SECTION PROCESS AND EMISSION STREAMS 28
2-7 SIGNIFICANT KOSOVO PLANT BY-PRODUCT STORAGE
SECTION PROCESS AND EMISSION STREAMS 30
3-1 SAMPLING PROCEDURES .................. 33
4-1 ANALYTICAL PROCEDURES FOR GASES 41
4-2 ANALYTICAL PROCEDURES FOR WASTE WATERS 42
4-3 ANALYTICAL PROCEDURES FOR SOLIDS 43
5-1 DMEG VALUES FOR GASEOUS SPECIES MEASURED
IN KOSOVO STREAMS 52
5-2 HEALTH-BASED DS, TDS, AND TWOS VALUES FOR
KOSOVO "HIGH PRIORITY" ATMOSPHERIC
EMISSIONS STREAMS ............................ 53
5-3 ECOLOGY-BASED DS VALUES FOR KOSOVO "HIGH
PRIORITY" ATMOSPHERIC EMISSION STREAMS....... 54
5-4 ANALYTICAL DATA FOR KOSOVO "HIGH PRIORITY"
GASEOUS EMISSION STREAMS SAMPLED DURING
PHASE I 55
VI
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TABLES (Continued)
Number Page
5-5 MAJOR SOURCES OF LIQUID EFFLUENTS, LIQUID
BY-PRODUCTS AND SOLID WASTES AT THE
58
5-6
5-7
5-8
5-9
5-10
KOSOVO WASTEWATER PROPERTIES (PHASE I
DATA)
KOSOVO LIQUID BY-PRODUCT DATA
MASS BALANCE ACROSS THE LURGI GASIFIER
AT KOSOVO
SULFUR BALANCE ACROSS LURGI GASIFICATION
FACILITY AT KOSOVO
KOSOVO WASTE STREAMS - GENERAL SUMMARY
OF ADDITIONAL DATA NEEDS
59
61
63
63
65
VI1.
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ACKNOWLEDGEMENTS
The authors wish to express their appreciation to the
following individuals for their timely and very beneficial con-
tributions to the work which is described in this report:
Mira Mitrovic and Dragan Petkovi'c (Rudarski
Institute - Belgrade, Yugoslavia)
Becir Salja, Shani Dulje, Emili Boti (Kosovo
Plant Operations)
Slobodan Kapor (Institute for the use of
Nuclear Energy in Forestry and Agriculture -
INEP)
Radamir Vicic, Branislav Tomasevi'c, Mile
Miloslavljevi/c (Kosovo Institute)
Klaus Schwitzgebel, Gordon Page, Bob Collins,
Chuck Hudak, Bob Magee and Ken Lee (Radian
Corporation)
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1.0 INTRODUCTION
The Kosovo test program was conceived by the EPA in
response to a need for representative data on the potential
environmental impacts of Lurgi gasification technology. Because
a number of U.S. companies have announced plans to construct
medium- and/or high-Btu gasification plants based upon Lurgi
technology and a number of other groups are seriously consid-
ering this possibility, the EPA is interested in taking
appropriate and timely steps to guarantee the environmental
acceptability of those future facilities.
1.1 Scope of Work
The test program at Kosovo involves four phases of
effort. This report summarizes the results of Phase I.
In Phase I, a group of approximately 50 feed, product,
by-product and gaseous, liquid and solid waste•streams were
studied. The test work consisted primarily of measuring the
flow rates of the major emission streams from the plant and
characterizing these streams with respect to their major compo-
nents. This phase of effort also served as a source screening
since essentially all of the streams were found to be sources
of harmful pollutants. They will be studied further in subse-
quent phases.
In general, the Phase I test program focused on the
plant process and waste streams that were expected to be major
sources of environmentally significant emissions. The selection
of streams for examination in Phase I was based upon:
-------
• visual inspection of the plant and its
process and waste streams,
• design flowrates and process schematics,
• the results of previous test work,
• a series of source screening measurements
(Orsat measurements), and
• engineering judgement.
During Phase II, a detailed characterization will be
made of approximately 30 key process and emission streams. The
work will involve gathering data on stream flow characteristics
and concentrations of selected minor and trace components, in-
cluding trace metals and trace organics.
In Phase III, ambient concentrations of selected pollu-
tants will be monitored at several locations'inside and outside
(upwind and downwind) of the plant's boundaries. It is expected
that data gathered during Phase III will define the potential
impact of a Lurgi plant on ambient air and will also validate
emissions data gathered in the other program phases.
Phase IV will concentrate on fugitive emission sources
within the Kosovo facilities and will define the relative signi-
ficance of fugitive emissions on the overall emission character
of the facilities.
1.2 Program Organization
As shown in Figure 1-1, the prime contractor for the
Phase I test work was Rudarski Institute of Belgrade, Yugoslavia
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PROGRAM STRUCTURE FOR PHASE I:
tladian Corporation
(Austin, Texas)
Consultant
Technical Support
Samoling and Analysis
Rudarski Institute
(Selgrade, Yugoslavia)
Prime Contractor
Sampling and Wet Chemical Analysis;
Data Analysis and Reporting
Kosovo Plane
Operating Department
Plant Access
and Operating Data
Kosovo Institute
Subcontractor
Sampling and
Analytical Support
Institute for
Applied Xuclear Technology
(Belgrade, Yugoslavia)
Subcontractor
CC Analysis
PROGRAM STRUCTURE "OR PHASES II-IV:
Radian Corporation
(Austin, Texas)
Prime Contractor
Technical Support
Sampling and Analysis
Rudarski Institute
(Belgrade, Yugoslavia)
Subcontractor
Overseas Coordination;
Sampling and Vet Chemical Analysis
Data Analysis and Reoorting
Kosovo Plant
Operating Department
Plant Access
and Operating Data
Kosovo Institute
Subcontractor
Sampling and
Analytical Support
AA Analysis
Institute for
Applied Nuclear Technology
(Belgrade, Yugoslavia)
Subcontractor
GC and CCMS Analvsis
Figure 1-1.
Kosovo Test Program Participating Organizations
and Areas of Responsibility
-------
Radian Corporation, of Austin, Texas, is prime contractor for
the work being performed in test Phases II-IV. The areas of
responsibility for the major program participants are also
shown in the figure.
1.3 Test Schedule
The test schedule followed in Phase I along with a
proposed schedule for subsequent phases of effort is shown in
Table 1-1. As indicated in the table, the first test phase was
divided into several test campaigns. Based on the results of
initial sampling, additional campaigns may be scheduled for
Phases II-IV.
1,4 Report Organization
Section 2.0 of this report contains a general descrip-
tion of the Kosovo Lurgi gasification facility and an overview
of the process. Selected parts of the plant are described in
detail, as they relate to the testing carried out in Phase I.
A description of the sampling procedures followed in Phase I
is given in Section 3.0 while Section 4.0 outlines the analytical
methodology. Section 5.0 contains a summary of the results of
Phase I testing and recommendations for future testing at Kosovo.
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TABLE 1-1. KOSOVO TEST PROGRAM OBJECTIVES AND SCHEDULE
Test Objectives
Date
Phase 1:
Campaign 1
Campaign 2
Campaign 3
Phase II:
Campaign 1
Campaign 2
Phase III;
Campaign 1
Campaign 2
Phase IV:
Campaign 1
Campaign 2
Emission Source Screening
(Major Components)
Perfect Methodology
Data Acquisition
Fill in Gaps
Additional Source Characterization
(Minor/Trace Components)
Data Acquisition
As Needed
Ambient Pollutant Concentrations
Data Acquisition
As Needed
Characterize Fugitive Emission
Sources
Data Acquisition
As Needed
November 1977
June 1978
November 1978
Summer 1979
TBD
Summer 1979
TBD
Summer 1980
TBD
TBD - To be determined
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2.0 PLANT DESCRIPTION
The major objectives of this section are to:
o describe briefly the Kosovo gasification
plant and its operating characteristics, and
• identify the sources of the plant's most
environmentally significant waste streams.
2 .1 Process Overview
The Kosovo Lurgi gasification facility is an integral
part of a large mine-mouth industrial complex. This complex
is located near the city of Pristina, in southern Yugoslavia.
As shown in Figure 2-1, the Kosovo gasification plant
consumes a dried lignite feedstock and produces two primary
products: a medium-BTU fuel gas and hydrogen, which is subse-
quently used for ammonia synthesis.
A detailed process flowsheet for the Kosovo gasifica-
tion plant is shown in Figure 2-2. This figure also shows the
sources of the plant's most significant air, water and solid
waste streams.
Many of the process units which have been proposed
for use in conceptual U.S. gasification plants are currently
being used at Kosovo. This includes tar/oil separation
facilities, a Rectisol acid gas removal unit, a Phenosolvan
unit and by-product recovery facilities. The Kosovo plant is
therefore felt to be representative of Lurgi gasification
facilities which are under consideration for future commercial-
ization in the U.S.
-------
Undersized Coal
Lignite
Mine
Raw
Coal
Steam and
Electric
Power
Generation
Crushing, Sizing
and
Drying
Coal
Electric
Power
Gasification
Plant
Medium-BTU
Fuel Gas
1
Air
02
\
\
Separation
N2
as
BiBKHIS^jJlp
H2
t
Nil 3
Plant
NH3 (Used for
Fertilizer
Manufacturing)
Figure 2-1. Kosovo Gasification Plant and its Relationship to
Surrounding Industries.
-------
Flue
Cas
treatment A
Chemicals I
flue G»s
(lignite)
H. P.
Steas to
©00©
tondeii$«te to
©©
Vent
Gases fruM
©0©—
Rich H,S
»ent CO, »enl
Helhanol lo^l) to Aim.
Vcnt Condensat
. Gases
*'nt to Af.
KM ,G""
Sludge t0/ •
Tirs, Heavy OIU I Phenolic Uater
Coolln, U.Ur
„ treated
Mater
Sludgl
Sludge
Notes: H.P. = High Pressure
L.P. = Low Pressure
(3 - The numbers shown in circles are the codes used by
plant personnel to identify specific plant units.
These codes are used in this report to identify
the sources of specific plant process and waste
streams.
-------
While the process flow scheme at Kosovo is representa-
tive of future U.S. Lurgi plants, the environmental control
practices followed at that plant are not. Although many of the
plant's waste streams are controlled, most of these controls
would not be characterized as "best available" by U.S. standards
For this reason, total emissions from the Kosovo plant greatly
exceed the emissions which are expected from a U.S. facility of
comparable size. Nevertheless, the types of emission problems
seen at Kosovo are representative of the problems which will
have to be considered by operators of future U.S. gasification
facilities.
The lignite which is fed to the Kosovo Lurgi gasifiers
is dried by the Fleissner method (high temperature steam soak)
and sized to reject particles less than 6 mm or greater than 60
mm in diameter. After the coal is gasified by reaction with
oxygen and steam at about 2.5 MPa (25 a tin) pressure, the raw
gas is sent to a series of gas cooling and purification opera-
tions. First, in the cooling section, tars, oils, and process
condensate (phenolic water) are condensed and removed from the
raw gas. Then, in the acid gas removal section, roughly 90%
of the carbon dioxide and more than 99% of the hydrogen sulfide
are removed.
Each of the six Kosovo Lurgi gasifiers is designed to
convert 16 metric tons of dried lignite into 12,500 Nm3 of clean
(after Rectisol) fuel gas per hour. Useful by-products re-
covered in the tar/oil separation, Rectisol and Phenosolvan
sections include tars, oils, gasoline, NH^OH and crude phenols.
Design capacity data for the Kosovo gasification plant are
summarized in Table 2-1.
The plant sections examined in the Phase I test pro-
gram include:
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TABLE 2-1. KOSOVO PLANT DESIGN DATA (ASSUMES 5 OF 6
GASIFIERS IN SERVICE)
INPUTS:
Lignite
Steam
Oxygen (96 Vol. %)
OUTPUTS:
Products:
Clean Gas
By-Products:
Tars
Oils
Gasoline
NH.+OH
Crude Phenols
80 MT/hr*
65 MT/hr
9,900 Nm3/hr
60,000 Nm3/hr
2.2 MT/hr
1.3 MT/hr
0.65 MT/hr
0.96 MT/hr
0.36 MT/hr
*MT = Metric Ton = 1000 kg
10
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• Gasification Section (gasifiers and ash
handling equipment)
• Rectisol Plant
• Tar/Oil Separation Section
• Phenosolvan Unit
• By-Product Storage
• Auxiliaries (flare)
These sections were selected for testing because they
are all sources of environmentally significant waste streams.
Plant sections not selected for testing in Phase I are indicated
in Figure 2-3. This figure also indicates the reasons why
specific plant sections were not selected for testing in the
Phase I program.
2.2 Fleissner Drying Section
The moisture content of raw Kosovo lignite is normally
very high (in the range of 40-5070 by weight) . A substantial
portion of this moisture (^507o) must be removed in order to
permit the efficient operation of a Lurgi gasifier. For this
reason, run-of-mine Kosovo lignite is dried and sized prior to
its introduction into the gasification section.
The drying process used at Kosovo was developed by H.
Fleissner in Germany in the 1920's. This process uses pressur-
ized, saturated steam to heat the coal (in several steps) to a
temperature sufficient to drive moisture from the coal without
11
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TOOt HER
*• IN PLANT
USES
I-J
rsj
ATER
r
WASTE
OASES
,
1
QUENCH
COOLING
r
",
.r
TARS. OILS t
CONOENSATE
H.JONH,
MEDIUM
" ITU OAS
B» PRODUCT TARS.
• OILS. GASOLINE,
PHENOLS I NH>
PLANT SECTIONS STUDIED IN THE
PHASE I TEST PROGRAM
PLANT SECTIONS NOT STUDIED IN THE
PHASE I TEST PnOORAM
PLANT SECTION IS A SIGNIFICANT AND UNIQUE SOURCE
j WHICH WILL 8E CHARAC1EHI2ED IN PHASE II
PLANT SECTION IS A SIGNIFICANT WASTE STREAM SOURCE:
HOWEVER.CHARACTERIZATION DATA FOR THIS TVPE OF
SOURCE CAN BE GATHERED MOST COST EFFECTIVELY
IN THE U.S.
PLANT SECTION NOT IN USE
PLAN! SECTION IS NOT A DIRECT SOURCE OF MAJOR
PROCESS. WASTE OR BY PRODUCT STREAMS REQUIRING
CHARACTERIZATION (EXCLUDES CONSIDERATION
OF FUGITIVE EMISSIONS)
FIGURE 2-3 SIMPLIFIED FLOW SCHEMATIC-KOSOVO GASIFICATION PLANT
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destroying the structural integrity of the coal matrix. Mainte-
nance of structural integrity is important because any altera-
tion of the internal pore structure of the lignite could ad-
versely affect its reactivity and weaken the coal particle to
the point that fracturing and generation of fines could become
a significant problem. According to published data on the
Fleissner drying process, the amount of moisture that remains
in the coal after treatment is a function mainly of the steam
pressure applied in the process. At Kosovo, the maximum steam
pressure used is about 3 MPa (30 a tin) and the moisture content
of the dried lignite is normally about 25 wt%. A simplified
flow diagram of the Fleissner drying section indicating the
sources of the major emission and effluent streams generated in
this section is shown in Figure 2-4. The emission streams are
listed in Table 2-2.
The autoclaves used to dry Kosovo lignite are operated
in a batchwise manner. A complete drying cycle, which lasts
from 160-200 minutes, involves the following steps:
Approximate
Step • Duration
Coal Charging 10 min.
First Preheating (low pressure steam) 20 min.
Second Preheating (int. pressure steam) 20 min.
Treatment with Fresh (high pressure steam) 60 min.
First Discharge (int. pressure steam) 20 min.
Second Discharge (low pressure steam) 20 min.
Emptying Autoclave 10 min.
TOTAL 160 inin.
13
-------
•Wet* Rm of
M1r»e Coal %-
(+30 BBS)
Q
«». To Baghouse
This Hooding System
Also Captures Gases
Released from the
Dried Coal Bunker
H.P. Steam
(30 atn)
Hot Condensate or
Intermediate Pressure
(10 atm) Steaa from
Other Autoclaves
Hot A1r (MOfTC)
Used for
Final Drying
Steam and Hoc
Co nd ens ace co
Other Autoclaves
(for uet-coal
warmup)
Dried
Coal
Bunker
Dried Coal
to Sizing Operation
Fleissner
Cofldensate
Figure 2-4.
Process Flow Diagram Showing Sampling Points In
Kosovo Plant Fleissner Drying Section
14
-------
TABLE 2-2.
SIGNIFICANT KOSOVO PLANT FLEISSNER DRYING
SECTION PROCESS AND EMISSION STREAMS
Ul
Screu'
Number
1.0
1.1
1.3
'Stream Io
Stream Description
"Wet" coal I torn mine
Coal bunker vent
Fleiaanar condensate
Scream2
Type
S
c
L
Jre 2-4.
Estimated
Flow Rate
24 HT/hr
Unknown
Unknown
Measured
Flou Rate
(Phase I)
NX
NM
MM
Cotmenci
Theae four stream* will be aaoapled In
Phase 11
*G - gaseous; L - liquid; S - aolid.
*MM - not tueadurcd.
-------
The autoclaves are arranged in groups of four, with the blowdown
steam and condensate from one autoclave preheating the coal
entering other autoclaves.
2.3 Gasification Section
A process flow diagram of the Kosovo plant gasifica-
tion and ash handling sections is presented in Figure 2-5. This
figure also shows the locations of major emission streams origi-
nating in these sections. Table 2-3 lists the process and
emission streams identified in Figure 2-5 and gives values for
their design, estimated or measured flow rates.
The Kosovo plant gasification section contains six
pressurized, fixed-bed, oxygen-blown Lurgi gasifiers. In this
section, dried lignite is fed by conveyor belts to a coal bunker
located above each gasifier. Nitrogen is used to purge each
bunker to guard against the danger of spontaneous ignition of
the lignite. Emissions from the coal conveying and storage area,
consisting mostly of particulate matter, are water scrubbed and
vented to the atmosphere.
Steam and oxygen injected at the bottom of each gasifier
react with the moving coal bed to produce a hot raw product gas.
Hot ash from the bottom of each gasifier is collected in a lock
hopper and water-quenched prior to disposal.
The hot raw gas exiting the top of each gasifier is
directly quenched with water and then further cooled in a series
of indirect heat exchangers. Condensed organic liquids and pro-
cess condensate from this section are sent to the tar/oil
separation section where the aqueous and organic fractions in
the stream are separated.
16
-------
•}
7O
^^ SU,,KO, --;--
COAL
WATCH -f OU.Sr
1 -Hg)
6jv-
TO W4S/f 64 S
INCINERATOR
r
PHENOLIC
Y/ATfH
Sf£AM
> LAHF
7H1Q--
^r^cr-J
f'OINJ
rn DUMP
Figure 2-5. Process Flow Diagram Showing Sampling Points
In Kosovo Plant Gasification Section
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TABLE 2-3. SIGNIFICANT KOSOVO PLANT GASIFICATION
PROCESS AND EMISSION STREAMS
Stream1
Number
2.0
2.1
2.2
3.1
3.2
3.3
3.4
3.5
3.6
12.1
12.2
12.3
Stream
G - goe
Stream Description
Dried sized coal
Coal bunker area - ambient sample
Coal bunker vent
Coal bucket vent
Low pressure coal lock vent
Start-up vent (to flare)
Liquor tank vent
Ash lock vent
High pressure coal lock vent
(to main flare)
Gasifler ash (dry)
Gaalfler asli (wet)
™Ji!iL1Catl0" eectloi> wastewater
locations are shown in Figure 2-5.
'ecus; I - liquid. s _ 8oU(J
Stream1
Type
S
G
G
G
G
G
G
G
C
S
S
I
Design or5'"1
Estimated
Flow Rate
16.0 MT/hr (d)
NA
4,000 Nm'/hr (d)
<26 Nm'/lir' (e)
36 Nm'/hr (d)
Variable
40 Nm'/hr (e)
28 Nm'/hr6 (d)
350 Nm'/hr (d)
2.7 MT/hr (d)
>2.7 MT/hr (e)
3 m'/hr (d)
Measured1 ' 5
Flow Rate
(Phase I) Comments
NM
MA
14,000 Nm'/hr (C2) j Reason for apparent high value during
4,200 Nra'/lir (C3) Campaign 2 cannot be explained
Negligible This vent line Is generally plugged with
coal dust and tars
NM Flow measurement attempted but not success-
fully obtained
NM This stream will be characterized In Phase II
NM
1.65 Nm3/hr (C3)
1-400 Nm'/hr (C3)
NM
NM
NM
'All flow rates normalized to a one-gasifier-in-servlce basis.
s< - ™*d-'1-c-"'-2
ow only - does not include steam injected into vent system.
-------
The high pressure purge gases from the coal lock hopper
are scrubbed in a venturi and routed to the flare. Low pressure
vent gases are released directly to the atmosphere. Coal lock
gas scrubbing liquor is stored in a vented holding tank. Re-
cycled phenolic water from the tar/oil separation section is
used as makeup scrubbing liquor to this system. Slowdown liquor
is routed to the tar separator. Ash lock hopper decompression
gases are scrubbed in a wet cyclone and vented to the atmosphere.
During the initial stages of gasifier start-up, raw
product gas is vented directly to the atmosphere. Later in the
start-up sequence, this gas is flared until desired conditions
are established and a consistent quality gas is being produced.
Start-up gas was not sampled during the Phase I test program.
2.4 Rectisol Section
The Rectisol unit at Kosovo is a major gas purification
step as well as a significant source of gaseous wastes. A pro-
cess flow diagram showing the locations of the key process and
emission streams in this unit is presented in Figure 2-6; avail-
able flow data on these streams are presented in Table 2-4.
Acid gases (e.g., C02, H2S and HCN) are removed from
the cooled raw gas at Kosovo by sorption in a cold methanol-
water solution. First, the cooled raw product gas passes
through a separator and an initial cooling stage where it re-
ceives a cold water wash. Then, the gas is cooled further in a
heat exchanger and a second cooling stage where it receives a
wash with cold, C02-rich methanol before it is scrubbed with
more cold methanol in the primary H2S absorber. The "H2S-free"
gas is then sent to a series of C02 absorbers. In these
columns, C02 is absorbed by a wash of "lean" methanol. Most of
19
-------
-S 6/1 S
GAS
\
°1 h-^ i
(
-------
TABLE 2-4. SIGNIFICANT KOSOVO PLANT RECT1SOL SECTION
PROCESS AND EMISSION STREAMS
Stream'
Number
7.1
7.2
7.3
7.4
7.5
7.6
Stream Description
lljS rich gas (to main flare)
COa vent gas
Rectlsol Inlet gas
Rectisol outlet gas
Cyanic water
Product gasoline to storage
Stream'
Type
G
G
G
G
I
1
Design or3
Estimated
Flow Rate
2,500 Nm'/hr
2.200 Nm'/hr
17.200 Nm'/hr
12.000 Nm'/lir
.8 m'/hr
.13 MT/lir
Measured3'11
Flow Rate
O'liase 1) Comments
NM Flow measurement attempted in Campaign 3,
but not successfully completed
1.100 Nm'/hr (C2)
A, 700 Nm'/hr (C3)
NM
NM
NM
NM
Stream J ocaL lona iire shown In Figure 2-6.
2G - gascoua; 1, - liquid.
3All flow rates nornialtzed to a one-gnaifler-ln-aervlcc basis.
"NM - not measured; (C2) - measured durJng Ciimpalgn 2; (C3) - meneurcd during Campaign 3.
-------
the overhead gas from the first C02 absorber is fed directly
inco the fuel gas distribution system. A second C02 absorber is
used for final C02 removal whenever "clean" product gas is needed
for feed to a cryogenic H2 separation unit.
The H2S-rich waste gas which is generated in this
unit (stream 7.1) is sent to the main plant flare while the
C02-rich waste gas (stream 7.2) is vented directly to the atmos-
phere. Gasoline and cyanic water condensed from the raw gas in
this unit are sent to the by-product storage and tar/oil separa-
tion sections, respectively. The clean fuel gas leaving the
Rectisol unit is fed into the product gas distribution system.
2.5 Tar/Oil Separation Section
The first step in the plant's wastewater treatment
sequence takes place in the tar/oil separation section. Liquid
stream's fed to the tar/oil separation section come from several
locations within the plant including the gasification, quench/
cooling, and Rectisol sections. Therefore, this section is the
source of several significant by-product streams.
In the tar/oil separation section a series of phase
separators are used to isolate heavy tar, light tar, and medium
oil from the incoming condensate streams. These organic frac-
tions are all sent to storage. Process condensate (phenolic
water) is sent to the Phenosolvan section for further treatment.
Major waste streams produced in the tar/oil separation
section include:
o a sludge consisting of a combination of a
heavy tar and dust (which is landfilled),
22
-------
• gases that are released from a series of
depressurization vessels and then collected
and incinerated, and
• vent gases from a series of atmospheric-
pressure surge tanks that are vented directly
to the atmosphere.
Figure 2-7 shows a process flow diagram for the tar/oil separa-
tion section and indicates the sources of these waste streams.
A detailed listing of the major by-product and waste streams
leaving this section is contained in Table 2-5.
2.6 Phenosolvan Section
The Phenosolvan section accomplishes three distinct
functions:
• residual tar and oil removal,
• ammonia (NH3) stripping, and
• phenol extraction.
Residual tars and oils entering the Phenosolvan unit
with the inlet wastewater are removed in a storage tank/gravity
separator and a series of sand filters. The phenolic water is
then heated and fed to two degasing columns where dissolved
gases such as NH3, C02 and H2S are steam stripped from the
water. According to the plant design, by-product NH^OH was to
be recovered at this point. However, during the Phase I test
program, all stripper vent gases were being released directly
to the atmosphere.
23
-------
to
C,AS COMDEMSAIt
FROM RCCHSOl
COOtING WA11R
HttEASED GASES
fO INCINERATOR
)fltCNOt/C WA1LR
10 PHtNOll PIAfjr
RC.JURN TO 7AR SEPARATOR
@
IAR JO STOHAGE
HVY TAR ( Pt/sr
TO DUMP
Figure 2-7. Process Flow Diagram Showing Sampling Points in Kosovo Plant Tar/Oil Separation Section
-------
TABLE 2-5.
SIGNIFICANT KOSOVO PLANT TAR SEPARATION
SECTION PROCIiSS AND EMISSION STREAMS
Stream'
Number
13
13
13
13
N> 13
Ul
13
13
13
13
13
13
.1
.2
.3
.4
.5
.6
.8
.9
.10
.11
.12
Stream DCS
crlptlon
Tar tank vent
Slop tank
Medium oil
S lop tiink
CondeiiBate
Expansion
„ 1 1
Heavy tar
Heavy tar
Light tur
Medium oil
(tar)
tank
( mod 1 i
tank
gaaes
vent
vent
itra oil) vent
vent
(to main flare)
and duat
Phenol Ic water
to phenosolvan
Stream2
Type
G
G
G
G
G
G
L/S
'-I
1- 1
L
I
Design or3 '^
KB tj ran ted
Flow Kale
>.4 Nm'/hr (c)
Negligible
>.25 Nio'/hr (c)
Negligible
Unknown
26 Nm'/hr (d)
.1 MT/Iir (d)
.4 MT/hr (d)
.25 MT/hr (d)
13 m'/hr (d)
Measured' • 5
F'low Rate
(Phase I) Comments
.5 Nm'/hr (C3) Intermittent flow. Tills tank Is filled and
emptied on a batch basis.
NM This tank IB not normally In service.
17 Nm'/hr (C3) ** Significant emission stream **
NM This tank Is not normally In service
1 Nm'/lir (C3)
NM
NM
NM
NM
NM
'Stre/im local JOHH are shown In Figure 2-7.
JG - gaseous; L - liquid; S - solid.
SA11 flow rates nonruillzed to a one-gaalfler-ln-8ervlce basis.
""(d) - dcBl^u; (e) - nstlm,iLed.
5NM - not raoaaured; (C3) - meaeured during Campaign 3.
-------
The phenolic water from the bottom of the first de-
gasing column is run through a series of heat exchangers and
columns where it comes in contact with diisopropylether (DIPE).
Plant design dictates that treated wastewater from the Pheno-
solvan unit be sent to a biological wastewater treatment plant
for further processing. However, this unit was not in service
during the Phase I test period. Phenol-rich DIPE is thermally
regenerated. The "lean" DIPE is recycled to the extraction
section while the raw phenol is routed to by-product storage.
Figure 2-8 shows a process flow diagram for the
Phenosolvan section. Major process and emission streams found
in this section are listed in Table 2-6.
2.7 By-Product Storage Section
As shown in Figure 2-9, the by-product storage section
consists of a series of liquid product storage tanks and a
pumping station. Each tank is equipped with a vent line which
exhausts directly to the atmosphere. The vents having the
greatest potential for emissions are the gasoline, medium oil,
and raw phenol tank vents. Sample point designations for
gaseous, liquid and solid waste streams generated in the by-
product storage section are summarized in Table 2-7.
26
-------
PHENOLIC
WATER
VI.NI
UNCLEAN OIL
TO
ro
COUDENSATf
NH3 TO
STOK.AGS
WASTE
\SATK TO
3/0
PHENOL
TO STORAGE
DEGASING CYCLONE
TEEDWATER STORAGE TANK AND OIL WATER SEPARATQR
UNCLEAN OIL STORAGE
SAND FILTERS
FILTERED FEEOW/VTER STORAGE TANK
FEEDWATER PREMEATERS
CONDENSATE STRIPPER
FEEOWATER COOLERS
2nd DEGASING COLUMN
SLOP TANK
EXTRACTION COLUMNS
FCEDWATER PREHEATERS
DIPE RECOVER! COLUMN
WASTEHATER COOLERS
CONDENSER/COOLERS
RICH DIPE STORAGE TANK
REGENERATION SECTION PREHEATERS
DIPE RECOVERY COLUMNS
CONDENSERS
DIPE STORAGE TANKS
BY-PRODUCT PHENOL COOLERS
BY-PRODUCT STORAGE
Nil, STRIPPER CONDENSER
NH, ABSORBER
BY-PRODUCT NH»OH STORAGE TANK
Figure 2-8. Process Flow Diagram Showing Sampling Points in Kosovo Plant Phenosolvan Section
-------
TABLE 2-6. SIGNIFICANT KOSOVO PLANT PHENOSOLVAN SECTION
PROCESS AND EMISSIONS STREAMS
O
Stream*
Number
14.0
14.1
14.2
14.3
14.4
14.5
14.6
14.7
14.8
14.9
14.10
14.12
14 . 13
14.14
14.15
14.16
•^TnT!
Stream Description
Plienosolvan inlet water
Cyclone (Cl) vent
Phenolic water tank (T2) vent
Unclean oil tank (T3) vent
Filtered water tank (T5) vent
Degasing column (C7) vent
NII3 atripper cooler (F.25) vent
2nd degasing column (C9) vent
Slop tank (T10) vent
I'henol storage tank (T24) vent
DIPE tank (T22) vent
Nlh absorber (C26) vent
Nllj storage tank (T27) vent
Nlli.011 product to storage
Unclean oil to storage
Raw phenols to storage
Stream2
Type
1,
G
C
G
C
C
C
C
G
C
G
G
G
I
L
L
Design or3-11
Estimated
Flow Rate
13 n'/hr (d)
2 Nm'/hr (d)
Unknown
Unknown
Unknown
9 Nra'/hr (e)
4 Na'/l.r (e)
.4 Nm'/hr (c)
Unknown
.08 Nm'/hr
.5 Nm'/hr (e)
13 m'/hr (d)
Unknown
Unknown
.2 HT/hr (d)
.03 MT/hr (d)
.09 HT/hr (d)
Measured'.5
Flow Rate
(Phase I) Comments
NM
NH
NM
NH
NM
60-150 Mra'/hr (C3)
NM
NM
NM
.00-. 24 Nm'/hr (C3)
NM
NM
NM
Nil] recovery system not in operation during
NM Phase I testing
NM
NM
NM
G - gaseous; L - liquid.
'All flow rates normalized to a one-gaslfier-in-service basis.
'(d) - design; (e) - estimated.
5A11 flow rates are expressed on a dry gaa (moisture free) basis; (C3) - measured during Campaign 3.
-------
LEGEND
A - VENT GAS
B - LIQUID IN TANK
C - SLUDGE
TO POWER
STATION
LOADING
FIGURE 2-9. PROCESS FLOW DIAGRAM SHOWING SAMPLING POINTS IN KOSOVO
BY-PRODUCTS STORAGE AREA
-------
TABLE 2-7.
SIGNIFICANT KOSOVO PLANT BY-PRODUCT STORAGE
SECTION PROCESS AND EMISSION STREAMS
O
Stream1
Number
15.1 A/B/C2
15.2 A/B/C2
15.3 A/B/C2
15.4 A/B/C2
15.5 A/B/C2
15.6 A/B/C2
Stream Description
Tar tank
Medium oil tank
Gasoline tank
Raw phenol tank
Unclean oil tank
NIK OH tank
Stream'
Type
G/L/S
C/L/S
C/L/S
C/L/S
G/L/S
C/L/S
Design or"1 • s
Estimated
Flow Rate
.5 Nm'/hr
.25 Nm'/hr
.13 Nra'/lir
.08 Hm'/hr
.03 NuVhr
.2 Nra'/hr
Measured*1 " 6
Flow Rate
(Phase I)
NM \
NM
03 Nm'/lir (C3)
NM
NM /
Basci
tank
emieu
NM Tank
Comments
upon visual observation the gasoline
is clearly the most significant
ion source among this group of tanks
not In service
Stream locations are Hluiwn in Figure 2-1).
A - vent gnsj B - liquid In tank; C - sludge In bottom of tank.
*C - gaseous; I - liquid; S - solid.
All flow rates normalized to a one-gaslfIcr-ln-nervlce basis.
Tank vent flows assumed equal to the volume displaced by normal process stream flow.
'NM - not measured; (C3> - neasured during Campaign 3.
-------
2.8 Auxiliaries
The only other Kosovo plant waste stream characterized
in the Phase I test program was the combined waste gas to the
main plant flare (sample point 20.1). This stream was sampled
as part of Phase I primarily because this sample point was easily
accessible and its location permitted making reasonably accurate
flow measurements. This combination of factors was not found at
any of the other sampling points used to sample the individual
streams that are sent to the flare (gasifier high pressure vent,
Rectisol H2S rich vent, and tar/oil separator high pressure
vent).
31
-------
3.0 SAMPLING PROCEDURES
The sampling procedures for Phase I are outlined in
this section. Standard EPA-approved sampling practices were
followed in most instances. Some sampling modifications occurred
due to a better understanding of sampling problems gained after
each of the three Campaigns in Phase I. Several of the improved
sampling procedures were incorporated during Phase I (Phase I
testing lasted over a year). All deviations from standard
practices are discussed in this section.
Table 3-1 contains a list of components sampled and
the sampling procedures used during Phase I. The sampling
methods can be separated into the following categories:
• flow rates,
• gases analyzed by wet chemical methods
(bubbler method or ORSAT),
• gases analyzed by gas chromatographic
techniques,
« particulates,
• waste water samples, and
• solid samples.
A discussion of the details of the gas sampling proce-
dures, flow rate determinations, particulate sampling procedures,
and their deviations from standard procedures follows.
32
-------
TABLE 3-1. SAMPLING PROCEDURES
Component
Sampling Method
Gas Streams
Flow Rate
Fixed Gases (H2, 02, N2
, CO, C02)
Hydrocarbons (Ci - Cs)
Sulfur Species (H2S, COS
S02, MeSH3, EtSH )
Particulate
Phenols
Ammonia
HCN
H2S
Moisture
Wastewaters
All Species
Solid Samples
Moisture
Ash Content
Phenols [(1) total and
(2) volatile]
Elemental Analysis
(C, H, 0, N, S)
COD
See discussion in text
A. ORSAT (Campaign 1 and 2)
B. Perma pure drier; collection in
silanized glass bulb (See text)
Perma pure drier; collection in
silanized glass bulb
Perma pure drier; collection in
silanized glass bulb
EPA Method 5 train with filter or
impingers (See text)
Bubblers with NaOH solution
Bubblers with H2SOit solution
Bubblers with NaOH solution
Bubblers or glass bomb - cadmium
acetate solution
EPA Method 5 train
All determinations were made on
samples collected in glass bottles
with teflon-lined caps
Grab sample (Composite)
Grab sample (Composite)
Water filtrate
Grab sample (Composite)
(1) Dried material at 105°C
(2) Ash at 850°C
Grab sample (Composite)
methyl mercaptans
ethyl mercaptans
-------
3.1 Flow Measurement Procedures
Traverses across at least one axis of the flowing
stream using an S-type pitot tube were used to determine flow
rate according to the EPA Method 2 procedure for the following
four streams:
• 2.2 Coal Bunker Vent Gases,
• 7.1 H2S-Rich Gases,
• 7.2 C02-Rich Gases, and
• 14.5 Phenosolvan Stripper Vent.
For gas streams with flows showing high variability
with time, centerline velocity measurements were made using an
S-type pitot tube. The resultant flow signal was monitored
over an extended period of time and an estimated "average" flow
rate value was calculated by integration over the period of
measurement. Streams monitored in this manner were:
• 3.2 Low Pressure Coal Lock Vent,
• 3.5 Ash Lock Vent,
• 3.6 High Pressure Coal Lock Vent, and
• 20.1 Waste Gases to Flare.
34
-------
Surge tanks were equipped with vent pipes mounted as
shown in Figure 3-1.
->.Vent Gas Flow
Pipe Diameter - 50 mm
(typical)
Length <1 m
(typical)
•* Flange
Tank
Figure 3-1. Typical Surge Tank Vent Pipe Arrangement
High velocity gas flows were estimated from velocity
pressure head readings using a standard pitot inserted into the
throat of the vent pipe (see Figure 3-2). Vent streams measured
using this approach included:
• 13.1 Tar Tank Vent,
• 13.3 Medium Oil Tank Vent, and
• 13.6 Phenolic Water Tank Vent.
Vent Pipe
—>-Stream Flow
Pitot Tube
Figure 3-2.
Flow Measurement Approach For
High Velocity Tank Vents
35
-------
Low velocity vent gas flows were measured using an
anemometer and flow tube, as shown in Figure 3-3.
•Plastic Bag
Hot-Wire
Anemometer
Probe
Flow-Tube
'." PVC Pipe)
Duct Tape Used
to Seal Bag to
Vent Pipe and
Flow Tube
where,
£ = 10 Pipe
Diameters
Figure 3-3. Flow Measurement Approach for
Low Velocity Tank Vent Flows
Vent streams measured using this approach included
14.9 Phenol Tank Vent
15.3A Gasoline Tank Vent
3.2
Particulates
The particulate concentration in the gas streams was
determined by one of two methods, depending on moisture content
of the stream. The standard EPA Method 5 technique, utilizing a
glass fiber filter heated to at least 110°C, was usable only with
relatively dry streams (e.g., stream 2.2). For sampling of gas
streams with high moisture content, an impinger technique was
developed. Two Smith-Greenberg impingers, each containing 200ml
of deionized water, were followed by two modified Smith-Greenbergs,
one dry and one containing indicating silica gel. During sampling,
all impingers were kept in an ice bath. This technique was used
at points 3.2, 3.5 and 3.6. Following sampling, the impinger solu-
tions were filtered through glass fiber filters and the suspended
lids were determined gravimetrically. An aliquot of the solution
so
36
-------
was evaporated to dryness to determine dissolved solids and a
second aliquot was extracted with methylene chloride. The
methylene chloride extract was then evaporated to dryness and
the residue weighed to determine extractable organics. The
reported particulate loading is based on the sum of suspended
and dissolved solids.
Moisture content of the gas streams was determined
from the weight gain of the impingers, for both the Method 5
and impinger techniques. Sample gas volumes were measured with
a dry gas meter and corrected to standard conditions.
3.3 Gas Sampling For Wet Chemical Analysis
Phenols, ammonia, hydrogen cyanide and hydrogen sul-
fide were collected from the gas streams by sorption using two
fritted glass bubblers connected in series. Sample gas volumes
were measured with a wet test meter. Separate sampling was
conducted for each species using the following sorption solu-
tions :
« Phenols - 5% NaOH
• Ammonia - 5% H2SC\
• Hydrogen Cyanide - 10% NaOH
a Hydrogen Sulfide - 4% Cd(OAc)2
In addition, an alternative method for hydrogen sul-
fide was used during Campaigns 1 and 2 and part of Campaign 3.
An -^IZOOrnl sample bomb was purged with a minimum of ten bomb
volumes of sample and then sealed at atmospheric pressure by
37
-------
closing ground glass stopcocks on each end. Hydrogen sulfide in
the captured gas sample was recovered by injecting successive 50ml
aliquots of cadmium acetate solution into the bomb, shaking the
bomb, and draining the solution. Sorption solution injections
were repeated until no yellow cadmium sulfide precipitate was
evident. The bomb was then rinsed with distilled water and
the rinse and all sorption solution aliquots were combined for
analysis. This technique was found to give results comparable
to gas chromatography except for those instances when moisture
condensed in the bomb during sampling.
3.4 Grab Gas Samples for Gas Chromatography
Gas samples for gas chromatographic determination of
fixed gases, Ci-Cs hydrocarbons and sulfur species were collected
in 125ml and 250ml glass bombs with teflon stopcocks on each
end. Teflon tubing was used to transport the gas to a sample
conditioning assembly. For samples with high moisture content,
the teflon tubing was heated to avoid condensation. The sample
conditioning assembly consisted of a heated teflon filter for
®
particulate removal, a Perma-Pure drier, and a teflon-lined
pump. The Perma-Pure drier consists of an extruded permeation
tube which removes water vapor by selective permeation across the
tubing wall. A dry air stream flows countercurrent to the sample
stream on the opposite side of the tubing wall. Driving force
for the permeation is provided by the moisture differential
between the sample stream and the dry air stream. Dry air was
®
provided by passing ambient air through a column of Drierite
and activated charcoal. Dry air and sample gas flow were monitored
with rotometers. A 0 - 1 x 105Pa gauge at the pump outlet
measured sample bomb pressure.
A gas sample was collected by first purging the system
with sample gas and then attaching a clean sample bomb to the
38
-------
pump outlet. Between each use, sample bombs were cleaned by
filling with distilled water to force out all residual gas and
then purging with dry nitrogen until dry. During sample collec-
tion, the bombs were purged with a minimum of ten volumes of
sample and the exit stopcock was closed. When the pressure in-
side the bomb reached ^6.9 x lO^Pa, the inlet was closed and
the bomb was detached from the pump outlet. Immediately follow-
ing collection, the samples were transported to the laboratory
for analysis. Sample collection was performed at least in dupli
cate. Sampling was repeated if leakage was apparent, either
from a loss of bomb pressure or the presence of oxygen (from
the fixed gas analysis) in gas streams where oxygen would not
be expected.
39
-------
4.0 ANALYTICAL METHODOLOGY
The analytical methodology for Phase I is outlined in
this section. The methodology includes standard EPA methods,
ASTM methods, DIN (German Institute for Standardization e. v.)
methods and Russian Unified Methods of water analysis.
The analytical procedures are classified according to
sample type:
• gases,
• waste waters, and
• solids.
The procedures for the various sample types are listed
in Tables 4-1 through 4-3. The discussion deals primarily with
deviations from the standard methods.
4.1 Analytical Methods for Gases
Both wet chemical and gas chromatographic methods were
used for the analysis of gases. Table 4-1 contains a list of
all gaseous species determined in Phase I, along with the appli-
cable analytical methods used and a brief description of the
standard methods and references.
All methods followed the standard procedures except
the gas chromatographic method for analyzing sulfur species.
The major changes for this analysis were the column and supply
system for the standards. The column used was a 3m (10 ft by
2mm ( 0.8 in.) ID teflon tubing packed with 1% TCEP and 0.5%
40
-------
TABLE 4-1. ANALYTICAL PROCEDURES FOR CASM
Coeponent
Hothod
Deacrlpclon
Reference*
Gaa Screama
Flou Rats
Fixed Gases
(111. 0,. N,, CHk.
CO. CO,)
Hydrocarbons (C,- Ct)
Sulfur Species (HjS,
COS, SOj. Mesh, ETSK)
Partlculatea
Phenols
Ammonia
HCN
H,S
Holature
EPA Method 2 (Moat Instances)
A. "ORSAT" (Campaign 1 and 2)
B. EPA Screening Methods
EPA Screening Methods
Modified EPA Screening Methods
EPA Method 5 or Gravlmetry for
TSS and TDS
ASTM 510A, 510B and 510C
ASTO 418*. 4180
ASTM 413A. 413C
DIN Waste Ucter Method C-3
(Same as EPA Method 11)
EPA Method k
Type S PI tot Tube Method
A. "ORSAT" Wet Chemical Methods
B. Gas Chromatographic Method Using
a Thermal Conductivity Detector
Gaa Chromatographlc Method Using
a Flame loulzutton Detector
Gas Chromatographlc Method Using
A Flame Photometric Detector
Weigh participates caught on a glass
fiber filter or filler and weigh iron
impinger catch
Spcctrophotometric with 4-amlno-
antlpyrlne Dye
Distillation of ammonia into boric
acid solution with back tltratlon
Distillation followed by silver
nitrate tltratlon
lodomecrlc tltration of CdS pre-
cipitate
Cold plus sillcs gel implngers
weight gain
Environmental Reporter, (Bef. 1)
October 21, 1977, P. 65-75
A. "ORSAT"
». "Level 1" Manual (R«f. 2)
Ref. 2
Ref. 2 (See Text for Modifi-
cation).
Bef. 1, P. 81-89
(See Text in Sampling Section)
Standard Methods for the Exami-
nation of Water and Waste water,
14th Edition (Kef. })
Ref. 1 (41BA,
Ref. 3 (413A, 413C)
Deutache blnliel tbuerfahren zur
Wasser Untersuchung (3rd Edition,
1975) (C-l) (Kef. 4)
Ref. 1 (pp 80-84)
-------
TABLE 4-2. ANALYTICAL PROCEDURES FOR WASTE WATERS
Component
Method
Description
References
Waata Waters
Nil i (free)
Nil, (bound)
HiS
ci-
COD
Pe rnangana ta
Phenols (volatile)
Phenolii (non-
volatile)
Tara and Oil*
Dry Solid*
TS (Total Solid.)
TDS (Total Dissolved
Solids)
TSS (Total Suspended
Solids)
pH Value
Sulfatea
Thloaulfates
Rhodanate
(CNS-)
ASTM 418A, 418D
DIN Waste Water Method E-5
(Same aa ASTM 421 and 418D)
DIN Uuste Water Method C-3
(Same aa EPA Method 11)
ASTM 414A. 414C
DIN Waste Hater Method D-l
(Same aa ASTM 408A or 408B)
DIN Waste Water Method D-9
(Same aa ASTM 419E)
DIN Waste Water Mothod D-10
(San* an ASTM 420)
ASTM 508
DIN Uuute Water Method 11*4
ASTM. 510A, 5108 and 510C
DIN Waate Water Method H-16
Russian Unified Methods - Tar
ASTM 208
ASTM 424
ASTM 427C
Ruualan Unified Methods -
Thloaulfatea
Runs Ian Unified Methods -
Rliodanute
Dlatlllatlon Into boric acid
followed by back tltratlon
Kjeldahl reaction plua aa above
for free Nllj
lodomeerlc tltratlon of CdS
precipitate
Distillation followed by
colorlnictrlc determination uulng
SPADNS reagent
Tltratlon with mercuric or silver
nitrate
Colorlmetrlc method ualng chrono-
troplc acid
Colorlmetrlc method ualng aulfanlllc
acid and naphthylamlne hydrochlorlde
Reflux utth KjCrjflj and HjSO^ and
back titrate ulth Fc(NIU )l(SO^)2
Acidic and basic reflun with KMnO,,
add excess oxalic acid and titrate
with KMn(K
Spectrophotometrlc with 4-andno antlpyrlne
Extraction, convert to phenolatea and
tltratlon using Iodine
Ether extraction between pH 3 and 4
followed by evaporation and weighing
(See text)
Dry to constant weight at 105 C
Filter before drying filtrate
Filter before drying precipitate
Electrometrlcally using a glass-reference
electrode pair
Turbldlmetric (Not Used)
lodotnetrlc tltration
Coloritnetrlc determination ualng
pyrldlne and barbituric acid
Ref. 3 (418A. 4i8l»
Ref. 4 (K-5)
Ref. 4 (C-3)
Ref. 3 (414A. 4I4C)
Ref. 4 (D-l)
Ref. 4 (D-9)
Ref. 4 (U-10)
Ref. 3 (508)
Ref. 4 (H-4)
Ref. J (5IOA, » and C)
Ref. 4 (H-16)
Uni fj ert Hethod__of_ Wattr Analysis
(LU-096)", kd'lcej by Yu. LuvT,"
"Hilmiya", M.»scow (Ref. $)
Ref. 3 (208)
Ref. 3 (424)
Ref. 3 (427C)
Ref. 5 (Thtoaulfates)
Ref. 5 (Rhodanate)
-------
TABLE *-3. ANALYTICAL PROCEDURES FOR SOLIDS
-P-
UJ
Component
Solid Samples
Moisture
Ash Content
Phenols
Total Volatile
Elemental Analysis
(C, II. O. K. S)
Method
ASTH D3173
ASTH 208
See Waste Waters
DIN Method 11-16
ASTM 510A. 510B and 510C
Standard Ultimate Analysis
See Waste Waters
Description
Dry to constant weight
at 105°C
Heat at 550 C to constant
weight
Extraction of solid with acidified
water then treat as waste water sample
Determination of combustion products
Slurry small araount of sample
Annual Book of ASTM Standards;
Part 26 Ganeous Fuels: Coal
and Coke; Atmospheric Analysis;
Ref. 3 (208)
Ref. 3 (5IOA. 1. C)
Ref. 4 (11-16)
Rcf. 3 (500)
-------
HaPOit on 60/80 mesh Carbopak B. The gas chromatographic oven
program was comprised of an initial hold for 4 minutes at 40 C,
heating at a rate of 16°C/minute to 110°C, and a hold for 5
minutes. Gas calibration standards were produced using certified
permeation tubes in a thermostated oven (Metronics Dynacalibrator
Model 230) .
4 .2 Analytical Methods for Waste Waters
Table 4-2 contains a list of all water quality measure-
ments made in Phase I along with the applicable standard methods,
and a brief description of the methods and references.
In cases where particulates, tars, oils and water were
mixed, the method for tars and oils varied from the Russian
Unified Method. In these instances, the water was extracted
with methylene chloride and the two layers were separated. The
aqueous layer and then the methylene chloride layer were fil-
tered through medium filter paper. The particulates stayed on
the filter paper and any tars and oils passed through with the
methylene chloride. The weight of the residue left after eva-
poration of the methylene chloride at room temperature repre-
sented the weight of tars and oils in the sample.
4.3 Analytical Methods for Solids
The analytical procedures for the solids followed
standard methods in Phase I. The methods along with a brief
description and references are listed in Table 4-3. No devia-
tions from standard methods were necessary.
44
-------
5.0 RESULTS AND RECOMMENDATIONS
One of the major objectives of Phase I testing at the
Kosovo facility was the identification of potentially harmful
waste streams associated with a Lurgi gasification plant and
the prioritization of control needs for those streams. The
identification was made in accordance with the EPA's Source
Analysis Model/lA (SAM/1A) which enabled prioritization of the
control needs according to the discharge severity associated
with the streams. These data provide reasonable bases for
identifying and prioritizing potential sources of environmental
problems associated with a Lurgi plant. However, the data are
not intended to exactly define the environmental impacts of
plants designed for construction and operation in the U.S.
The data that were collected during Phase I testing
reveal a high degree of variability. Two factors contribute
heavily to that variability:
• variation in plant operation as experienced
during the test periods, and
• variation in the characteristics of the
lignite that was used as the gasification
feedstock.
The Kosovo gasification facility is operated as a
peaking rather than a base load unit. As a result, gas produc-
tion is varied to meet the demand and likewise, conditions in
the gasifier can vary significantly with time.
Analysis performed on the lignite feedstock during
the test period revealed variation in several critical para-
meters (Figure 5-1) . The differences seen in heat value (HV),
45
-------
Typical or
Average Value
4000 -
HV
/Kcal\ ]
V Kg /
3000 -
30 -
•
•
£* a
(wt. %)
20-
20-
*
Ash "
(wt. %) I
10-
1.6-
•
S
(wt. %) "
.6-
O >
0
: o ° o 3600 oo0-
0 o °
o
•o o
«
. o
»
•
M
«
o •
• °° 0°000 o° 24% °°
0
L. O
<->„
o
•
•1
^
! ° o ° 0 0 15% •
. o o
o
•
. 0 0
o 0
Oo OOOo ° "*
o
«•
V
00°.
o o .
•
d % ^ Q O
•
41
• 4000
•
•
•
• 3000
- 30
•
0
V
*
• 20
• 20
•
rt
•
•10
-1 .6
•
r .6
1234567891012 14 16 18 20 24 26
NOV. 1977
Figure 5-1. Kosovo Lignite Data Gathered
During Campaign I
46
-------
moisture content, ash and sulfur can be significant contributors
to the variations found in the test data. Problems similar to
those experienced during Phase I testing often necessitate
acceptance of single point samples from streams having flow,
temperature, pressure and composition characteristics that
changed with time. In spite of the variation problems, the
point values measured are reasonably valid indicators of the
stream's characteristics. In addition, as testing progressed
sampling and analytical procedures were refined such that the
impact of process variability on sample validity was less severe
in the latter stages of Phase I.
Based on the EPA SAM/1A method for prioritizing
pollutants, the data from Phase I testing indicates the
following:
• Of the components measured, benzene
presents the most significant potential
for adverse health effects .
• Mercaptans present a potential for
adverse health effects comparable to
benzene and greater than H2S.
• Of the fixed gases measured, CO is the
most significant pollutant.
« Of the two nitrogen species measured, NH3
appears to present a greater potential
for adverse health effects than does HCN.
e Organic loading (COD) in the major aqueous
waste stream from the Kosovo plant (Pheno-
solvan effluent) is substantial, despite
47
-------
the effective removal of phenols by the
process.
• Sulphur species in the liquid by-products
is more concentrated in the "lighter"
fractions. Therefore, the heavier hydro-
carbons might be used to satisfy on-site
fuel needs with little resultant impact on
SO? emission levels.
5.1 Gaseous Emissions
A SAM/1A analysis (Ref. 2) was used as a basis for
prioritizing both the atmospheric emission streams and the
individual components present in those streams. SAM/1A is the
simplest member of the Source Analysis Models (SAM's) which are
being developed under the direction of the Energy Assessment
and Control Division of EPA's Industrial Environmental Research
Laboratory at Research Triangle Park, NC. Basically, the SAM/1A
analysis involves comparing measured emission stream pollutant
concentrations with concentration values for those pollutants
which may cause adverse health and/or ecological effects. The
"target" values which are used for this analysis are referred
to as Multimedia Environmental Goals (MEG). A discussion of
the procedures used to establish specific MEG values for the
compounds addressed in this program is contained in Reference 3.
The SAM/1A methodology was developed to provide a
rapid screening technique for identifying potentially harmful
waste streams and prioritizing waste streams for more detailed
analysis. Major assumptions implicit in the use of the SAM/1A
methodology are as follows:
48
-------
• The components currently included in the
MEG's are the only species that must be
addressed at this time.
• Transport of waste stream components to
the external environment occurs without
chemical or physical transformation of
those components.
• Actual dispersion of a pollutant from a
source to a receptor will be equal to, or
greater than, the safety factors normally
applied to acute toxicity data to convert
those data to estimated safe chronic ex-
posure levels.
• The MEG values (Ref. 3) developed for each
substance are adequate for estimating acute
toxicity.
• No synergistic effects occur among the
waste stream components.
These assumptions, along with the accuracy of the test data and
the basic assumptions used in developing specific MEG values,
must be considered when interpreting test results using a
SAM/1A analysis scheme.
The following procedure was used in performing a
SAM/1A analysis of the Kosovo test data:
1) Concentrations of major and minor components
of each stream sampled were determined.
49
-------
2) Health and ecological MEG values were ob-
tained from Reference 3 for each compound
identified. Discharge MEG (DMEG) and
Ambient MEG (AMEG) values were considered
3) Health and ecological discharge severity
(DS) values were calculated for the com-
pounds found in each waste stream. The
following equation defines DS for com-
ponent "i":
(DS)i = (dc)i/(DMEG)i
where dc. = measured concentration of
component "i" in stream.
DMEG. = Discharge MEG value for
component "i" obtained from
the MEG's data base (Ref. 3).
Separate health and ecological
values are listed.
4) Total stream OS's (TDS's) were calculated by
summing the DS values for individual compounds.
5) Total stream weighted discharge severities
(TWDS's) were calculated for each stream
by multiplying the TDS by the appropriate
stream flow rate.
The resulting TWDS's for each stream were used to prioritize
the emission streams of major concern. DS values were used to
prioritize individual stream components or component classes
to determine needs for more detailed analysis .
50
-------
DMEG values for the specific gaseous species measured
in the Phase I test program are listed in Table 5-1. From this
table, it can be seen that the most toxic ambient pollutants
addressed in the Phase I test program, from a health-effect
point of view, were benzene and methyl and ethyl mercaptans.
C2 hydrocarbons (as ethylene) and NH3 represented the compounds
that may have the most harmful ecological effects at low concen-
tration levels.
Potential health-related (based upon health DMEG's)
discharge severity values for the high priority emission streams
identified in Section 2.0 are shown in Table 5-2. Ecology-based
DS calculations are presented in Table 5-3. The analytical data
used to support these calculations are given in Table 5-4. The
data presented in Tables 5-2 through 5-4 support the conclusions
stated in Section 5.0.
While the data presented in Tables 5-2 through 5-4
show some interesting trends, several factors limit the extent
to which these data can be used to draw firm conclusions about
the environmental impacts of the process. Some of these factors
are :
• Most of the data presented in Table 5-4 are
based on single point measurements and there-
fore are not representative of mean operating
conditions encountered during normal plant
operation.
e Other components not analyzed as part of Phase
I (e.g., polynuclear aromatics) may have a
significant effect on final DS and TODS values,
thereby changing the indicated priorities .
51
-------
TABLE 5-1. DMEG VALUES FOR GASEOUS SPECIES MEASURED IN KOSOVO STREAMS
Ln
Fixed Gases
Hydrocarbons
Sulfur Species
and Other
Component
H2
02
CIU
CO
C02
C2'a
CS'8
Cn's
Cs's
C6's
Benzene
Toluene
H2S
COS
CH3SH
C2II5SH
Nil 3
1ICN
Phenol
Health
UMEG Value
(Hg/ra')
HA
NA
3.3 x 10s
4.0 x 10"
9.0 x 10s
6.1 x 106
9.0 x 10s
1.4 x 106
1.8 x 10*
3.6 x 10s
3.0 x 103
3.8 x 10s
1.5 x 10*
4.4 x 10s
1.0 x 10J
1.0 x 103
1.8 x 10"
1.1 x 10"
1.9 x 10"
Basis
-
Asphyxiant
Asphyxiant
Asphyxiant
Asphyxiant
Asphyxiant
Asphyxiant
Asphyxiant
Asphyxiant
Toxic
Toxic
Toxic
Toxic
Toxic
Toxic
Irritant
Toxic
Toxic
Ecology
DMEG Value
(Mg/n.3)
NA
NA
NA
1.2 x 10s
NA
1.0
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
3.5 x 102
3.4 x 10"
NA
Bouie
-
-
Plants (Tomato)
-
Plants (All)
-
-
-
-
-
-
-
-
Plants (Mustard)
Plants (Orange Trees)
-
NA - Not available
-------
TABLE 5-2. HEALTH-BASED DS. TD8. AND TWOS VALUES FOR KOSOVO "MICH PRIORITY"
ATMOSPHERIC EMISSIONS SirKAMS
01
CO
13.1
3.2 3.6 Tar
Lock Hopper Vent Caeca Tunk
13.3
Medium
Oil
Low Pressure High Preuaure Vent Tank Vant
Fl«d Onsen (DS)
HI
Oi
N,
au
CO
COj
Hydrocarbon! (DS)
c,
c,
C,
Ci
c«
Bentene
Toluene
Sulfur Specie* (DS)
HiS
COS
CH,SH
CilliSU
Other
NHi
HCN
TUSb
Streu Flow lata (Nai'/hr)
TUUS (NmVhrF 2
-
-
200
2900
91
1.6
0.7
1.9
0.9
3.2
2300
-
71
1.1
590
250
290
5.3
6700
40
.7E5
-
-
240
4100
80
1.6
0.4
0.4
0.4
1.1
-
-
110
1.9
910
750
NF
19
6200
400
2.5E6
Calculations ere baaed upon compoaltlon data
and DMEC valuta lluted In Table 5-1.
. All Component
TDS - X
1-1
a
(DS)
CTWDS - TDS • Flow Rate (AE8 - A
Xr - Hoc Found
TR • Trace
a 10B)
-
-
2.2
NF
7.0
TR
TR
TR
TR
TR
4700
1.1
190
HP
1400
690
110
14
7100
2
1.4E4
preaented In Tabli
-
-
170
NF
190
1.3
0.4
3.7
1.8
11.0
5800
22
1300
<2.5
2200
1300
-
-
11.000
50
5.5E5
s 5-4
13.6
Tar
Separation
Expn. Gaaea
-
-
130
2300
160
0.9
0.7
5.6
3.6
11.0
12.000
43
1200
-
2100
810
830
7.5
20.000
26
5.1E5
13.7
Phen. II 20
Tank Vent
-
-
4.3
NF
63
TR
TR
TR
TR
TR
19.000
65
190
NF
1500
1200
510
4.2
23.000
40
9.0E5
14.5
Stripper
Vent
-
-
TR
NF
72
TR
TR
TR
TR
NF
NF
NF
760
NF
330
83
2900
130
4300
400
1.7E6
7.1
HiS Vent
-
-
91
810
190
0.7
0.4
1.9
1.8
1.1
-
-
2300
3.5
9)00
2100
94
9.1
15.000
2500
3.7E7
7.2
C02 Vent
-
-
20
NF
200
0.7
0.7
T*
T«
NF
-
-
0.5
NF
18
9.7
0.2
1.4
250
5000
1.3E6
7.3
Rectleol
Inlet Cee
-
-
280
4100
72
1.5
0.9
3.7
0.7
2.1
700
-
470
0.5
1200
280
0.2
6.6
7100
-
-------
TAJJLE 5-3. ECOLOGY-BASED DS VALUES FOR KOSOVO "HIGH PRIORITY" ATMOSPHERIC
EMISSION STREAMS*
Compound
CO
Cj
Nil,
IICN
Calculations are ba
and DHEC values 11s
NF: Not found
TRi Trace
3.2
Lock Hopper
Low Pressure
970
7.500,000
15,000
1.7
3.6
Vent Cases
High Pressure
1400
7.500,000
NF
6.2
s£d upon composition data prei
ted in Table 5-1
•
13.1
Tar
Tank
Vent
NF
TR
5700
4.5
lented in
13.3
Medium
Oil
Tank Vent
NF
6,400,000
-
-
Table 5-4
13.6
Tar
Separation
Expn. Cases
750
4,300.000
43,000
2.4
13.7
Phen. II jO
Tank Vent
NF
TR
26.000
1.4
14.3
Stripper
Vent
HP
TR
150,000
41
7.1
II jS Vent
270
3,200,000
4900
2.9
7.3
7.2 Rtctlsol
CO] Vent Inlet Cti
NP 1400
3,200,000 7.500,000
11 a. 6
0.44 2.1
-------
TABLE 5-4. ANALYTICAL DATA FOR KOSOVO
SAMPLED DURING PHASE I
"HIGH PHIOR1TV" CASEOUS EMISSION STREAMS
Ul
Ln
Compound
Fixed Caaea (Vol. Z)
",
Oj
Hj
CIU
CO
C02
Hytlrocarbona (Vol. X)
C2
C)
c»
C5
c»
Benzene
Toluene
Sulfur Species (ppm)
HiS
COS
ClljSII
C21I5SI1
Others (g/100 Km')
Nil]
1ICN
3.2
Lock Hopper
Low Pressure
34.0
0.7
2.5
9.4
9.3
42.0
0.7
0.3
0.1
0.05
0.03
0.2
-
700
170
270
90
530
5.8
3.6
Vent Gasea
High Pressure
32.0
0.2
6.1
11.0
13.0
37.0,
0.7
0.2
0.02
0.02
0.01
-
-
1100
300
A 20
270
NF
21
13.1
Tar
Tank
Vent
TR
21.0
76.0
0.1
NF
3.2
TR
TR
TR
TR
TR
0.4
0.01
1900
NF
630
250
198
15.3
13.3
Medium
Oil
Tank Vent
NF
0.9
3.4
7.6
NF
86.0
0.6
0.2
0.2
0.1
0.1
0.5
0.2
13,000
<400
1000
480
.
-
13.6
Tar
Separation
Expn. Gases
11.0
0.5
0.6
6.1
7.2
72.0
0.4
0.3
0.3
0.2
0.1
1.0
0.4
12,000
-
950
290
1500
8.2
13.7
Phen. II20
Tank Vent
TR
13.0
53.0
0.2
NF
29.0
TR
TR
TR
TR
TR
1.6
0.6
1900
NF
680
420
920
4.6
14.5
Stripper
Vent
NF
9.0
58.0
TR
NF
32.0
TR
TR
TR
TR
NF
NF
NF
7500
NF
150
30
5300
140
7.1
HjS Vent
_
0.5
1.4
4.2
2.6
86.0
0.3
0.2
0.1
0.1
0.01
-
-
23,000
<560
4300
740
170
10
7.2
C02 Vent
0.8
0.1
0.3
0.9
NF
94.0
0.3
0.3
TR
TR
NF
-
-
4.6
0.5
8.5
3.5
0.4
1.5
7.3
Rectlsol
Inlet Gat
36.1
0.6
1.6
13.0
13.0
33.0
0.7
0.4
0.2
0.04
0.02
0.06
-
4700
80
570
100
0.3
7.3
Data from Campaign Three Test; November 1978
-------
• No information could be gathered on the
effects of normal variability or variabi-
lity due to abnormal, upset, or startup and
shutdown conditions.
In spite of these limitations, the Kosovo Phase I
test data provide a reasonable definition of the scope and
magnitude of the atmospheric emission problems which will need
to be addressed in a U.S. Lurgi plant. The results also pro-
vide strong justification for continued testing at Kosovo.
-------
5.2 Liquid Effluents, Liquid By-Products and Solid Wastes
During Phase I, the liquid and solid wastes from the
Kosovo facility were not generally examined to the same degree
of detail as were the air emissions. Nevertheless, some useful
data on these streams were gathered.
A summary of the major Kosovo plant liquid effluent,
liquid by-product and solid waste streams is presented in Table
5-5. Also indicated in the table are the liquid and solid
streams that were studied in Phase I and those that will be
studied in Phase II.
The major aqueous waste stream at Kosovo is the
Phenosolvan effluent water stream. According to the plant
design, this stream is to be treated in a biological oxidation
process, but this system was not in operation at the time of
testing.
Preliminary data obtained from a series of source
screening samples indicate that the Phenosolvan unit at Kosovo
is effective in recovering the phenols present in the raw
process gas liquor. However, as the data in Table 5-6 indicate
the organic loading in the effluent water from the Phenosolvan
unit is still substantial. The indicated phenol concentration
is not sufficient to account for the COD value obtained for
that stream. It is expected that the organic characterization
work scheduled for Phase II will identify more specifically the
potential environmental problems and control needs associated
with the Phenosolvan effluent water stream.
57
-------
Ui
co
TABLE 5-5. MAJOR SOURCES OF LIQUID EFFLUENTS, LIQUID BY-PRODUCTS
AND SOLID WASTES AT THE KOSOVO PLANT
Approximate Studied In To Be Studied in
Flow* Phase I Phase II
Aqueous Wastes
Phenosolvan Effluent
Fleissner Condensate
Generator Section Wastewater
Liquid By-Products
Tars, Oils, Gasoline
Phenols
NHi»OH
Solid Wastes
Gasifier Ash
Heavy Tar & Dust
Other Process Residues
13 MT/hr x x
Unknown x
3 MT/hr x x
0.8 MT/hr x x
0.1 MT/hr
0.2 MT/hr
2.7 MT/hr x x
0.1 MT/hr x x
Unknown x (By-Product Stor-
age Residues)
Design values; normalized to a one-gasifier-in-service basis.
-------
TABLE 5-6. KOSOVO WASTEWATER PROPERTIES (PHASE I DATA)
Fhenosolvan
Effluent Water
Gasifier Section
Wastewater
Units
pH
Susp. Solids
Diss. Solids
COD (K2Cr207)
Phenols
CN~
CNS
F~
N03
9.2-9.4
150-190
880-1300
3100-3300
170-270
.02
16-120
100-110
3
Trace
11-12
11.4-12.1
180-590
1100-2100
.8-150
.01 Max.
20-70
320-670
.01-.03
.6-1.2
4-6
mg/£
mg 0,i/
mg/£
mg/Jl
mg/£
mg/£
mg/A
59
-------
As shown previously (See Figure 2-5) , the gasification
section wastewater stream is a composite stream. It consists
primarily of ash quench water. However, small quantities of
coal bunker and ash lock vent gas scrubber blowdown liquid
are also discharged in this stream. This stream has a relatively
high pH because of the highly alkaline nature of the Kosovo ash
(See Table 5-6) .
A limited amount of data on the liquid by-product
streams was gathered during the Phase I test period. These
data are presented in Table 5-7.
One of the major points to be noted is that the sulfur
contents of the liquid by-products become progressively higher
in the "lighter" fractions. These data indicate that heavy
hydrocarbon by-products similar to those generated at Kosovo
might be used to satisfy on-site fuel needs of Lurgi plants
operated in the U.S.
The bulk of the work necessary to characterize the
liquid and solid wastes associated with the Kosovo plant will
be performed as part of the Phase II program. The program will
include the quantification of trace and minor components present
in all significant liquid and solid waste streams. Particular
attention will be directed to the leachable species in the
solid waste streams and soluble components in liquid effluents.
60
-------
TABLE 5-7. KOSOVO LIQUID BY-PRODUCT DATA
Feed Coal
(Dry)
C
H
N
S 1.1
Ash
0
HV* 21.6
S02** 510
Heavy Tar
+ Dust
56.0
7.6
0.87
0.33
6.6
28.6
26.5
120
Tar
81.9
8.4
1.3
0.49
0.22
7.8
37.3
130
Medium
Oil
81.2
8.9
1.0
0.71
0.03
8.2
38.3
190
Gasoline
85.7
9.8
0.2
2.2
-
2.1
41.6
530
*HV = Heat value expressed as KJ/g.
**Expressed as ng/J assuming 100% conversion of S to SOz.
S02 Emission Limitations for Utility Steam Generators (Ref. 4)
Solid Fuels 86-520 ng/J (0.2-1.2 lb/105 Btu)
Liquid Fuels 340 Ng/J (0.8 lb/106 Btu)
61
-------
5.3 Mass Balances
To determine the correlation between design and experi-
mental data, a series of mass balance calculations were performed
on the Kosovo gasification system. The first effort involved a
component balance around a single gasifier. The second effort
involved a sulfur balance which encompassed the gasification,
quench/cooling, tar/oil separation, Rectisol and Phenosolvan
sections. The primary bases used for these calculations were
the operational data obtained during the three sampling campaigns,
In cases where critical data gaps existed, design data were used.
A number of assumptions were made in the execution of
mass balance calculations. The assumptions made and a summary
of the calculated results are presented in Appendix C.
Table 5-8 contains a summary of the results of mass
balance calculations normalized to a single Kosovo gasifier in
operation. A summary of the results of sulfur mass balance
calculations is given in Table 5-9.
An examination of the tables shows that reasonable
accountability was observed for all of the major components
considered. The number of assumptions necessary to these calcu-
lations limits the usefulness of the results. Nevertheless,
the results imply that no serious errors exist in any of the
data used in the calculations.
62
-------
TABLE 5-8. MASS BALANCE ACROSS THE LURGI
GASIFIER AT KOSOVO *
Component
S
C
H
N
0
Input
(kg/hr)
179
6500
2354
442.5
19,189
Output
(kg/hr)
140.5
7091
2635.9
367
22,446.8
Percent
Accountability
78.5
109
112
86.8
117
*Mass balances are normalized to one gasifier in operation.
TABLE 5-9. SULFUR BALANCE ACROSS LURGI
GASIFICATION FACILITY AT KOSOVO
Section(s)
Gasification, Quench ,
Cooling And Tar
Separation
Rectisol
Phenosolvan
Input
(kg/hr)
142
114
•k
Output
(kg/hr)
128.9
92
3.3
Percent
Accountability
91
81
*
*- Flow rate and composition unknown. This stream will be sampled
during Phase II.
63
-------
5 .4 Discussion of Results and Recommendations for
Future Testing
Based upon the results of the Phase I test program,
it is recommended that future testing at the Kosovo facility
focus on the following areas:
• more comprehensive characterization of
solid and liquid waste streams,
• detailed analyses for trace organic and
trace elements in high priority waste
streams, and
• evaluations of control options for high
priority waste streams.
The specific nature of the data needed in each of these areas
is summarized in Table 5-10.
During Phase I, the solid and liquid waste streams
from the Kosovo plant generally were not examined to the same
degree of detail as were the gaseous streams. In Phase II, the
solid and liquid streams which have the potential for causing
significant environmental problems will be evaluated.
Gasifier ash should be carefully evaluated with
respect to recently published RCRA guidelines (Ref. 5). This
attention is justified primarily by the size of this stream
(2.7 MT/hr of dry ash from each Kosovo gasifier.)
64
-------
TABLX 5-10. KOSOVO UASTK STKKAMS alNKRAL SL->?1AKTf
OF ADDITIONAL DATA NEKDS
Screan Type
Description
Flow fute
1. Solid Wastes C4*Ultacu;* of arfli Iviil
1C b* cLjsstlHed js a lu'jrdous vasce?)
Sanw js for jsh <*xc«»pc ^ i--o evaluactf the env 1-
ronmental ispaccs of disposal opcions och?r
Chan landi'UL (e.g., tnclnerac Ion)
2. Liquid Wastes
3. Liquid By-
Products
4. Recclaol
Process
Vent Cues
S. mv Generator
Vent Gases
6. Slch Ezpanslcm
Oases
Process Condensace:
Fletssner
Phenosolvan
Ash Quench Water
Tars/Oils/CasolLse
Phenols
NH.OB
HiS-Rich flash Cases
COj-Sich Vent
Unknown
13 Kl/hr
3 MT/hr
0.8 MT/hr
0.1 MT/hr
0.2 MT/hr
2500 Nm'/hr
2200 Nm'/hr
Coal Lock System Vents 400 Hm'/hr
Generator Scare-Up Unknovn
Vent
Drying:
Fleissner Auto—
clave Vent
G&slficatlon:
Liquor Tant Veot
U-aknovn
40 Km'/hr
Tar Separation:
Separator-Flash Cases 26 Nm'/hr
Additional physical and chemical characterization
data2
Evaluate treatment, reuse, disposal options
Additional physical and chemical characterization
data:
Evaluate utilization options
Additional physical and chemical characterization
data:
Assess needs/options for further treatment
Additional physical and chemical characterization
data:
Assess collection and treatment options
Need comprehensive physical and cheoical data for
screening purposes
Additional physical and chemical characterization
Tank Veat£
Ph«aoeolvaa:
Strlpp«r Vents
7. Storage All Liquid By-
T««ir Vents Products
3. Air and 02- Coal Eandllng
Rich Vents System Vents:
with Fleiasner
Particulates Coal Handling,
Crushing, Sizing
Gasification
Ash Lock System Vent
•V20 Sa'/hr
i-lOO No'/hr
Small compared
to streams
listed under
itea 6
Unknown
Unknown
3600 Nm'/hr
28 Nm'/hr
data'
Assess collection and treatment options
Additional physical and chemical characterization
data2
Assess collection and treatment options
Additional physical and chemical characterization
data with emphasis on particulates. Other co«-
ponents of potential interest include:
Coal Devolatilizatioo Products
Raw gas components?
Additional physical and chemical characterization
data with emphasis on particulates
'Per gasifier.
'With enphasis on components not adequately addressed in the Phase I program (e.g., trace organics and trace
elements). Attention should also be focused on the variability of key scream flow rates and pollutant
concentrations during periods of oonaal operation as well aa during startup/shutdown and upset periods.
65
-------
Heavy tar and dust as well as a variety of other solid
process residues are currently landfilled at Kosovo. Because
these streams probably contain significant quantities of harmful
organic components, landfill would not be environmentally
acceptable in the U.S. Combustion of these residues in an in-
cinerator or process heater to recover the energy available in
the combustible residues is one control option. The acceptabi-
lity of this approach must be confirmed with respect to the
fates of hazardous trace species during combustion.
Additional data needed to properly characterize the
Kosovo liquid by-products closely parallels that outlined for
combustible solid residues. One of the more promising disposal
options for some of these materials is combustion in on-site
steam generators, but the fate of hazardous trace species during
combustion of the liquid by-products is of concern. Therefore,
emphasis in Phase II should be placed upon characterizing liquid
by-products.
The Kosovo Rectisol unit should receive considerable
attention in the Phase II program. Since this unit is the
source of two of the plant's most significant gaseous waste
streams its operation is critical to the overall air quality
impact of the plant. The presence of residual sulfur species
and light hydrocarbons in the C02-rich vent stream is of parti-
cular concern. This stream may be the source of significant
hazardous pollutant emissions from the plant, particularly
during upset conditions.
66
-------
The H2S-rich gas stream from the Kosovo Rectisol unit
should be examined in detail during Phase II. Emphasis should
be directed toward components such as COS, mercaptans, and light
hydrocarbons which might cause problems in a downstream sulfur
recovery process .
Several significant gaseous emission sources identified
in the Phase I program should be studied further during Phase
II. The most significant sources are the Phenosolvan condensate
stripper vents, the surge tank vents in the tar separation
section, and the lock hopper vent gases.
67
-------
REFERENCES
1. Lentzen, D. E., D. E. Wagoner, E. D. Estes, and W. F.
Gutknecht, IERL-RTP Procedures Manual: Lf^g1 I ^nyj-ron"
mental Assessment (Second Edition). EPA-600-7-78-201.
Research Triangle Institute, Research Triangle Park, NC,
October 1978.
2. Schalit, L. M. and K. J. Wolfe, SAM/1A: A Rapid Screening
Method for Environmental Assessment of Fossil Energy Process
Effluent's"! EPA-600-7-78-015. Acurex Corporation/Energy
and Environmental Division, Mountain View, CA, February 1978
3. Cleland, J. G. and G. L. Kingsbury, Multimedia Environmental
Goals for Environmental Assessment, Volumes I and II.
EPA-600-7-77-136a & b.RTI, Research Triangle Park, NC,
November 1977.
4. Environmental Protection Agency, Standards of Performance
for Electric Utility Steam Generating Units for Which
Construction is Commenced After September 18, 1978.
(40 CFR 60.432) Revised as of July 1, 1979.
5. Environmental Protection Agency, Hazardous Waste: Proposed
Guidelines and Regulations and Proposal on Identification
and Listing.(40 CFR 250) Federal Register, Volume 43,
No. 243, Monday, December 18, 1978.
6. Salja, Becir, Mira Mitrovic, and Dragon Petkovic, Environ-
mental and Engineering Evaluation of Kosovo Coal Gasitica-
tion Plant, Yugoslavia (Phase I), Symposium on Environ-
mental Aspects of Fuel Conversion Technology, IV, Hollywood,
Florida, April 17-20, 1979.
63
-------
APPENDICES
APPENDIX A
PHASE I DATA SUMMARY TABLES
FOR GASES
The following tables contain summaries of the raw
Phase I test data as reported by Rudarski Institute. Comments
related to data quality which are based upon Radian's observa-
tions of the plant's operation are also included.
A-l
-------
GENERAL NOTES ON ESTIMATED DETECTION LIMITS
OF SAMPLING/ANALYTICAL METHODS
Fixed Gases
NF - not found; <0.1 vol. % (Orsat)
<0.01 vol. % (GC)
T - trace; -vO.l vol. % (Orsat)
0,0.01 vol. % (GC)
Hydrocarbons
NF - not found; <1 ppm ( .0001 vol. %)
T - trace; '^1 ppm
Sulfur Species
NF - not found; <0.1 ppm
T - trace; '^0.1 ppm
Impinger Measurements
H2S NF - not found; <1 ppm
T - trace; 'V-l ppm
NHa NF - not found; <1 ppm
T - trace; '^1 ppm
HCN NF - not found; <1 ppm
T - trace; ^1 ppm
Phenol NF - not found; <1 ppm
T - trace; ^1 ppm
A-2
-------
PHASE I TEST DATA F06 SAMPLE POIWT 2.2
2a«
Jlow Jata, Hm3/hr
Particulate, g/NmJ
Moisture, I Volume
leaperarura, *C
1
c
i
en
w
g
X
iZ
g.
-^
I
g
X
Jl
i
!
o
a
™
3§
^
1 i:
5
J
i
w
K
Z
r
r
Method
Hz
0:
Si
ca.
CO
COj
Add Gases
Sat. HC
Dn&ae. SC
Ci
Ci
c»
3
c*
Ct
RvntAna
Toluene
H2S
COS
CH,SH
c a,sa
so
X
H2S
SH,
HOJ
Pheaol
Camp^jn I
HI
S£
Orvit
NF
20.4
79.4
NF
T
a3
NF
RI
1977
O^i
0.8
20.4
73.7
NF
O.I
NF
NF
Hf
two
MM 10
1377
*•*
NF
NF
Campai'im T£
RI Kosovo
J,^f July I97S
T 1,000
0.04b
tA-
1
NF
10. .r
T
NF
1.2
T
RL
-------
PHASE I TEST DATA =OR SAMPLE POiMT 3.
Oaca
Flow .=Uce, SmVhr
Particulars, g/Na:
Moisture, Z Volume
Teaperature , *C
a!
3
|
3
X
'*
CJ
3
o
M
1
2
a;
0
G
"•
VI
i§
il
3
VI
a
7
VI
-
JJaehod
H2
02
CH»
CO
CO J
Acid Cases
Sac. SC
Unsac. EC
<=»
Cj
c.
Cs
C«
Senzene
Toluece
HjS
COS
C3jSH
C23SSH
SO^
HjS
MH,
ac.
Pbeaol
c^^'jr/7 r
K-L
S&p+ 1977
O^t
1.3
17.6
7.. 3
0.4
2.4
0.4
,VF
C.j,«/M£yyr5 /,vor£3
S&mplina impossible, in Campa-i'^ns H
A-4
-------
PHASE I TEST DATA POR SAMPLE PO/MT
3.2.
, Dace
Flo» Sate, SaJ/hr
P»rtieulace, g/Na1
MolscuTttt * 7oluoe
Tesperitura. 'C
ed
1
«
i
a
X
^
|
i
3
M
I
Z
O
a
|
=
VI
ui
§g
SULFUR SI
ppnv
a
p
z
x
Method
Es
Oj
Sj
CO
COj
.Acid Gists
3ac. EC
Uoiac. HC
C2
C,
c.
Cj
c«
Benzene
Toluene
Has
COS
CHjSH
HjS
NS,
HQJ
Phenol
Rl
t^7
»u»
(4.2
12.9
50.3
4.0
13.5
4.i
MF
440
C*mpa.-9n I
RI
Nov 1
1917
Oridt
li.4
44.2
3.3
17.3
5.'e
0.4
RI
1977
-------
a J. T£ST DATA
Dace
Tlow Race, Nm: /hr
Particulace, g/Nm3
Xoisture, I Volune
Temperature, *C
3
0
i
•J3
<
X
^
1
o
M
1
U5
2
O
=
VI
kJ O
" >
! *
V)
3
7
^
=
Method
H:
Ot
Hz
ca.
CO
COs
Acid Cases
Sac. EC
Unsac . HC
Cj
C»
Cj
C8
Benzene
Toluene
Hj5
COS
CHjSH
C2Hs5H
^
a,s
SH,
aa
Pheaol
Ca.mpa.ian I CCMMS.fJTS //V OTBS
Rl
Mew 1
er
Mov 3
1917
0^
11.8
13.3
Si.fe
2.fc
12. a
3.0
0.4
1
1 400 1 3CO
«I
K.so.o|^Mva
M av 10 1977 | °^
^rsd.t
10.2
490
T
0.4
320
99
9.5
7
•* — bt °"^
A-6
-------
t. Z T£ST DA-TA FOK SAMPLE POIVT
Date
Flov Rate, NnVhr
Paniculate, g/Ne'
voisture, I Voluae
Temperature, "C
I VOLUME
XEI> OASES -
to.
U
a:
s
1
in
I
o
C
""
en
as
M
eC 5
3
i
i
w
a
z
X
Method
Ej
Oj
S2
CEi.
CO
COj
Add Gases
Sat. HC
Uajsat. HC
C2
C,
C.
c»
c(
c..
ene
Toluene
H2S
COS
CH,SH
C2BSSH
H2S
KB,
ECS
Phenol
£««/«^ r
^r
/977
^
NF
20. fc
79.0
0.4
A/F
A/^
A/F
/ei
Nw 1
Or^
H?
20.5
79.3
0.2
HF
A/F
A/F
«r
Vev 3
^
1.0
22.8
75. «
WF
A/F
0.4
A/F
A/F
/«!
/Vav // /?77
^•l
7.5
NF
^t
^
/VF
0.5
^1M»0
Da
/977
Cajnpa.iqn 7J"
1978
i.'.l
51.4
10
j
f.fcc',
A/P
•T&
Ife
—
]N£P
5C
I8.9
79.4
,.2
0.004
ta
ItoSMtt
July 1973
M
300
r
fi
300
"
KI
fefl«
Sept- I97g
W^
/30
A/f
/30
271
/978
SZ
340
54
Hovii
i
:' w. O
31.3
6C
T
A/P
r
T
r
T
WF
UF
Ui-
Nh
A/'ov /9
. --
V..&
1&
^j^^£>rs//v^r£S
1 P^-y &
-------
I TEST DATA FOR. CAMPLE Po/nJT 3.(,
Date
Flov Ract, NaVhr
Paniculate, g/Sm3
Moisture, 1 Voluw
Teaperature, *C
FIXED CASF.S - % VOLUME
IIVUROCARBONS - 1 VOLUHK (CC)
SUI.KUR SPECIES
ppmv (GC)
IMPINCERS - ppmv
Method
Os
Nz
CEi,
CO
C02
Acid Gases
Sat. HC
Ensat. HC
Cz
C,
C.
C5
=«*
Benzene
Toluene
HjS
COS
CjHsSH
S0x
HjS
NHj
HO)
Phenol
C*w'f« x
zt
SzpT
1977
Orsif
2.4
0.2
3.2
1.0
84.8
8.2
0.2
12000
£1
NJov 1
1977
**
4.4
0.4
3.4
3.4
SS.t
MF
izooo
RZ
1977
0^
37.0-
37.2
0.2-
0.3
4.6-
11.7
8.0-
12.S
J4.8-
9^4
0.9-
1.2
Z800
/er
Mov II
1977
340
ZI
^WVC,
Nw 25 '977
NF
Orsai
31-4-
0.4
Mean
Cec.
-
Canp^gn TL
\ TN£.P\ KI
0.19
iO
GC
7.8
30.8
4.8
4.0
4.8
2.7
4.2
0.08
O.U
0.09
tdxfvo
Ju/y /975
-
te
1600
76
avV
AS'.ftJ
7i
/?r
S*f
kaevo\
H976
Na.V,o
3200
"> 1
/30
Campaign
ur
W%7/
400
/. / r -
54
6C
0.23
6.07
II. 0
IZ.1
37.3
0.11
0.2.1
O.OZ
0.02
0.01
o.os
300
420
270
2.400
NF
no
COMMENTS /
NOTES
' Dry 1*3 tlouj
^'J kncutn °^/
fai <^i^i •sw)
-/3^«"'
-2J ppm
A-3
-------
^
7 /
1
Dice
Flow Race, SmVhr
?ar^icuiace, g/NmJ
.Moiscure, Z Voiuae
Teaperacure, °C
3
*
1
3
2
SJ
X
~
^
^j
M
Z
o
c;
1
in
^ u
si S
£l. £.
.J
3
1
1
«
Z
Method
a2
Oj
H,
ca*
CO
COi
Acid Gases
Sac. EC
Uosar. HC
Cj
Ci
c.
C5
::_
Saazene
Toluene
Ht 5
COS
CH5SH
cza,sa
»*
azs
SH,
aoi
Phenol
C
,?-
St>r
GILSAT
I.I.
^f
a.i
/.?
f.L
0.1.
«...
\~>.,^ - ' - 1 (a,*.
*•<* „•„
n
"f
c^
».*
"
J4.e
^
lfj(f | r«|
V*7o
7J"?
t
, ^ ...
^«c
: w
1
A-9
-------
?HASE x TEST CATA "CR SAMPLE PO/AJT r.2.
Dace
Flcv !Uca, SmVbr
Paniculate, g/Nm:
Hoiscure, * Voluma
Teoperacure, "C
iJ
£
O
^
1
V)
V\
3
X
'•*•
£
"-"
1
o
X
z
i
OS
o
H
"™
M
11
* i
=1 C.
fa a.
=
3
Q.
&
I
•J\
5
z
™
2
Medjod
Hj
Oi
Sz
ca.
CO
COi
Acid Gases
Sac. HC
Onaac. HC
Cl
Cj
c»
Cs
C,
C4i
Senzene
Toluene
H:S
COS
CH,SH
Z 5
S0*
a;s
NH,
HCT
Phenol
Citt?AlG,W T
_ , , I
i i 3
*X
*
OirscrV
GC
HP-
1
1
HP
9S-.3 j S?->
9.4
W
97.0
3.4-
Wp
1
j
140
HF
/VP
1
i
i
93. 5-
0 7-
Nr
o rs
1
;. r
/ s
1
V —
1*.fc
1
2.1=1
o.rr
MF
N?
N?
UIL
A/P
WP
M£
>J TT
<"O5DVO '
,W ;
1
j
I
°°f
H,
A/f=
N^
^ P-
"*"
HL .vorss
.V.v, ti-i
I408tti 5 3«.n«.ra.-TO«
i
f "^i^
T
r
Hf
Hf
A- O
T
s.r
3.S"
3s?
46>
'3
Cas V4,_S)
-4;^,
A-10
-------
7.3
C-* SnOA'QI -li.
Xosovo I TTI " '
3aca
Flow Sae«, SaJ;hr
?»r=tcul4«, g/Na1
Moisture, * Volume
?«*«,««. 'C
W
Z
o
*
1
«
o
a
=
•j
1
o
^
1
5
3
5
^
3
11
w >
1 '
yj
a
1
VI
UJ
M
7"
r
Machod
«
0^
Si
CH»
CO
COj
Acid G^ses
Sac. EC
Dnsac. SC
Cz
C,
C.
Cs
C4
C,.
Benzene
Toluene
HjS
COS
ca3sa
C23sSH
3O
X
3lS
SH)
HCT
Pieaol
'
; ,Vov 24
!! ! .'978 '
^«wx-
m«nr» of
i.rerm,^-
7^''~r
i
1
1
I
1
1 \ \
LS1 ' ^ '
! 20
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39.3 ' . 3C. 1
i ;
C.2. ': C.55
: ' i
; 0. 9 ' 1 . 55 '
1 '
: ' /2.S
II. i j i 13.5 j
' i ! 33. •V
37.2! '
; 9.9 i
i 3.4: ! |
l.'i- I ; i o.i5
0.35" i 0.3S
0. 20 1 i i 0.16
0.02. ] 0.04
; \ 0.021
1 i i
; : 4470 i
Sio
1
i i
;78coi f^co ~^co
2.1 NP 3.3
60
-r -
A-L1
-------
TE5T DATA
SAMPLE. Po I AJT 7.4
Date
n.ov Rate, Nn'/br
?»rticul*te, g/N»J
Moisture, Z Volrae
Temperature, *C
=
c
'
1
u)
X
u.
1
Ed
M
W
1
|
=
i?
EC 1
i
2
1
w
a:
i
Method
a,
0:
S:
CEk
CO
CO;
Acid Cases
Sat. EC
Unta t . EC
Cj
Cj
ck
Cs
C4
Beczene
Toluene
HjS
COS
CS|SB
CjBsSH
s0*
S2S
SB i
HCN
Phenol
Ca*>p*iy» I
KMO*
*77
firs-t
66.3
0./
/.2
/5.S
3.0
/3.t
0.1
Kcv»
&WO
/Vov3 (977
O^t
66.5
a/
1.0
li.S
!• (e
14.0
0.3
Cnii
U.I
O.I
1.5
lt.S
2.0
13.6
0.3
^
Kfffie
Hov 9
fill
Orttt
66.5
0.1
0.5
tb.9
Z..I
13.L
0.3
I
Nm 10
/977
Onat
te.o
O.i
1.5
li.S
Z.&
13.1
0.3
Wtw //
Crud.
65.9
0.2
0.9
H»9
2.4-
/3.7
0.3
Cc*
TNiP
c-c
tit
/.fe
Z.6
/5-.T
a 2
2..t
NF
NP
NP
HO
^;?« z
/el
Ka«vo
OrSft
62.4
O.I
a.l
17.3
2.6
/&.!
0.4
NF
UF
NF
MF
/VF
/V^
/>//=•
NP
HL
Ho* Ik
tc
(.0.1
O.trO
4.64
«.9
/«.«
T
7
//A
NF
Z
r
/JF
T
r
H«,/9,ng
GC.
63.2
/.4
6.77
12.3
15.9
V?
0.42
0.006
NF
NF
0.0 1
1.2
fJF
T
r
GC
63.9
/.73
£«7
//.9
/4.33
NF
0.75
A/P
/(//=•
5.i52
0.02
1.0
fJF-
T
T
UevZ*
Iflt
GC
62.2
0.1
Z.O
n.u\
17.1
0.1
O.V)
0.0Z
T
r
1.4
tit
1.0
T
COMME.MTS / MOT&S
A-12
-------
A
Dace
rlov Race, HmVhr
?artieulace, g/No3
Moisture, I Voluae
Temperature, 9C
|
*
1
VI
IT)
•*•
'J
~
§
«
z
aC
i
•-J LJ
iJ y
SULFUU SI
P|IMV
s
a
VI
X
z
Method
CA*..,^ r
fr ti (Tcio.o &*,<„
•SfiT
V., ^ /,„
^re.
' \
OttJtr QLS*T
3* /./ !
Oi
Si
C3»
CO
COj
Acid Cases
Sac. 3C
u=sac. SC
Cj
Cj
c.
Cj
c«
c..
Toluene
HjS
COS
C2H,SH
H23
SH,
HCS
Phenol
ff.l
l».i
0.3
i.o
C.L.
"
Jo~>
..,
1
i
3"!
NP
o.C
i
I
!
i
'
/6
-------
ru
/Wr /3. i.
1
-------
c I. TEST DATA FOR
LE POlWi
r
Dace
rlov Race, HnVhr
Paniculate, g/Nm1
Xoiscure, * Volume
Temperature, "C
z
H
V5
|
3
>^
z.
a
I
^
3
=
10
r £
3 ?
3
3
in
aS
7S
Z
Method
32
Oi
Si
ca.
CO
COz
Aj;id Gase^
Sac. SC
unsat. HC
C2
Cj
c*
C5
c<
*
Benzene
Toluene
ass
cos
CHjSH
r
HO
Phenol
r
CAMPAl&N X
CAMPAVGAJ 11
R.*^. 1 S.X co^ovjoito^oMoi 51. INEP W i
i COMMSWT3 , .UOTSS
J-i
^SS™i
5i . \ i ' " ' **• i^'^ _ *•'
1
CM.O c«+,^«)
4-8 : '
GC
AlP
C.99 !
3 .36.
1 6.4-
,VF
SJ..4-
ll ' ' • '
'
; *.*
[
•i
I
O.-tZ. |
[ o. 3> i
j 0.31.
3.4-1
?42!
o'f'j
,
1
'
! 1
40
AVP
12.
i
I
[3+000 'Jzooo
U 1 ooo i 54 coc
r.3 •!•:?-
-r | T
O.G.2. i
O.fO
O.08
O.C9
1
i
1
1
0 49
0 i r-
I Z.
-------
PHASE r TEST DATA
e POINT 13.4-
Daca
Flow 3j.ca, Sn'/hr
Particulace, g/Nm1
Moiscura, I Voluae
Teaperacure, "C
i
5
1
V.
V)
a
X
£
s
X
VI
a:
I
=
•ii
a. --*•
VI
as a
z» a.
u. &
3
=
t
g
z
Method
Sz
02
MI
ca.
CO
COz
Acid Gases
Sac. EC
Onsac. 3C
Cj
c.
c,
c,
Benzene
Toluene
H2S
COS
CHjSH
HjS
HH,
Eca
Phenol
CAMPAISW 1
i- ' ' ^T ]
S«pT I9^T" ' ' ; ,-„.. , ai~
\
0^
COWA/IEMT5 / :\JOTES
r.,s ^r O^^fJ ^
7^ ' ^5 <^L^ r / V e"(, •/ — Ji^ /* uCtij <'1 ^-
j
O«-s«-V ; O-so-+
A.P
;*.z
15". 2.
*f.O
fif
<". 0
O. j>
A)F
' i
i
,Vr
5*.0
(yp
o.r
If 00
1.4-
/ 0
/so
340
!
,VP
•VP
^
A-16
-------
PHASE I
±.-31 \_/ f
'A "OR.
E PO;AJ~T
\
Data
CAiWP
si :to«o«o|
Se?^ ' Aiov ;,'
^7=t i /=I7?
Flow Sate, Mm3 /Sir
Particulata, g/Nm!
Moisture, I Volume
Temperature, *C
s
o
=.
w
'
•3
V3
2
X
=-
£
5
^
g
M
«
z
X
1
>.
=
l§
>
2 §
p
a
i
VI
%
0
r
±
Method
Hi
0:
Sz
CS*
CO
COt
Acid Cases
Sac. HC
Unsat. ac
C2
cs
c.
c,
C4
c«.
Benzene
Toluene
H2S
COS
CHjSH
C2a53H
H23
'
2Ci
Phenol
i
i !
, j
j j
1
0'«=+ 0<,a+|
ifr Z- i
12 a
+1 a
3.(> |
i ;
j
IZ i II. 0
*.'->
\
0.3 1.2.
I
\
i
i
i
!
i
MS*
C-SOVO
Uov R
If ?T
I
Z4eo
331
I
KI !
Mov Z"
1=55 '
i
]
i
M>
1"-
.OSOUOI ^^
-1
" a"* ' ' J t
'l
]
1
•
IA PAIG
iwe?
.\c 1 ^
i
O.JO
U.JI
o 27
! ° '-
o.oo
'
VJ H
C AM P A i G(^ C2*l*l£,vTS /
| _; • ; .VoTS-5
^ S Vo\y Z 3 / ? T 8 '
1 ^ ' i - -^-^,
i V^-Vr "
i
i
, / . . \
!^i • ^ ) \ - ^a
i *
•i
: Gc :
1
!
j ;
/' 4 6>
/6 .LP
^ / O
/ / ^
,i
! 1
;| .V f
\ j
. :
1
! I
ll !
: 1
i
i
j
>i
i
1
! i
/f 3
tjZO
-=?0
1/3 ! T.Z
c.o^
O.O-T i
0 03 i
0.04-
003
0 5"2
o 30
3 (ff Z.
HCi i H°.M^'(ltMI
Zl?
_'*''* "* .
.0-,,'../
i^O 0
'^ 1
/ rO
i
A-17
-------
PHASE I TEST DATA = O P. t>Art\f>t-S. POINT !
Dace
Flow Sate, SoVhr
Jarticulace, g/Na:
Moisture, ' Volume
teaperacure, *C
1
i
w
1
12
3
«
2
X
"*•
§
**"'
1
o
«
V3
1
X
1
=
£§
_ ^
M >
3 =.
j. 2.
5
1
2"
!
S
z
X
Method
32
o2
s,
ca.
CO
COj
Acid Cases
Sac. SC
Hnsac. EC
Cj
Ci
C.
Cs
c«
c,.
Benzene
Toluene
H2S
COS
CH3SB
CiHjSH
sox
H23
NH,
HCN
Phenol
CAMPAI&W I 1 CAiWPAldM XI !] r \ , ««ie«Ts /
RI !so»oviol«iic\;o eoaovo RX
lA/e?
tosowi TTT ,vorss
*^;T1Ai7^ JiT«; Ou"e |i:|>9
;
i
Orta* io^j +i J
*ff.*l i
O.(t
s.r !
•T. o
1
rz £0
0.3
10 OOO
»2 at
, j
a.f '
i
5700
£••
7"
!
Uou 5 3 ."?5a
1 1
!
3c !
i i
i
: ;/ i ':
II :
!
0 4r !
i !
t : i
i
i cr
zsoo
;; o oo
C.toi
O.Tt.
o./f
o.lf
19 g OO
430
._ , i
3330
40* i
r IT'
•* z i
1
jl
0.* ;
<5 33
0.2? ;
i
o./s- !
o.os
C.9S-
;3 ooo
/(i,CCO
300
1 O
/o
1
o.*o i
,5 oo^
A/Q ; iVa - ,Vo+
4:?-
298
1 4" GOO
"Z. C? OO O
63 j
i
A-18
-------
= HAS£ Z TEST C AT A FOR, SAAAPl-E PCIM"
CAM PA\ GM T
Dace
n.ov Race, Sm'/hr
Particulace, g/Na3
Moiscure, I Voluae
Teaparacure , *C
I
5
I
2
<
%
=
^
-
O
«
2
a;
|
=
PI
» a
p c.
3
a
t
cfl
1
=
Method
5a^. , '%|.[ . 'V^7'J' • -(»- ^
i ;
1
i
0-,*+ o,«-r
Hz
Oj
Sj
C3»
CO
CO,
Acid Gases
Sac. SC
Dnsac. HC
Cz
Cj
C»
Cs
C«
c**
Benzene
Toluene
3z3
COS
CHiSH
2
*°x
HzS
KB,
ECS
Pheaol
Hf •
(3.0
r3.^
^
t
3,3.0 ; 3* 2.
0 -4- i
Hf Z.Z. \
|
|
! |
i !
1
j
j
|
!
?00
I
i
[
t
I
^r
!
o.ot
0.08
O.OS"
AJ ^"
^Jr
ITJ OOO I
9 too
34-
» l^rS.«.' I
33. z' 'j i-c~»/nr5«-
1 Ci* 3) ^^.^crrca)
i 1C,
; O.C
|
i
-r
IS i
-="- T
0 2.
,V? '
-/ 1 i
1
1
o at-
t
'
!«co
0-0 1 i
o.oi"
0.01 \
i
c.os
i
I
/ . i /
0. i.0 |
! 33O i
I
A/r !
i
;z 300 !
sa '
i
A-19
-------
E I TEST DATA FCR SAMPLE PCI.MT 14-. /
Dace
Flow Site, XmVbr
'articulate, g/Nm!
Moisture, I Volume
temperature, *C
i
..
§
§
W
1
-ji
;j
<
o
Id
X
*
u
"•"
1
2
i
M
en
\
*
a
=
II
5 >
3 3.
s
3
t
p
2
^
£
Method
a,
02
Si
CH»
CO
COj
Acid Gases
Sac. 3C
Onsac. ac
Cz
Cj
C,
Cj
C,
cs
3enzene
Toluene
COS
CHj33
CjHsSH
SH,
aci
Phenol
ca«Pfti&N I !
! -OM/WE.VTS ' ,UOTES
RX X.O5OMO ;
A/ov Z3 l^fT ^ASfOufAr C*"fA**i* but
T, t-n &L*r,<,r^ ^^ fuxJ
1
1 Oria-f
: 1
i
i i
I
; IZ Z.
0. 4-
!
I
i
1
I
1
/ 1
(V P
I
2. 1 OO
A-20
-------
PHASE
= ST P AT A FoR SAMPLE PoiMT i4.Z
Date
rlov SLate, HnVhr
Paniculate, g/NmJ
Moisture, I 7oluae
Tenperacure , *C
o
bl
X
b
CJ
-
O
«
tn
a;
1
E
|c
i. ^-
a: 3
P —
p
a
2.
C.
1
•z
Method
Hj
Oj
Hz
CO
COj
Acid Gases
Sat. HC
(Jusat. HC
C2
cs
C>
Cs
c«
C4i
Benzene
Toluene
HtS
COS
CH,SH
H2S
NH,
aca
Phenol
CAMP Al& A) i
RX KC5c\yo |
1
i
COMETS /.VCTBS
3;f,,rt££:^v
Or,^ 0,,a*
I.Z.
(9.3
5-4 4-
A/F
!.«.
i
i
i
i
i
i
i.o.
/ 0
1
N P °-Z-
4-30
S"40
A-21
-------
PHASE X TEST DATA TOR SAWPLS. POirtT I-4-.3
Date
Flow Rata, NnVhr
Particulars, g/Ntn!
Moisture, " Volume
Temperature, °C
s
g
'
wl
O
3
i
§
a
en
as
I
—
3 u
3- '^
1 i:
5
a
i
IMI'INCERS
Method
as
Oi
HI
CH»
CO
C02
Acid Gases
Sat. 3C
Uasat. ac
Cj
Cj
c»
Cs
Ct
Benzene
Toluene
Bj3
COS
CHjSH
c2H,sa
S0x
azs
3d
Phenol
CArWPAl6N I.
KX. . RX
^-e.vi/wguTS , .UCTSS
f , 10^1. ',i -7 A. iQ 33, . *7># / i rfa/d'f u£ 6#P€ 4 /**
^ < ^T / T T T i rJOV i **" IT T"T / <"• ' «• ^
7-0 /rj ^«r , 4y 6
:
A/P
2.0. 3 ;
78 6» i
«P
1
O . ^
/VP
.VP
1
1 '
I
i
1
1
1
NC
„
I
A-22
-------
T /fs-r
Date
Flov lUce, Hm!/hr
?articulace, g/tin'
Moisture, " 7oluoe
Tentp«ratur«, "C
z:
>
v;
|
2
x;
^
^
a
3
«
V)
Z
O
=
11
- i
3
a
3.
3i
•jl
Z
Method
az
02
Hz
CHi,
CO
CO,
Acid Gases
Sat. EC
Cosat. EC
C:
Cj
C.
Cs
C4
Benzene
Toluena
HjS
COS
CHjSH
CjHjSH
r
aa
Phenol
SI J.
2 1
5f?r
0«*r
o.i
J.0.0
11. i
^
1.4
/. o
^
"
.-
!
0**r
\
-0.7 j
J. ^ i
1
V.T
A-23
-------
At -i"
Dace
Flov tece, Sa3/hr
Parrieulace, g/Nm1
Stoiscure, Z 7oluae
Temperature, *C
1
3
M
i
cn
«
y
a
X
'•*•
s
-.^
§
X
1
en
i
a
•™
1§
^ i
1 £
V3
a
I;
-
si
'j
2
Method
Hj
02
S:
C2»
CO
COj
Acid Gases
Sac. 3C
Uosac. HC
Cz
C3
C,
C5
c.
3enzene
Toluene
HiS
COS
CHjSH
C2H5SH
30
X
H2S
MH,
ao!
Phenol
^»* r
«.- X.JM,.. t- i
-•;•/
«»,
?» C
^ ^_
1 ("jam*
I '
.^,,
*~
/"» '-
vf^ - t ' • •*«* /7
».,, i
v.
jv=«
4?
r
Uu/JC ill! i -J7f •
:
1
i
|
-
'
y.j !
^•2 !
i
/l/" ,
,V^ '
» u'
1
! |
^:r
i
i
,«?
flf
-,
«.w 2T ^-^^f.jrj l^irt;
•••tf .
+•*' ', 7rL^"r°"*
^ j
- i
ve.
:Jf
? -'
/ J
~~
.4?
J-t.-?
T
T
r
r
tir
?j"'S
/Vr'
/rc
.53
I
i
1
I
|
1
* V :'tfJ : ^; ccc
'• ---c
' u ? ; ;
.'-••'- i-
~l
I
A-24
-------
/Wr- i- L
Dace
Flov -Uce, SnVar
Paniculate, j/Nm1
Moisture, I Volume
Tenperacure, *C
a
3
I
|
id
X
Ck.
§
"** '
1
2
W
Z
31
1
VI
PI
01
ad 3
3 Q.'
bu C.
3
3
V5
31
iJ
i
i
Machod
Sj
ca.
CO
COz
Acid Gises
Sat. HC
Caaae. HC
Cj
Ci
C,
c,
Cs
c.*
Toluene
a,s
cos
CH,SH
c,..
H2S
SH,
aa
Fhenol
CjmfAit.* r
^J0/0 !
-------
T,.,n /U A/r
i^fna.^ i
<•: ' AT ! fajavo ' I— 9""* f.v/rj
ii I vWj;j| JiV .'71 ~,j ,-Wr
^aic
Jlov Race, SmVhr
Parrlculace, j/Nm3
iiaisture, ! Voluae
Temperacure, °C
1
i
i
2
<
CJ
2
X
•**
c
3
M
s
-^
o
M
1
M
1
2
=
VI
s G
a. ^-<
3.
1 1
J ""
V)
§
ai
iJ
1
Method
/fit i ."?77 /m 1 /•??/' SvASfiUf.'T '>/)/n>>J/*vi iff"
0£A.r
Hi
Oj
N,
ca.
CO
COz
Acid Gijes
Sac. 3C
tlnsac . HC
C;
C3
C»
Cs
C«
c..
^anzeae
Toluene
3JS
COS
CH,SH
c2H5sa
so
H^S
sra,
aa
Phenol
A/P
7/./
flf
j •" ''-1 C"'J """ '-frr
1
i
i
i
**IT
i
i
\
O.J
fjf
/V
-------
T 7
IX- Sa^S'-l /*3^T /«
Dace
rlov Site, Ha'/hr
Particulate, g/^m3
Moisture, * 7olune
Temperature, °C
.j.
i
I
1
i£
<
5
X
* *
—
a
i
5
«
I
to
|
i <
o
g
=
V)
as
a. --^
yl
^ B
2 ii
5
i
H!
si
I
Z
Method
Hi
0:
Sz
ca.
CO
COj
icid Gases
Sat. HC
3nsat. HC
Ci
C3
C.
Cj
C,
c««.
Benzene
Toluene
32S
COS
CH3S3
CjHsSH
*° *
SlS
NH,
HO
Jhenol
r^y.^V J
J „ > , • \ !** '' '
3tfr ' A/'.V J v'.v j^ -> = «. AJ
i
^,r ,«r
JF i
x'ff 7 1
i ' 1
77. i !
*jf
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0.1
\ •
I ^ ; v f <
\
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i
M? fJ £
77
-r^,4 ,^,MT f^faffts
. , r; ,^-r.^ •_„ -,^
i
1
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i
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1
/7
i
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>** r | , j /-
l
A-27
-------
T 77 ir 2)-»r4
/^ . - \
'^Antiid.4 I i
Dace
Flow Race, SmVhr
Paniculate, g/Nm3
Moisture, £ 7oluma
Teoperacure, °C
=3
»
1
•Jl
|
a
X
=••
^
-j
*"*
M
.:
o
«
i
z
3
O
i
=
V!
•w U
U U
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3! 9
S i:
!
I
«
y
CJ
|
Method
;
O*'#.*' JT :
Ax c-»«i -^r t«,..ii C
Stfr
A/OV JJ
J.,» M
j 1
1
Hj
Oi
^
ca.
CO
COZ
Acid Gases
Sac. HC
Uasac. ?-C
fif
It.L
3o. 1
fif
fif
o.C
fif
1
C2 |
Ci
c»
c.
c«
c«t
Senzena
Toluenft
a,s
cos
CH,3H
CjHsSH
SH,
aa
Phenol
JF
dF
3-t
Hf
^
^
•jf
.^^V^i
-J^^/ /?7f;
1
jit.
1
-i.i-3
^,n^4,^.v iZT
A/,, /? /f»/
0 Ji - 0 7^.
fill if
I
-------
_r»
s/vr /tl./Q
Dace
Flow !Uca, Sm'/hr
Particulace, g/Nm3
iioiscure, I Volun*
Tesperatura, "C
i
o
«
VI
2
X
:*<
CJ
a
o
M
en
1
•-J
=
SG
c. — •
si a
£ i:
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3
1
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a
z
Me chad
* " ! r j v
J«/-r
"",£
i>fC. A3
'111
s't -»"'t r'"' vs j e
1
\
1 ' ;
',
1
1 • ' ':
a,
Oj
M:
CH*
CO
.Veld Gases
Sac. HC
Ousat. 3C
C2
C,
C.
C5
C,
c«.
Benzene
Toluene
HjS
COS
C2]5H
CiHsSH
30,
H,3
SH,
acf
Phenol
ftf
A».t
7f.f
.
^e
\
\
fJI' '^^
^•7
>"
rt?
fif
JT/
i
i
1
"
\
A-29
-------
Fix. Sa^PLf Pa i*
Dace
Flov Sats, XnVhr
Particulata, g/Nm1
Moisture, I Voluoe
Temperature, 'C
g
I
CsJ
VI
X
"•
1
1
z
sc
I
VI
!§
SUl.FUK SP
ppcuv I
a
a
1
sn
a.
Method
Sj
Sj
CE»
CO
COj
Acid GAS^S
Sat. 3C
Unsat. HC
C2
Ci
C,
Cs
c,+
Benzene
Tolueae
HjS
COS
CHiSH
SH,
acs
Phenol
^,,,^ r 1
f.-
Sf'ri
Otur
"
f/.o
fif
JF
0.1.
f5o
tea;, <•«««. Ca~~f>Jrs/ /OT«VS
•
,0,,
o.-/
/.^
ijo
/oo
JXJ /? T-,i ^r J)«WJ ,w
i
i
j
i
i
T"
A-30
-------
r^Ase T 77Jr bun f~,± Sa^scf /c/wr /-S~. i
Dace
Flow SUtft, Nm'/hr
Parciculace, g/Nm3
Moisture, Z Volume
Temperacurs, *C
iJ
1
cn
VI
X
*•
^
3
o
M
1
CO
|
C
=
SULFUR SPECIES
|>|imv (GC)
a
z
5
Mechod
Oj
,t
CO
COj
Acid Cases
Sac. HC
Cosae. HC
Cz
C3
C,
Cs
Ct
Benzene
Toluene
COS
CH3SH
H,S
3C3
Phenol
X) | j
^r •
-------
PMS£ I TeiT 2>ArA -~<_ *\1-^f Pi.or '^.3
Data
Flov Sate, Sa'/hr
Particulate, zlTSn?
Moisture, ' Volume
Tenperacure, *C
1
3
i
en
C
a
X
a.
u
"-'
r
5
g
M
1
z
1
=
to
i 5
«7
ad 3
3 C.
1
in
a:
2
H
Method
Hz
Oz
Si
CH,
CO
COZ
Acid Gases
Sac. HC
Unaat. HC
Ci
C3
C.
C5
c.
3elzeae
toluene
HzS
COS
ca,sa
CjEsSH
».
H,S
SHi
HCJ
Phenol
^««/*j r :
Csm,tlijJ x
t
/t,T
/J«-r
"'i-ii
^
1.0
».t
v^-
o./
V^
O.A
flf
-
^
"°:^
OMT
J*M 11
/ = •>?
•
':
0.2.
O.I
n°
?JF
-Tuj*t ds C^ttfSu}-
~ IT ff« •
A-32
-------
rn
1
Sate
Flow JUce, No'/hr
Paniculate, g/No1
Moisture, Z Volume
Temperature , " C
u
o
1
1
X
"•
Method
Si
02
N.
C3»
CO
COi
Acid Gisea
Sat. HC
Da&at. HC
CAnttuJ I
gr li-r
Sefr rJm AI
^
fif
Ji.o
13. L
fif
fif
»•/
fif
1* ^
~ In fai.*TiSfLy Lm fiatJ
^
I
3
„
i
'i
=
'Sl
it
- i
u. Z
5
i
r
SOTONI.IH1
Cj
Cj
c.
Cs
Ct
Benzene
Toluene
H23
COS
CH,SH
CjHsSH
HjS
NH,
HOI
Phenol
v^
1
t
^
^^
J.7
,-/,'
A-33
-------
Date
71ov late, Sm'/hr
Partleulate, g/Nm3
Moisture, * Volume
Temperature, °C
1
1
<
a
s;
x
~
•^
2
X
1
i
a-
1
=
as
a- •—'
ua
* i
P &
, c>
=
va
|
l
VI
Z
r
Method
Sj
Oj
ca.
CO
COj
Acid Gases
Sat. EC
Cnsat. HC
C:
Cs
C,
c,
c..
Benzene
Toluene
HjS
COS
CH3SH
so*
H2S
SCi
Phenol
C^,,
i* IT
-/fi0
^,,,,v -
<- 1 <.-^/=
•x*'
JT:^- -97^
/,„«,
'teeo
1 f-f
I.4S
/ ei.
0 /I
-rr- \ '~
'""-^
9i"n
If
C-C.
^
1 £~C
,^
*F
r~
0 - f
- ei
C ft
c,4
;?!<*
^
^
'i^;^"
A-34
-------
APPENDIX B
PHASE I DATA SUMMARY TABLES -
LIQUIDS AND SOLIDS
The following tables contain summaries of the raw
Phase I test data for liquids and solids. Most of the data has
been reported in a previous document (Reference 6) and the re-
maining data resulted from samples analyzed by Radian Corporation
in the United States.
Flow rate data are presented in Appendix C and are
not repeated in this section.
B-l
-------
TABLE B-l. UASTHMTER DATA
Components
pH value
SuapenJed solids
(105\:). nig/l
Total Residue on Eva-
ponillun (105°C), mg/l
Tot<*l Healdue of sample
((.00 C). ms/l
DUuolvtd Mutter (105°C)
(Ftltr.ihK- Heal. 1.. if), mK/l
Fixed Keuldue of !>la-
aolvvJ gutter (600 C),
»g/l
COD (KjCrjO,), mg Oj/l
Permanganate Value
(OlnO,) m«/l
tri
1 Total Phenols, cag/1
10 Volatile Phenols, mg/l
Atnmmta free, ng/1
Atonunia fixed, rag/1
Cyanide (CN~), mg/l
Tar, Oil (Other
extracts), fflK/1
ChlurlJe (C1-), mg/l
SuHatea, ng/1
Rliodanate (CNS*), mg/l
Thlouulf atea (SjOja~),
ng/1
Fluorides (F-), Bg/1
Nitrites (NOi), ng/1
Nitrates (NO,), ng/1
Note: n.d - not determined
RI
11/1/77
11.75
559
1991
1780
1432
1275
n.d.
n.d.
n.d.
0.3
Trace
1.5
0.01
0
25.5
515
0.025
Trace
0.65
0.29
4.00
Koaovo
RI
Cyanic Waste
Sampling Point
Koaovo
Xl/3/77
11.75
585
1935
1650
1352
1125
4
74
n.d.
0.2
n.d.
n.d.
n.d.
n.d.
21.3
490
n.d.
n.d.
n.d.
n.d.
n.d.
Is
11.73
241
1338
1170
1097
934
n.d.
n.d.
n.d.
0.04
Trace
1.64
0
0
20
323
0.01
Trace
0.80
0.05
4.25
11.5
172
1307
n.d.
1135
n.d.
0.8
74
n.d.
0.04
n.d.
n.d.
n.d.
n.d.
21.3
480
n.d.
n.d.
n.d.
n.d.
n.d.
Water
I 12.3
RI
Phenoaolvan
Waste Water
a
Sampling Point: 14.11
Kouovo
11/10/77
11.4
179
2091
X
1912
X
23.8
16.4
n.d.
0.1
Trace
2.5
0
0
37
55)
0.04
Trace
0.92
0.06
5.34
11.45
179
2091
16SO
1912
1484
23.8
69
n.d.
0.1
n.d.
n.d.
n.d.
n.d.
53.2
553
n.d.
n.d.
n.d.
n.d.
n.d.
RI Koaovo RI
11/21/77
12.1
204
2314
X
2110
X
154
139
n.d.
0.25
Trace
2.2
0.01
0
36.5
668
0.0)
Trace
1.19
0.82
5.61
Kosovo
11/22/77
12.1 9.25
204 190
2314 1450
1778 62
2110 1260
1588 56
154 3136
1 10 6800
n.d. 270
0.15 153
n.d. Trace
n.d. 201
n.d. 0.02
n.d. 0
71 95. 1
n.d. 112
n.d. 2.8
n.d. Trace
n.d. Trace
n.d. Trace
n.d. 11.84
9.25
154
1032
64
878
83
3136
5395
270
151
n.d.
n.d.
n.d.
n.d.
16. 1
n.d.
n.d.
n.d.
n.d.
n.d.
n.d.
RI
toaovo
11/21/77
9.4
150
1190
101
10)8
10)
3)12
7300
170
160
Trace
209
0.017
0
121.5
105
1.3
Trace
Trace
0.0)
10.91
9.4
n.d.
965
50
952
40
11)2
7648
170
162
n.d.
n.d.
n.d.
n.d.
16.6
n.d.
u.d.
n.d.
n.d.
n.d.
n.d.
a - During sampling. Pl.enoaolvan section was not operating within
nor dial production conditlona,
Sourc*i Reference 6
»I <• Rudarskl lastltutt (Yugoal«vl«)
Ko*ovo - Kouova Coinbin* (Yugo«Uvi«)
-------
TABLE B-2. PROXIMATE AND ULTIMATE ANALYSES OF SOLIDS AND LIQUIDS
I
Co
Ltenlte (2.0)
Wet Dry
Moisture Z
Ash 7.
Sulfur 1
Carbon Z
Hydrogen Z
[Iltrogen Z
Chlorine Z
Oxygen (Difference) Z
Cross Heating
(kcal/kK)
Methylene Chloride
Insoluble Partlculates Z
20.23
14.28
0.89
44.52
3.51
1.08
0.01
15.48
4100
-
-
17.90
1.11
55.81
4.40
1.36
0.01
19.41
5150
-
Dry Slag (12. 1)
Wet Dry
2.05
93.46
0.15
1.74
0.25
0.03
0.04
2.28
28
-
-
95.42
0.15
1.78
0.26
0.03
0.04
2.32
28
-
Tar and Duat (13.0)* Tar (15.1)
Dry Dry
6
0
55
7
0
28
-
.61
.33
.98
.63
.87
-
.58*
6340
26
.0
-
0.
0.
81.
8.
1.
-
7.
22
49
92
35
26
76
8910
-
Medium Oil (15.2)
Dry
-
0.
0.
81.
8.
1.
-
8.
03
71
16
91
01
18
9150
-
Gasoline (15.3)
As Received
-
-
2.15
85.67
9.85
0.18
-
2.15
9940
-
* Sample wet when analyzed
Mote: Samples brought back to USA for analysis
-------
TABLE B-3. LIQUID BY-PRODUCT DATA
By-Products
Measurement Point
Amounts, calculated
from design (tons/hr)
Water
Ash
Total Sulphur
Gross Heating Value
(kcal/kg)
Carbon
Hydrogen
Total phenols
Spec, gravity, g/cm3
Residue after extraction
with toluene and benzene
Gaso-
line
15.3
0.65
-
0.0
1.45
9395
78.07
8.72
-
0.845
—
Medium
oil
15.2
1.55
0.80
-
0.95
9880
82.43
8.96
2.1
0.972
—
Tar
15.1
2.2
1.08
0.92
0.75
8710
72.51
8.06
0.7
1.059
6.9
Source: Reference 6
B-4
-------
TABLE B-4. PROXIMATE AND ULTIMATE ANALYSES OF LIGNITE FROM
2.0 (COMPOSITED EACH DAY)
W
Ui
7/25/77
Moisture %
Ash %
Total Sulfur %
Free Sulfur %
Fixed Sulfur %
Coke %
Fixed Carbon %
Vo La tiles %
Combustibles "L
Gross Heating Values
(kcal/kg)
Carbon dioxide (C02) %
Carbon %
Hydrogen %
Nitrogen -f Oxygen %
WET
22.00
15.71
1.03
0.85
0.18
42.91
27.20
35.09
62.29
3875
42.70
3.10
16.31
DRY
—
20.14
1.32
1.09
0.23
55.01
34.87
44.99
79.86
4970
54.74
3.97
20.92
RUDARSKI
INSTITUTE
11/1/77
WET
28.66
17.03
1.43
0.96
0.47
39.49
22.46
31.85
54.31
3220
3.70
35.61
3.19
15.04
DRY
—
23.87
2.01
1.35
0.66
55.35
31.48
44.65
76.13
4510
5.19
49.92
4.47
21.08
\—^z- i =;
11/2/77
WET
24.59
12.00
0.91
0.69
0.22
39.71
27.71
35.70
63.41
4010
—
43.64
3.59
15.96
DRY
—
15.91
1.21
0.92
0.29
52.66
36.75
47.34
84.09
5320
—
57.87
4.76
21.17
-------
TABLE B-4. CONTINUED
RUDARSKI INSTITUTE
td
11/3/77
Moisture %
Ash %
Total Sulfur %
Free Sulfur %
Fixed Sulfur %
Coke %
Fixed Carbon %
Volatiles %
Combustibles %
Gross Heating Values
(kcal/kg)
Carbon dioxide (C02) %
Carbon %
Hydrogen %
Nitrogen 4- Oxygen %
WET
24.34
15.20
1.07
0.78
0.29
•41.49
26.21
34.17
60.38
3760
DRY
—
20.2
1.41
1.03
0.38
54.84
34.64
45.16
79.80
4970
11/4/77
WET
22.86
17.73
1.03
0.71
0.32
43.37
25.64
33.77
59.41
3520
DRY
22.99
1.34
0.92
0.42
56.22
33.23
43.78
77.01
4560
11/5/77
WET
24.65
20.65
1.27
0.81
0.46
43.29
22.64
32.06
54.07
3210
33.35
2.85
18.04
DRY
27.41
1.68
1.08
0.60
57.44
30.03
42.56
72.59
4255
44.27
3.78
23.94
-------
TABLE B-4. CONTINUED
RUDARSKI INSTITUTE
w
11/6/77
Moisture %
Ash %
Total Sulfur %
Free Sulfur %
Fixed Sulfur %
Coke %
Fixed Carbon %
Volatllea '%
Combustibles %
WET
23.82
14.06
1.07
0.76
0.31
41.22
27.16
34.96
62.12
DRY
—
18.46
1.41
1.00
0.41
54.11
35.65
45.89
81.54
11/7/77
WET
22.63
16.66
1.08
0.64
0.44
43.06
26.41
34.31
60.72
DRY
—
21.53
1.40
0.83
0.57
55.66
34.13
44.34
78.47
11/8/77
WET
22.64
12.61
1.05
0.75
0.30
41.70
29.09
35.66
64.75
DRY
__
16.30
1.36
0.97
0.39
53.93
37.61
46.09
83.70
Gross Heating Values
(kcal/kg)
Carbon dioxide (C02)
Carbon %
Hydrogen %
Nitrogen + Oxygen 7.
3865
5075
3665
4740
4100
5300
-------
TABLE B-4. CONTINUED
RUDARSKI INSTITUTE
11/9/77
Moisture %
Ash 7.
Total Sulfur %
Free Sulfur %
Cd Fixed Sulfur %
i
^ Coke %
Fixed Carbon %
Volatile^ %
Combustibles %
Gross Heating Values
(kcal/kg)
Carbon dioxide (C02) %
Carbon %
Hydrogen %
Nitrogen + Oxygen %
WET
23.77
15.32
1.06
0.69
0.37
42.00
26.58
34.23
60.81
3785
• DRY
—
20.23
1.39
0.91
0,48
55.10
34.87
44.90
79.77
4965
11/10/77
WET
20.28
14.93
1.43
0.95
0.48
41.62
26.69
38.10
64.79
4035
DRY
18.73
1.80
1.19
0.61
52.21
33.48
47.79
81.27
5060
11/11/77
WET
23.55
15.20
1.18
0.80
0.38
42.62
27.42
33.83
61.25
3810
2.70
41.83
3.36
15.68
DRY
19.88
1.54
1.05
0.49
55.75
35.87
44.25
80.12
4990
3.53
54.72
4.40
20.51
-------
TABLE B-4. CONTINUED
RUDARSKI INSTITUTE
11/12/77
Moisture %
Asli %
Total Sulfur %
Free Sulfur %
Fixed Sulfur %
Coke %
Fixed Carbon %
Vola tiles %
Combustibles %
WET
24.06
10.43
1.16
0.80
0.36
39.95
29.52
35.99
65.51
DRY
—
13.73
1.53
1.05
0.48
52.61
38.88
47.39
86.27
11/21/77
WET
21.28
12.19
1.11
0.84
0.27
41.84
29.65
36.88
66.53
DRY
—
15.49
1.41
1.07
0.34
53.5
37.66
46.85
84.51
11/22/77
WET
23.86
10.85
1.13
0.84
0.29
40.45
29.60
35.69
65.29
DRY
—
14.25
1.48
1.10
0.38
53.12
38.88
46.87
85.75
Gross Heating Values
(kcal/kg)
Carbon dioxide (C02) %
Carbon %
Hydrogen %
Nitrogen + Oxygen %
4185
5515
4210
5350
4170
5480
-------
TABLE B-4. CONTINUED
RUDARSKI INSTITUTE
o
11/23/77
Moisture %
Ash %
Totul Sulfur 7,
Free Sulfur %
Fixed Sulfur %
Coke %
Fixed Carbon %
Volatiles %
Combustibles %
Gross Heating Values
(kcal/kg)
Carbon dioxide (C02) 7,
Carbon %
Hydrogen %
Nitrogen + Oxygen %
WET
23.85
12.12
1.15
0.84
0.31
40.89
28.77
35.26
64.03
4050
1.29
44.07
3.62
16.03
DRY
—
15.92
1.51
1.10
0.41
53.69
37.77
46.31
84.08
5320
1.70
57.87
4.76
21.04
11/24/77
WET
25.66
10.57
0.99
0.71
0.28
39.12
28.55
35.22
63.77
4075
DRY
—
14.22
1.33
0.95
0.38
52.62
38.40
47.38
85.78
5480
11/25/77
WET
22.77
13.34
1.05
0.89
0.16
42.41
29.07
34.82
63.89
3980
DRY
—
17.27
1.36
1.15
0.21
54.92
37.65
40.08
82.73
5150
Source: Reference 6
-------
TABLE B-5.- PROXIMATE ANALYSES OF DRIED LIGNITE
FROM 2.0 (COMPOSITED EACH DAY)
KOSOVO INSTITUTE
11/2/77
Moisture Z
Ash Z
Total Sulfur Z
Free Sulfur Z
Fixed Sulfur Z
Coke Z
Fixed Carbon Z
Volatiles Z.
Combustibles Z
Moisture Z
Ash Z
Total Sulfur Z
Free Sulfur Z
Fixed Sulfur Z
Coke Z
Fixed Carbon Z
Volatiles Z
Combustibles Z
WET
25.23
12.16
1.00
0.69
0.31
38.54
26.38
36.23
62.61
WET
25.13
18.49
1.46
0.87
0.59
42.82
24.33
32.05
56.38
DRY
__
16.27
1.35
0.93
0.42
51.55
35.28
48.45
83.73
11/5/77
DRY
—
24.69
1.95
1.16
0.79
57.19
32.50
42.81
75.31
11/3/77
WET
25.14
15.28
1.21
0.79
0.42
39.54
24.26
35.32
59.58
KOSOVO
DRY
_
20.41
1.62
1.06
0.56
52;83
32.42
47.17
79.59
INSTITUTE
11/6/77
WET
24.50
13.23
1.24
0.81
0.43
38.72
25.49
36.78
62.27
DRY
—
17.52
1.64
1.07
0.57
51.29
33.77
48.71
82.48
11/4/77
WET
23.30
17.26
1.09
0.77
0.32
41.69
24.43
35.01
59.44
DRY
22.50
1.42
1.01
0.41
54.36
31.86
45.64
77.50
11/7/77
WET
23.42
15.68
1.00
0.72
0.28
42.09
26.41
34.49
60.90
DRY
—
20.48
1.30
0.94
0.36
54.96
34.48
45.04
79.52
B-ll
-------
TABLE B-5. CONTINUED
KOSOVO INSTITUTE
11/8/77
Moisture Z
Ash :
Total Sulfur Z
Free Sulfur Z
Fixed Sulfur Z
Coke %
Fixed Carbon Z
Volatiles %
Combustibles Z
WET
22.49
13.48
1.16
0.81
0.35
41.12
27.64
36.39
64.03
DRY
—
17.39
1.50
1.04
0.46
53.05
35.66
46.95
82.61
11/9/77
WET
24.33
15.09
0.98
0.79
0.19
40.78
86.69
34.89
60.58
DRY
—
19.94
1.30
1.04
0.26
53.89
33.95
46.11
80.06
WET
21.17
10.17
1.84
0.84
1.00
39.40
28.73
39.39
68.12
11/10/77
DRY
—
13.58
2.34
1.07
1.27
50.03
36.45
49.97
86.42
KOSOVO INSTITUTE
11/11/77
Moisture Z
Ash Z
Total Sulfur Z
Free Sulfur Z
Fixed Sulfur Z
Coke Z
Fixed Carbon Z
Volatiles Z
Combustibles Z
WET
24.17
14.64
1.57
0.83
0.74
41.73
27.09
34.10
61.19
DRY
__
19.31
2.07
1.09
0.98
55.03
35.72
44.97
80.69
WET
23.81
14.35
1.14
0.76
0.38
41.33
26.98
34.86
61.84
11/12/77
DRY
— _
18.83
1.49
0.99
0.50
54.25
35.42
45.75
81.17
WET
22.65
17.91
0.90
0.73
0.17
43.22
25.31
34.13
59.44
11/13/77
DRY
_
21.16
1.17
0.94
0.23
55.88
32.72
44.12
76.84
B-12
-------
TABLE B-5. CONTINUED
KOSOVO INSTITUTE
11/21/77 11/22/77
11/23/77
WET DRY MET DRY
Moisture I
Ash Z
Total Sulfur Z
Free Sulfur Z
Fixed Sulfur Z
Coke I
Fixed Carbon Z
Volaciles Z
Combustibles Z
22.16 — 24.77 —
11.78 15.13 10.49 13
1.28 1.65 1.44 1
0.89 1.14 0.86 1
0.39 0.51 0.58 0.
39.53 50.79 38.40 51
27.75 35.66 27.91 37
38.31 49.21 36.83 48
66.06 84.87 64.74 86
.95
.92
.15
77
.04
.09
.96
.05
WET
24.84
13.87
1.34
0.94
0.40
40.85
26.98
34.31
61.29
DRY
._
18.46
1.78
1.25
0.53
54.35
35.98
45.65
81.54
KOSOVO INSTITUTE
Moisture Z
Ash Z
Total Sulfur Z
Free Sulfur Z
Fixed Sulfur Z
Coke Z
Fixed Carbon Z
Volatilea Z
Combustibles Z
11/24/77
WET
30.16
11.45
0.93
0.73
0.20
36.46
25.01
33.38
58.39
DRY
16.39
1.33
1.04
0.29
52.21
35.82
47.79
83.61
WET
26.14
12.07
1.03
0.83
0.20
39.37
27.30
34.49
61.79
11/25/77
DRY
__
16.34
1.40
1.12
0.28
53.31
36.97
46.69
83.66
Source: Reference 6
B-13
-------
TABLE B-6. PROPERTIES Of SLAG MOM 12.2
•P-
Propertlca
7/26/77 11/1/77
Wet Dry Wet Dry
11/3/77
Wet Dry
11/10/77
Wet Dry
Jl/21/77
Uet Dry
11/21/77
Wet Dry
RuJarukl Institute
Hotatura
Aah
C fix
Coke
VolatlUa
Coobuat Iblea
Carbon dioxide (CO,)
Upper Hire limit
(mm)
X
X
X
X
X
X
X
36.30 - 28.75
58.16 91.31 61.78
0.90 1.40 2.46
59.06 92.71 64.24
4.64 7.29 7.01
5.54 8.69 9.47
-
MO
-
86.71
3.45
90.16
9.84
13.29
-
1.10
37.15
54.89
0.96
55.85
7.00
7.96
5.94
M
-
87.33
1.53
88.86
11.14
12.67
9.46
0
32.68
60.20
1.16
61.36
5.96
7.12
-
89.42
1.73
91.15
8.85
10.58
MO
29.34
63.16
1.56
64.72
5.94
7.50
-
89.38
2.21
91.59
8.41
10.62
MO
35.88
57.69
O.I)
57.82
6.30
6.43
-
89.97
0.20
90, 1/
9.83
10.03
MO
Kosovo Institute
Moisture
Ash
C (In
Coke
Volatllea
Conibuat Iblea
Sulphur total
B combust .
B bound
X
X
X
X
X
X
X
X
X
0.46
89.89
3.10
92.99
6.55
9.65
0.40
0.22
0.18
-
90.31
3.11
93.42
6.58
9.69
0.40
0.22
0.18
0.37
80.24
6.03
94.27
5.36
11.39
0.63
0.48
0.15
-
88.57
6.05
94.62
5.38
11.43
0.63
0.48
0.15
0.28
89.47
6.20
95.67
4.05
10.25
0.45
0.22
0.23
-
89.72
6.22
95.94
4.06
10.28
0.45
0.22
0.23
0.50
92.22
2.33
94.55
4.95
7.28
0.41
0.20
0.21
-
92.68
2.35
95.03
4.97
7.32
0.41
0.20
0.21
0.43
92.12
3.13
95.25
4.32
7.45
0.41
0.17
0.24
-
92.52
3.14
95.66
4.34
7.48
0.41
0.17
0.24
Source: Reference 6
-------
APPENDIX C
MASS BALANCE CALCULATIONS
To determine the correlation between design and experi-
mental data, a series of mass balance calculations were performed
on the Kosovo gasification system. The first effort involved
a component balance around a single Lurgi gasifier. The second
effort involved a sulfur balance which encompassed the gasifica-
tion, quench/cooling, tar/oil separation, Rectisol, and Pheno-
solvan sections. The primary bases used for these calculations
were the operational data obtained during Campaigns I-III of
Phase I. In cases where critical data gaps existed, design data
were used.
Component Mass Balance Around the Lurgi Gasifier
The goal of this mass balance was to determine the
extent of recovery for selected components from the feedstock in
the product gas. The input streams used in this set of calcula-
tions are:
• coal,
• steam, and
• oxygen,
while the output streams are:
• ash, and
9 hot raw gas .
C-l
-------
Since the hot raw gas stream could not be sampled directly,
other output streams from downstream units were chosen to form
a "calculated" composite output stream. The streams believed to
be most representative for purposes of generating this informa-
tion were:
• Rectisol inlet gas,
• by-product tars, oil, gasoline, phenol, and
0 Phenosolvan wastewater.
Several assumptions were made in the execution of
this mass balance. Figure C-l presents a compilation of these
assumptions.
The basis chosen for these calculations was the design
flow of coal to each gasifier (16,000 kg per hour). In order
to perform the necessary calculations, the compositions and
flow rates of all other input streams were determined using
data from the Campaign I sampling program. The composition of
the output ash was also obtained from Campaign I data. Table C-l
shows all of the values used to initiate the mass balance calcu-
lations .
By using the assumptions given in Figure C-l, component
flow rates for the three input streams and the ash stream were
calculated and are given in Table C-2.
The next step in the calculation sequence was the
determination of similar quantities for the hot raw gas stream
using sampling data obtained primarily from Campaign III. Tables
C-3 and C-4 give the appropriate compositions and flow rate data
C-2
-------
FIGURE C-l. ASSUMPTIONS USED IN GASIFIER MASS BALANCE
Coal feed to gasifier contains 2 wt% N and 14.5 wt% 0. Ultimate
analysis data (see Appendix B) did not discriminate between these
elements in most cases.
Oxygen input to gasifier is 95 percent 02 and 5 percent N2.
The amount of inert ash entering with the coal equals the amount
of inert ash leaving with the gasifier ash.
Volatiles in the gasifier bottom ash are H20 and 02 and are in
the same proportions as in the input steam/oxygen mixture.
Gasifier bottom ash contains no H2 or N2.
Rectisol inlet gas flowrate can be closely approximated by the
summation of the measured flow rates of the following streams:
1) Rectisol outlet gas flowrate
2) H2S-rich gas flowrate
3) C02 vent gas flowrate
C H (ORSAT data) is equivalent to propane (C3H3).
n m
By-product phenol to storage can be represented by C6H60
(molecular weight = 110).
Cpal and ash lock expansion gas volumes are negligible compared
to those of the hot raw gas and bottom ash output streams from
the gasifier.
C-3
-------
TABLE C-l. COMPOSITION OF FIXED STREAMS FOR TIATERIAL BALANCE
Component
H20
Inert ash
S
C
H
N
0
02
N2
Fixed carbon
Volatiles
Flowrate
*
Coal Steam Oxygen
(wt %) (wt %) (vol %)
23.9 100
14.4
1.1
40.8
3.3
2.0
14.5
95
5
100.0 100 100
16,000 12,700* 1640*
(kg/h) (kg/h) (Nm3/h)
A
Ash
(wt %)
90.4
0.5
4.1
5.0
100.0
^Selected from Campaign I data.
04
-------
TABLE C-2. MASS FLOWRATES OF ELEMENTS IN THE MAJOR INPUT STREAMS AND
ASH OUTPUT STREAM OF THE LURGI GASIFIER AT KOSOVO
Component
S
C
H
N
0
Coal
179
6500
943
320
5680
Input (kg/hr)
Steam/Oxygen
-
-
1411.0
102.5
13,509
Output (kg/hr)
Ash
11.5
105
11.9
-
114.8
C-5
-------
TABLE C-3. COMPOSITION AND FLOWRATE INFORMATION FOR RECTISOL INLET
GAS AS EXTRACTED FROM CAMPAIGN III SAMPLING DATA
Composition3
Component
H2
CO
N2
CH.(
CO 2
CnH
n m
H2S
o 02
i
<* NH3
HCN
Vol %
36.2
13.6
1.56
12.9
33.5
1.21
0.47
0.55
0.00033
0.00605
100.0
Flowrate
Rectisol outlet gas flowratec 12,840 Nm3/h
H2S-rich gas flowrated 1,243 Nm3/h
C02 vent gas flowrate6 4,694 Nm3/h
Total 18,417 Mm3 /h
*3
From Sample Point 7.3, Campaign III
One gasifier-in-service basis
r*
Design flowrate
From Sample Point 7.1, Campaign III
Sample Point 7.2, Campaign III
-------
TABLE C-4. COMPOSITION AND FLOWRATE INFORMATION FOR ADDITIONAL STREAMS
NEEDED TO FORM COMPOSITE HOT RAH GAS STREAM
O
i
Tar & Dust
S
C
H
N
Ob
Inert ash
Gasoline,
S
C
H
N
Ob
Inert ash
, 100 kg/h
wt %, dry
0.33
55.98
7.63
0.87
28.58
6.61
130 kg/h
wt %, dry
2.15
85.67
9.85
0.18
2.15
0.00
Tar, 400 kg/h Medium Oil, 250 kg/h
wt %, dry wt %, dry
S 0.49 S 0.71
C 81.92 C 81.16
H 8.35 H 8.91
N 1.26 N 1.01
Ob 7.76 Ob 8.18
Inert ash 0.22 Inert ash 0.03
c
Phenosolvan Wastewater ,
13,000 kg/h Phenol, 90 kg/h
mg/& 100% C6H60
Phenol 220
Fixed NH3 205
HCN 0.018
2L
Design data
By difference
CAs averaged from Campaign I data
-------
for the streams chosen to comprise the composite hot raw gas
stream. The component flow rates for the streams which were
used to generate a composite hot raw gas stream are tabulated
in Table C-5. Table C-6 provides a summary of the component
mass balance calculations.
An examination of the data presented in Table C-6 shows
that reasonable accountability was observed for all of the major
components considered. Although the number of assumptions
necessary for the calculations limits the usefulness of the
results, it can be concluded generally that there are no serious
errors in any of the data used in performing these calculations.
Sulfur Mass Balance
The goal of the sulfur mass balance was the determina-
tion of whether the sulfur entering the Kosovo gasification
system could be accounted for in the effluent streams. The
result of this balance is discussed below.
The sole source of sulfur entering the system is the
dried lignite fed to the gasifier. Sulfur leaves the system in
solid, liquid, and gaseous streams. For the purpose of this mass
balance, it appeared more useful to perform these calculations
around key plant sections rather than around the entire gasifi-
cation plant. For this reason, a decision was made to study
these key areas of the plant independently. These areas consist
of the:
» Gasification, quench/cooling, and tar
separation sections,
-------
TABLE C-5. MASS FLOWRATES FOR ELEMENTS AND ASH IN THE STREAMS FORMING COMPOSITE HOT RAW GAS STREAM
Component Flowrate, kg/h
Rectisol
Inlet Gas
O
i
vD
Component
S
C
H
N
0
Inert ash
122
6,227
1,098
356
10,667
—
Tar
2
328
33.4
5
31
0.9
Tar &
Dust
0.
56
7.
0.
28.
6.
3
6
9
6
6
Medium
Oil
1
203
22
2
20
—
.8
.3
.5
.5
Gasoline
2
111
12
0
2
.8
.4
.8
.2
.8
-
Phenosolvan
Wastewater Phenol Total
129
1.9 58.9 6,986
1,445 4.9 2,624
2.2 - 367
11,556 26.2 22,332
7.5
-------
n
i
i—'
o
TABLE C-6. SUMMARY OF MASS BALANCE RESULTS FOR THE LURGI GASIFIER AT KOSOVO
Component
S
C
H
N
0
Inert Aah
Coal
179
6500
943
320
5680
2287.5
Input (kg/hr)
Steam/Oxygen Total
179
6500
1411 2354
102.5 422.5
13,509 19,189
2287.5
Ash
11.5
105.0
11.9
-
114.8
2280
Output (kg/hr)
Hot Raw Gaa
129
6986
2624
.367
22,332
7.5
Total
140.5
7091
2635.9
367
22,446.6
2287.5
Percent
Accountability"
78. 5
109
112
86.8
117
100
* (Total output/total Input) x 1001
-------
• Rectisol section, and
• Phenosolvan section.
Figures C-2, C-3, and C-4 are schematic representations
of these areas with the principal sulfur containing streams
entering and leaving each section indicated.
The information used to calculate the amounts of
sulfur in the appropriate input and output streams were taken
from several sources. Most of the information came from sampling
data obtained during Campaign III. Flow rate information was
taken predominantly from design data. The combination of these
data was felt to provide a sufficiently reliable base for an
initial attempt at a sulfur mass balance.
A summary of the sulfur mass balance calculations per-
formed for the gasification, quench/cooling, and tar separation
sections is presented in Table C-7. Table C-8 contains a
summary of the sulfur mass balance calculations for the Rectisol
section.
A complete analysis of Phenosolvan inlet wastewater
was not made in Phase I. Therefore, it was not possible to make
a sulfur balance around this unit. A simulated sulfur inlet
flow rate was computed, however, since this datum point was
needed to complete a mass balance around the gasification,
quench/cooling and tar separation sections. An independent
check of this balance should be made in Phase II, when Pheno-
solvan inlet and outlet water should be sampled and analyzed. A
summary of the sulfur mass balance calculations for the Pheno-
solvan section is presented in Table C-9.
C-ll
-------
o
Off Gases (Sample Points 3.2, 3.4, 3.5, 3.6)
Coal *
(Sample
Point 2.0)
Gasification
Section
Hot Raw Gas
Venturi Scrubber
Medium Oil &
Slowdown
Ash (wet)
(Sample Point 1
Wastewater
(Sample Point 12.3)
Gas Liquor
Phenolic Water
Quench/
Cooling
Section
Tar & Phenolic Water
Gas to
~~*Rectisol
(Sample
Point 7.3)
Cyanic
->-Water from
Rectisol
(Sample
Point 7.5)
Tar
Separation
Section
->-Off Gases (Sample Points 13.1
13.3, 13.5, 13.6,
13.7)
-^-Phenolic Water to Phenosolvan
Heavy Tar & Dust (Sample Point 13.8)
Tar (Sample Points 13.9 & 13.10)
Medium Oil (Sample Point 13.11)
Figure C-2.
Principal Sulfur-Containing Streams in Kosovo Gasification,
Quench/Cooling, and Tar Separation Sections
-------
o
f-1
OJ
Gas from
Quench/Cooling
(Sample Point 7.3)
Cyanic Water to
Tar Separation ,<—
(Sample Point 7.5)
Rectisol
Section
H2S-Rich Waste Gas
"(Sample Point 7.1)
JL,02 Vent Gas
"(Sample Point 7.2)
Product Gas
"(Sample Point 7.4)
Gasoline
(Sample Point 7.6)
Figure C-3. Principal Sulfur-Containing Streams in Kosovo Rectisol Section
-------
Off Gases (Various Vents - The Stripper Vent, Sample Point 14.5,
is the major one)
O
i
Phenolic
Water
(Sample Point 14.0)
Phenosolvan
Section
^Wastewater
'(Sample Point
14.11)
Figure C-4. Principal Sulfur-Containing Streams in Kosovo Phenosolvan Section
-------
TABLE C-7. SUMMARY OF SULFUR MASS BALANCE CALCULATIONS FOR THE KOSOVO
GASIFICATION, QUENCH/COOLING AND TAR SEPARATION SECTIONS
O
M
Cn
Stream
Input Coal
Output Bottom Ash
Wastewater
Heavy tar
Tar (13.9
Medium oil
Gas to Rec
Flow/hr
1600 kg
, wet (12.2) 2700 kg
(12.3) 3000 kg
and dust (13.8) 100 kg
+ 13.10) 400 kg
(13.11) 250 kg
tisol (7.3) 16,000 Nm3
Phenolic water to Phenosolvan a
Off gases
3.2
3.4
3.5
3.6
13.1
13.3
13.5
13.6
13.7
36 Nm3
40 Nm3
28 Nm3
402 Nm3
0.45 Nm3
0.4 Nm3
9.3 Nm3
26 Nm3
13 Nm3
S Content Stream S Flow Total S Flow
(kg/hr) (kg/hr)
0.89 wt%
0.15 wt%
0.017 wt%
0.33 wt%
0.49 wt%
0.71 wt%
5000 ppmv*
a
MO 00 ppmv *
%15,000 ppmv*
•WOO ppmv*
%2500 ppmv*
VL800 ppmv*
%35,000 ppmv*
V5000 ppmv*
M.5,000 ppmv*
^6000 ppmv*
142 142
4
0.5
0.33
1.96
1.8
114
3.3a
0.07
0.76
0.0025
1.43
0.001
0.02
0.066
0.56
0.11
128,9
(91% accountability)
* As H2S
'' Estimated value calculated from Phenosolvan unit output streams.
-------
O
i
I-4
ON
TABLE C-8. SUMMARY OF SULFUR MASS BALANCE FOR
THE KOSOVO RECTISOL SECTION
Input
Output
Stream
Gas from Quench/
Cooling
Cyanic Water
Gasoline
Product gas
H2S-rich gas
COa vent gas
Flow/hr
16,000 Nm3
a
130 kg
12,480 Nm3
2500 Nm3
4700 Nm3
S Content Stream S Flow Total S Flow
(kg/hr) ' (kg/hr)
5000 ppmv*
a
2.1 wt%
^1.5 ppmv*
%25,000 ppmv*
V>0 ppmv*
114 114
2.7
0.027
89.3
0.33
92
(81% accountability)
* As H2S
a Flow rate and composition are unknown. This stream will be sampled
during Phase II.
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TABLE C-9. SUMMARY OF SULFUR MASS BALANCE FOR
THE KOSOVO PHENOSOLVAN SECTION
Stream
Flow/hr
S Content
Stream S Flow
(kg/hr)
Total S Flow
(kg/hr)
Input
Phenolic water
O
i
Output
Wastewater
Off gases
14.1
14.5
13,000 kg
2 Nm3
100 Nm3
0.0033 wtZ
%2000 ppmv*
^20,000 ppmv*
0.43
0.006
2.86
3.3
* As H2S
Flow rate and composition are unknown. This stream will be sampled during Phase II.
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TECHNICAL REPORT DATA .
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-600/7-79-190
2.
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE Environmental Assessment: Source
Test and Evaluation Report--Lurgi (Kosovo) Medium-
Btu Gasification, Phase 1
5. REPORT DATE
August 1979
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
K.J.Bombaugh, W.E.Corbett, and M. D. Mats on
8. PERFORMING ORGANIZATION
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Radian Corporation
P.O. Box 9948
Austin, Texas 78766
10. PROGRAM ELEMENT NO.
E HE 62 3 A
11. CONTRACT/GRANT NO.
68-02-2608, Task 57
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 Phase 1-9/78 - 6/79
14. SPONSORING AGENCY CODE
EPA/600/13
15. SUPPLEMENTARY NOTES T£RL.RTp project officer is William J. Rhodes, Mail Drop 61,
919/541-2851.
16. ABSTRACT
repOrt summarizes an ongoing 'test program involving a commercial
medium-Btu Lurgi coal gasification plant in the Kosovo region of Yugoslavia. The
environmental data acquisition program is sponsored by the U.S. EPA and the gov-
ernment of Yugoslavia. The objective of the program is to characterize potential
environmental problems and control technology needs associated with the gasification
of lignite coal in a state-of-the-art Lurgi gasification plant. This timely program
is enabling the EPA to study firsthand the environmental problems which may be
encountered by future operators of U.S. gasification plants. Phase I of the tests ,
now complete, concentrated on the characterization of major pollutants in the
plant's gaseous emissions. Some characterization of the plant's liquid and solid
waste streams and its by-products were also performed. A SAM/IA analysis of the
gaseous emissions indicated that the major pollutants of concern are CO, benzene,
H2S, mercaptans, and NH3. The Phenosolvan effluent contained a high concentration
of organics and had a high (11-12) pH. The sulfur concentration of lights (i.e. , gaso-
line) in the by-product streams was significantly higher than that of the heavies
(i.e. , tar). Phase n will emphasize detailed characterization of trace organics and
trace elements in the plant's multimedia waste streams and control options.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS
c. COSATl Field/Group
Pollution
Assessments
Coal Gasification
Lignite
Carbon Monoxide
Benzene
Hydrogen Sulfide
Thiols
Ammonia
Pollution Control
Stationary Sources
Lurgi Process
Phenosolvan
13B
14B
13H
2 ID
07B
07C
8. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (This Report)
Unclassified
21. NO. OF PAGES
141
20. SECURITY CLASS (Thispage)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
C-18
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