EPA PROJECT REPORT NO. 74-KPM-20
MEAD CORPORATION
Chillicothe, Ohio
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Office of Air and Waste Management
Office of Air Quality Planning and Standards
Emission Measurement Branch
, Research Triangle Park. North Carolina
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KRAFT PULP MILL LIME KILN EMISSION TESTS
THE MEAD CORPORATION
CHILLICOTHE MILLS
CHILLICOTHE, OHIO
A REPORT PREPARED FOR
U.S. ENVIRONMENTAL PROTECTION AGENCY
RESEARCH TRIANGLE PARK
NORTH CAROLINA 27711
EPA REPORT NO. 7*ป-KPM-20
CONTRACT NO. 68-02-0239
TASK NO. 10
PREPARED BY:
COTTRELL ENVIRONMENTAL SCIENCES, INC.
A SUBSIDIARY OF RESEARCH-COTTRELL, INC
P.O. BOX 750
BOUND BROOK, NEW JERSEY 08805
G.J. GRIECO
CES-13^-10
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TABLE OF CONTENTS
PAGE
INTRODUCTION 1
SUMMARY AND DISCUSSION OF RESULTS 4
PROCESS DESCRIPTION AND OPERATION 6
LOCATION OF SAMPLING POINTS 10
SAMPLING AND ANALYTICAL PROCEDURES 12
LIST OF FIGURES
FIGURE I: STACK LAYOUT AND TEST PORT LOCATION 2
FIGURE II: KRAFT PULPING PROCESS 7
FIGURE III: FLOW DIAGRAM OF THE LIME KILN 9
FIGURE IV: LOCATION OF SAMPLING POINTS 11
LIST OF TABLES
TABLE I: SUMMARY OF RESULTS 5
APPENDICES
APPENDIX A: TEST DATA CALCULATIONS AND SUMMARY SHEETS
APPENDIX B: RAW DATA SHEETS
APPENDIX C: VELOCITY PROFILES
APPENDIX D: VISIBLE EMISSIONS REPORT
APPENDIX E: PROCESS DESCRIPTION AND OPERATION (EPA)
APPENDIX F: TEST METHODS
APPENDIX G: TEST LOG
APPENDIX H: PROJECT PARTICIPANTS
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INTRODUCTION
A Cottrell Environmental Sciences, Inc. test team performed
stack sampling tests at a kraft pulp mill lime kiln owned
and operated by the Mead Corporation, Chillicothe Mills,
Chlllicothe, Ohio, during the period of August 4 through
August 12, 1974.
The process tested was a 200 tons/day CaO rotary kiln that
can operate on either #2 fuel oil or natural gas. The emis-
sions are controlled by a high energy venturi scrubber/
demisting tower and are emitted to the atmosphere through a
69" I.D., 73' high smokestack (See Figure I). An induced
draft fan is located between the kiln and the venturi scrub-
ber. The lime kiln was operating at approximately 60% of
design capacity (120 tons/day) during the test period; this
production rate is typical of normal operation at this kiln.
The purpose of the test program is to obtain emission data
as part of the background data needed to establish new
source performance standards as authorized by the Clean Air
Act. The United States Environmental Protection Agency's
Emission Standards and Engineering Division of the Office of
Air Quality Planning and Standards selected this particular
lime kiln control system because it is thought to represent
best available control technology. Several other kraft pulp
mill lime kilns are also being tested by the EPA to obtain
additional emission data.
Particulate samples were extracted from the smokestack
approximately 60' from ground level. The nearest upstream
disturbance was the straightening vanes (2.0 E.D.'s) and the
nearest downstream disturbance was the top of the smokestack
(2.3 E.D.'s). Hence, forty eight (48) sampling points were
utilized In accordance with EPA Method I. The original in-
tention of this task was to perform six (6) particulate
sampling runs in accordance with EPA Method 5 andtsix (6)
Orsat analyses (CO, C02, and 02) in accordance with EPA Method
3. Three particulate tests were to have been performed
while the kiln was fired with #2 fuel oil and three tests
were to take place while firing natural gas. The particulate
samples were then to be analyzed for particulate mass and
trace elements. However, due to kiln operational problems
and test equipment malfunctions, only one valid particulate
test could be performed.
During the pretest visit (April 18, 1974) a preliminary
velocity traverse was performed to determine the variation
In the direction of flow of the gas stream across the stack
(See Appendix C). This data indicates that the gas flow
was not parallel to the stack. The velocity traverse data
from the presurvey was not used to calculate a stack gas
flow rate because Cp was not known, the temperature was not
monitored at each traverse point, and the traverse points
were equally spaced instead of at the centroid of equal
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TEST
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FIGURE I
STACK LAYOUT AND TEST PORT LOCATION
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-3-
areas. The velocity traverse was used to check for cy-
clonic flow, and the relative variation In magnitude of
the velocity head across the stack was sufficient for this
purpose.
It was decided that this "cyclonic" flow (due to the demist-
ing tower) could be alleviated by the installation of straigh-
tening vanes. The Mead Corporation requested that the vanes
be temporary (no modifications to the existing stack). Temp-
orary vanes were designed and installed prior to testing
and marginal success was achieved. The straightening vanes
were located 11.5' (2 E.D.'s) upstream from the test site
(See Figure I and Appendix C).
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SUMMARY AND DISCUSSION OF RESULTS
A summary of test results Is presented in Table I. Appendix
A of this report contains a computer printout, sample cal-
culations, a handwritten calculation form, a sample weight
"master sheet" and a laboratory analysis form. All raw data
sheets may be found In Appendix B.
An unusually high particulate mass concentration was measured
in the acetone blank (0.0132 gm/100 ml). There is no appar-
ent reason to believe that the sample was contaminated. Rea-
gent grade acetone was utilized.
i
Appendix C contains velocity and volumetric flow rate data.
It includes velocity profiles based on two preliminary vel-
ocity t raverses and one particulate sampling run from this
EPA test program. Due to a kiln operational problem (over-
flowing storage tanks), the only test performed had to be
terminated after 217 minutes. Two minutes had elapsed while
sampling from the 44th point (point B20) when the test team
was notified of an Impending shutdown. The kiln was operating
on natural gas. The isoklnetic rate for this run was 92.83%.
Appendix D contains a paper prepared by Scott Environmental
Technology, Inc., entitled "Test Visible Emissions of a
Kraft Pulp Mill Lime Kiln." This report concerns the results
of visibly determined smoke opacity data corresponding to
periods of particulate testing. The aforementioned run I
was designated Test 2 in this visible emissions report (see
Page 3, Figures 3a and 3b of the report).
The probe used during run I was glass lined; however, there
was a 2" stainless steel connection at the ball joint end of
the probe that was in contact with the sampled gas.
The test program was terminated on August 11, 1974 due to
recurring equipment malfunctions. One meter box developed a,
serious pump motor-shaft problem; the spare meter box was
broken beyond (field) repair in shipping. The probe heater
was not operating properly. The broken filter holder glass-
ware was the result of an oversized stainless steel ball
joint located on the glass lined sampling probe. When test-
Ing was terminated all of the "front half" portions of the
filter holders were broken (about six were originally ship-
ped to the job site).
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TAJil-E 1
SUMMARY OF P.ESULTS
RunNun^ber ' ! /- AJ/^UAL
Date
Stack Flow Rate - SCFM * dry
* *
7, Wciter Vapor - % Vol. .
. % C02 - Vol % dry
% 02 - Vol % dry
% Excess air @ sampling point
S0_ Emissions - ppm dry
NO __ Emissions - ppra dr>'
A _ .
Particulntes. :..'.
Probe, Cyclone, & Filter Catch
gr/SCF* dry
gr/CF @ Stack Conditions
Ibs./hr.
Total Catch
gr /SCF*dry
gr /CF @ Stack Conditions
Ibs./hr.
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* 70 F, 29.92 "Hg. . . ' .
** The Saturated Mo.fsture Content from the Psychometric Chart
was used to determine Emission Data Shown.
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PROCESS DESCRIPTION AND OPERATION
The Mead Corporation Mill at Chillicothe, Ohio produces 600
tons of kraft pulp per day. All the pulp is bleached and
converted into paper. In 1964, the mill converted from the
soda pulping process to the kraft pulping process.
PROCESS DESCRIPTION
A. GENERAL
The process for making kraft pulp from wood is shown in
Figure II. The process wood is chipped into small pieces
and then cooked in eight batch digesters at elevated pres-
sure and temperature. The cooking chemicals, called white
liquor, are sodium hydroxide and sodium sulfiddein water
solution. The white liquor chemically dissolves lignin,
leaving wood cellulose (pulp) which is filtered from the
spent liquor and washed. The pulp is then bleached, and
made into paper.
The balance of the pulping process is designed to recover
the cooking chemicals. Spent cooking liquor and the pulp
wash water are combined for treatment to recover chemicals.
The combined stream, called weak black liquor, is concentrat-
ed in multiple-effect evaporators. The black liquor receives
its final concentration in direct contact evaporators and is
then fired to a recovery furnace.
Combustion of the organic matter in the black liquor provides
heat needed to generate process steam. Inorganic chemicals
in the black liquor are recovered as a molten smelt at the
bottom of the furnace. The smelt, consisting of sodium car-
bonate and sodium sulfide, is dissolved in water and trans-
ferred to a causticizing tank. Lime added to this tank con-
verts sodium carbonate to sodium hydroxide, completing the
regeneration of white liquor, which is then recycled to the
digesters. The calcium carbonate mud that precipitates from
the causticizing tank, is recycled to a kiln to regenerate
1 i me.
B. LIME KILN
The lime kiln was designed byTraylor Company to produce 200
tons of lime (CaO) per day. This is equivalent to a pulp
production rate of about 800 tons per day. This rotary kiln
Is 300 feet long, with an inside diameter of 11 feet. It is
fired with either natural gas or No.
2 fuel oil
The feed to the kiln is the calcium carbonate slurry that
precipitates from the causticizing tanks. The slurry is
washed and then dried on a rotary vacuum drum, as shown in
Figure III. The dried cake is removed from the drum on a
knife edge and conveyed to the kiln. In the kiln, the calcium
carbonate mud is roasted and carbon dioxide is driven off,
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JJ
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(No
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Oil + Na
UOR
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RECOVERY
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HFAVY MULTlPLi:
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LIQUOR sYSlfr
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SMELT
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SMELT
DISSOLVING
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GREEN LIQUOR
DIGESTER)
CAUSTICIZING
TANK
1ANK
II[
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leaving calcium oxide (lime) as product.
The combustion gases from the kiln are cleaned in an adjust-
able throat venturl scrubber manufactured by Air Pollution
Industries. The gases then pass through a mist eliminator
and out a kO foot stack. The scrubber water is recycled from
the mist eliminator and blended with fresh water makeup. A
portion of the recycled water is purged to prevent excessive
accumulation of solids, and recycled back to the mud washers.
PROCESS OPERATION
The purpose of the tests was to measure emission levels dur-
ing normal kiln operation. Process conditions were carefully
observed, and testing was done only when the test facility
appeared to be operating normally.
During the tests, important process conditions were monitored
and recorded on data sheets. Readings were taken about
every half-hour. These records are in Appendix E. As far
as known from the process information and conversations with
the operators, the kiln and scrubber operated normally during
the only test performed. However, the test was terminated
just prior to completion when the kiln was shutdown due to
the lime storage tanks being full.
The test was performed while the kiln was burning natural
gas at a rate of about 13,200 cubic feet per hour. The kiln
was operating at about 65 percent of capacity, which is nor-
mal operation. During the test, the venturi scrubber was
operating at a pressure drop of 21.0 inches of water. The
water flow to the scrubber was ^70 gallons per minute.
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LIMESTONE
MUD
AIR
GAS OR
NO. 2. OIL
LIME
(PRODUCT)
SAMPLING PORTS -
EXHAUST
.""" GAS "
FRESH
WATER'
STACK
\
DEMISTER
RECYCLE-
^ BLEED
Figure I I I. Flow Diagram of the Lime Kiln at the Mead Mill in Chillicothe, Ohio
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LOCATION OF SAMPLING POINTS
Figure IV illustrates the location of the A8 test points
used during velocity traverses and particulate runs (EPA
Test Program). The nearest upstream disturbance was straigh-
tening vanes (2.0 E.D.'s) and the nearest downstream distur-
bance was the top of the stack (2.3 E.D.'s). A cyclonic de-
mister was located k.k E.D.'s downstream of the sampling loc-
ation, as shown in Figure I.
The straightening vanes were the most restrictive factor in
determining the number of traverse points. However, the re-
quirements of EPA Method I were fulfilled in that k8 trav-
erse points were selected.
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B
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SAMPLING AND ANALYTICAL PROCEDURES
Appendix F contains a copy of pertinent sections from the
Federal Register, Volume 36, Number 2^7, December 23, 1971,
a schematic of the sampling train utilized, and a laboratory
analysis procedure.
The Federal Register outlines the methods to be used for
sample and velocity traverses for stationary sources (Method
1), the determination of stack gas velocity and volumetric
flow rate (Method II) and the determination of particulate
emissions from stationary sources (Method V).
The sample train schematic illustrates the remote filter box
modification of EPA Method V. The "optional" cyclone located
in the heated area between the probe and filter was not used.
Prior to testing, 100 ml of distilled, deionized water was
placed in both impingers, one and two, and 200 grams of sil-
ica gel was placed In impinger four. Due to the high % mois-
ture In the flue gas stream, it was necessary to remove some
of the water collected in the impingers and replace the sil-
ica gel part way through run I.
The fI berg lass filters were prepared using a slightly dif-
ferent method than is outlined in the laboratory analysis
procedure. Each filter was dessicated for 2k hours, weighed
to +_ 0.0002 grams, and stored in a tin container prior and
after use. A "front half" water wash was also included in
the cleanup procedure, the resulting sample weight being
added to the "front half" acetone wash catch.
analyses were performed per EPA Method V part1
in accordance with EPA Method III utilizing a
Fisher brand Orsat Analyzer with a 100 ml burett.
Three Orsat
i cu1 a te run
A different analytical balance was used
testing, and so the filter weights were
blank v a 1 u e .
before and after
corrected for a
An organic extract was performed on the impinger water.
WRITTEN BY
APPROVED BY
GJG/nak
x1 r\ /i
l0?ฎ^!^. \^AJjfjR
G"ary(TJA. Gr ieco
Source Testing
Superv i sor
N.R. Troxel
Manager, Source
Testing Operations
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