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Background Report Reference AP-42 Section Number: 1 1.17 Background Chapter: 4 Reference Number: 32 Title: Air Pollution Test of Woodville Lime and Chemical Company US EPA September 1974
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Transcript of Background Report Reference AP-42 Section Number: 1 1.17 4 · PDF fileFailure of a field in...
Background Report Reference
AP-42 Section Number: 1 1.17
Background Chapter: 4
Reference Number: 32
Title: Air Pollution Test of Woodville Lime and Chemical Company
US EPA
September 1974
EPA
Text Box
Note: This is a reference cited in AP 42, Compilation of Air Pollutant Emission Factors, Volume I Stationary Point and Area Sources. AP42 is located on the EPA web site at www.epa.gov/ttn/chief/ap42/ The file name refers to the reference number, the AP42 chapter and section. The file name "ref02_c01s02.pdf" would mean the reference is from AP42 chapter 1 section 2. The reference may be from a previous version of the section and no longer cited. The primary source should always be checked.
. . . . . , ... .. . . -- .. : . , .. .. :
. . , , . ~ . . . . , . .. . . , . . . , _ _ . . ..:~,.. - .. :
PEDCO- ENVIRONMENTAL SUITE13 - ATKINSON SQUARE
CINCINNATI. O H I O 4 5 2 4 6 513 /771-4330
EMISSION TESTING REPORT EPA REPORT 74-LIM-3-B
WOODVILLE LIME AND CHEMICAL CO. WOODVILLE, OHIO
Contract No. 68-02-0237 Task 26
Submitted by :
PEDCo-Environmental Specialists, Inc. 13 Atkinson Square
Cincinnati, Ohio 45246
f li c
Septeinber 16, 1974
Prepared by:
W. G. DeWees Richard W. Gerstle, P. E.
11.
111.
IV . V.
VI.
VII.
A.
B.
C.
D.
E.
F.
G.
n .
I.
J.
K.
L.
1. TABLE OF CONTENTS
INTRODUCTION
SUMMARY OF RESULTS
PROCESS DESCRIPTION
LOCATION OF SAMPLING POINTS
PROCESS OPERATION L TEST CONDITIONS
SAMPLING AND ANALYTICAL PROCEDURES
PARTICULATE RESULTS AND EXAMPLE CALCULATIONS
GASEOUS RESULTS AND EXAMPLE CALCULATIONS
VISIBLE EMISSIONS RESULTS
OPERATING RESULTS
FIELD DATA
-
SAMPLE IDENTIFICATION LOG
LABORATORY REPORT
SAMPLI / EMTHODS ’
TEST LOG
RELATED REPORTS
PROJECT PARTICIPANTS
SUMMARY OF TESTING COSTS
- - - ~ ... \
u
i
1
. 3
9
12
14
19
11. INTRODUCTION
Under the Clean Air Act of 1970, as amended, the Environ-
mental Protection Agency is charged with the establishment of
performance standards for stationary sources which may contri-
bute significantly to air pollution. A performance standard is
based on the best emission reduction systems which have been
shown to be technically and economically feasible.
In order to set realistic performance standards, accurate
data on pollutant emissions must be gathered from the stationary
source category under consideration.
Woodville Lime and Chemical Co. in Woodville, Ohio, was
designated as a possible representative well-controlled
stationary source in the lime production industry and therefore
was selected for an emission testing program. The process under
investigation in this test series was operation of the No. 1 lime
kiln at the Woodville plant, from which emissions are controlled
by a cyclone in series with a Buell electrostatic precipitator.
Preliminary tests were performed during the week of May 20,
1974, to ascertain composition and velocity of the gas stream
and to observe visible emissions. ..
The emission test program was conducted from July 8 to 10,
1974, on three test runs. Sampling was done at the kiln stack to
determine concentrations of filterable and total particulate,
1
oxides of nitrogen, and sulfur dioxide. Determinations of
moisture content and dry molecular weight were performed
simultaneously. Samples of the kiln feed, kiln product,
kiln fuel, and effluent dust from the ESP unit were collected
for calculation of a sulfur balance. In addition, visible
emissions were recorded by two certified observers during this
time. Because of difficulties with process.operation and
above-normal production rates, further tests were scheduled
for August 5, 1974. In the interim between test periods the
kiln was shut down, at which time the ESP was cleaned and
inspected.
. .
c
2
111. SUMMARY OF RESULTS
Data on particulate emissions from the lime kiln are
summarized in Table 1. Emissions of filterable particulate,
as measured by the probe and filter catch, averaged 9.27
pounds per hour at a concentration of 0.041 grain per DSCF.
Total particulate emissions averaged 18.3 pounds per hour
at a concentration of 0.077 grain per DSCF. Emissions of
filterable particulate were higher in the first two tests
than in the third. This can probably be attributed to discon-
tinuity in process operations and to problems with control
equipment, described in Section IV, "Process Operation".
Because of these difficulties, the emissions data reported
in this report are considered questionable with respect to
being representative of a welr-controlled lime-producing
process . Data on oxides of nitrogen emissions are summarized
in Table 2. These data show an average concentration of
3 3 9 ppm by volume and an hourly emission rate of 67.7 pounds
per hour of NO2.
Data on sulfur dioxide emissions are summarized in Table
3 . These data show an average concentration of 4 4 . 5 ppm
by volume and an hourly emission rate of 12.0 pounds per
3
1
Tab le 1. SUMMARY OF PARTICULATE 3ATA
4 R u n Number - _. Date
1
7 / 8 / 7 4
--
, Volume of Gas S a m p l e d , DSCFa 237.923
Average S t a c k Tempera tu re , OF 6 2 1
11.3
S tack V o l u m e t r i c Flow R a t e , DSCFMb 2 7 6 1 9
Stack V o l u m e t r i c Flow R a t e , ACFM' 6 4 3 9 3
I s o k i n e t i c 1 0 2 . 9
i
a ' 5 P e r c e n t Mois tu re by Volume, %
. : 'Unit P roduc t ion Rate, t o n / h r ma>+
P a r t i c u l a t e s - probe , bypass , and f i l t e r c a t c h
1c1
s tPr'DSCF g 2
* .II" gr/DSCF
l b / t o n @ P a r t i c u l a t e s - t o t a l
g g r / A c F
iiYt:n ai
Dry s t a n d a r d c u b i c f e e t a t 70°F Dry s t a n d a r d c u b i c f ee t per m i n A c t u a l c u b i c f e e t p e r minute .
7 8 1 . 1
0 . 0 5 1
0 .022
1 2 . 0
1 7 0 4 . 6
0.111
0 .047
26 .2 -
3 -
7/9 /74
2 3 9 . 6 4 2
6 6 9
1 2 . 1
2 7 3 9 0
6 7 2 9 6
1 0 4 . 5
- 5 A 3
7 /10 /7 4
24.8.641 242 .07
6 7 4 6 5 5
11 .4 1 1 . 6
2 8 6 5 8 2 7 8 8 9
7 0 3 3 0 6 7 3 4 0
1 0 3 . 6 1 4 0
718.9
0 .046
0.019
1 0 . 9
4 4 3 . 5
989.9
0 .064
0 .026
1 5 . 0
._
2 9 . 9 2 i n H g . :e a t 7ODF, 2 9 . 9 2 i n . H g .
417.0 6 3 9
0.026 0 . 0 4 1
0.011 0 . 0 1 i
6.4 9 .77
' 6 5 3 8 0
8 8 9 . 3 1 1 9 4 . 6
0.055 0 .077
0 .022 0.03;
13.6 1 8 . 3
7374+7
4
Y
u
tu
w
U
4
N d
a
. . m C a u U y1 W U
O P m u n
P P
m u m u m
'' " m a m N O I
Y
al U m 4
0 .* U U m a
a
0, E .* u Y a m al E
.A m U R 0 m a cn X
N m m N
.c1 0 U U 01 u U 0 U
W U Y C .* E
5
Table 3. SUMMARY OF SULFUR DIOXIDE DATA
Test No.
Date, 1974
Flow rate, DSCFMa
Sample volume , D S C F ~ SO2 in sample, grams
SO emissions, lb/hr
SO2 concentration, ppm by volume
2
2 4 6 Avg . 7/8 7/9 7/10
27619 27390 28658
166.917 165.549 166.705
0.867 0.130 0.649
19.1 2.42 14.4 12.0
70.2 10.6 52.6 44.5
a) .Dry standard cubic feet at 7 0 ° F 29.92 in. Hg.
6
i.
1 c
r -
i
hour of sulfur dioxide.
Visual determination of the opacity of emissions from
the lime kiln exit stack was performed independently by two
PEDCo personnel. Data on opacity measurements are summarized
in Table 4 . The average opacity was less than 5 percent
in all tests. A period of high emissions occurred, however,
for about 1 minute in the first test, during which opacity
levels exceeded 20 percent. Failure of a field in the-electro-
static precipitator caused the discontinuity; with the result
that the opacity values are not considered typical of those
occuring with well-controlled lime-product.ion operations.
During sample recovery on test 1, the probe glass liner
tip was found to be broken. This test was therefore not
representative of true emissions. Because of the higher
than expected opacity and various process problems, this
test series was terminated before enough measurements were
obtained to provide representative results.
a I n t e r v a l of Observa t i ons
b D u r a t i o n o f Observat ion, min
T o t a l No. o f ReadingsC
No. o f Readings Unobservable
No. of Readings @ 0% O p a c i t y
5 %
10%
15%
20%
.252
30%
35%
40%
45%
50%
Percent Readings Unobservable
Percen t Readings @ 0% O p a c i t y
5%
10%
15%
20% . .
Pe rcen t Readings Cxceediny 20%
- 1 - 3 5 7 / 8 / 7 4 7 / 9 / 7 4 7 / 1 0 / 7 4
Obs. 1 . Obs. 2 Obs. 1 Obs. 2 Obs. 1
S t a r t
.End
0.2 20.2
a 24-hour c l o c k s t a r t and end t i i i i cs
Obs. :,
8 3 8
1 2 3 9
212 .5
8 5 0
0
7 8 2
66
1
1
-_ ~ . .
- --- - -
.- - .
- - - - -- 0
92 .0
7.8
0 .1
0.1
.
-- -.
-- -. .
- . -
Excluditi! l t h e t i r i ic t h a t r e a d i n g s were n o t r c c o r d e d f o r p e r i o d o f o b s e r v a t i o n .
l tcadit igs r e c u r d e d nL: 15-second i n t c r v a l s ultlcss o t h e r v i s e noted.
b
C
Observer 1 - R . S . Arn ick Observer 2 - W. G. DeWees
8
Lime tone onsis
IV. PROCESS DESCRIPTION
ing primarily of calcium c n t C mbina-
tions of calcium and magnesium carbonate with varying amounts of
impurities is quarried at the Woodville Plant. The limestone is
calcined or burned to form lime, commonly divided into two basic pro-
ducts--quicklime and hydrated lime. Calcination expels carbon
dioxide from the raw limestone, leaving calcium oxide (quicklime).
With the addition of water, calcium hydroxide (hydrated lime) is
formed.
The basic processes in production are: (1) quarrying the lime-
stone raw material, ( 2 ) preparing the limestone for kilns by crushing
and sizing, ( 3 ) calcining the limestone, and ( 4 ) optionally processing
the quicklime further by additional crushing and sizing followed by
hydration. The majority of lime is produced in rotary kilns which
can be fired by coal, oil, or gas. Rotary kilns have the advantage
of producing high production per man-hour and a more uniform product.
However, they do require higher capital investment and unit fuel
costs than most vertical kilns.
The Woodville Lime and Chemical plant has cwo rotary kilns
each equipped with a Buell electrostatic precipitator. The kilns
are almost identical. The feed for both is a dolomitic stone,
quarried on the site and fed in sizes ranging from 1 inch to
2 1/4 inches at a rate of about 700 tons per day. There is no
~
9
p r e h e a t e r . Normally t h e k i l n i s f u e l e d w i t h a mix tu re of
9 5 p e r c e n t Number 6 f u e l o i l and 5 p e r c e n t n a t u r a l gas . Both
k i l n s have two h e a t t r a n s f e r s e c t i o n s , each 20 f e e t long . The
p r o d u c t , about 3 5 0 t o n s p e r day , i s cooled i n a N e i m s c o o l e r b e f o r e
s t o r a g e . There i s no p r o d u c t c r u s h i n g , b u t u n d e r s i z e m a t e r i a l -
i s s e p a r a t e d and r e t u r n e d t o t h e k i l n . The m a j o r i t y of t h e
p roduc t is used i n t h e s teel i n d u s t r y , most ly i n b a s i c oxygen
f u r n a c e s ; none of t h e p r o d u c t i s h y d r a t e d .
The e l e c t r o s t a t i c p r e c i p i t a t o r on k i l n Number 1 w a s p u t i n
o p e r a t i o n i n J u l y 1 9 7 1 . I n t h i s k i l n t h e main p r o c e s s f a n i s
l o c a t e d b e f o r e t h e ESP , w i t h a c y c l o n e b e f o r e t h e f a n t o reduce
f a n b l a d e e r o s i o n . The p r e c i p i t a t o r on k i l n Number 2 was p u t i n
o p e r a t i o n i n December 1973. The main p r o c e s s f a n is a f t e r t h e
ESP and t h e r e i s no cyc lone .
I n bo th sys tems t h e i n l e t g a s t o t h e p r e c i p i t a t o r s i s cooled
t o about 600°F w i t h a c o n h i n a t i o n of w a t e r i n j e c t i o n and/or
tempering a i r . Each p r e c i p i t a t o r has 2 8 , 8 0 0 s q u a r e f e e t o f
c o l l e c t i n g s u r f a c e a r e a , which i n c l u d e s one c e l l and two f i e l d s ;
des ign gas v e l o c i t y i s 1 . 5 f e e t p e r second and t r e a t m e n t t ime ,
10.0 8econds-
emissim t e s t showed e x i t l o a d i n g s o f less t h a n 0 . 0 0 5 g r a i n
p e r d r y s t a n d a r d c u b i c f o o t .
The p l a n t manager r e p o r t e d t h a t an e a r l i e r
A t p r e s e n t t h e d u s t c o l l e c t e d from t h e p r e c i p i t a t o r s is
d i sposed of i n t h e q u a r r y . I t i s expec ted t h a t i n t h e f u t u r e t h e
10
dust will be granulated and used as a component of dry mix
fertilizers that are blended in another part of the complex.
At the time of the initial plant inspection (February 8,
1974) the precipitators were working satisfactorily and had
been very well maintained. The plant is representative of
modern design; raw materials and products.are typical of those
in the industry.
.
11
_.
i i b b V . LOCATION OF SAMPLING POINTS
F igu re 1 shows t h e sampl ing p o r t s and sampling p o i n t s used
i n t h e N o . 1 l ime k i l n e x i t s t a c k . The sampling p o r t s were
l o c a t e d i n a 63.5-inch i n s i d e - d i a m e t e r v e r t i c a l s t a c k , . 4 f e e t
( 0 . 7 5 d i a m e t e r ) from t h e s t a c k e x i t , and 1 2 f e e t ( 2 . 2 6 d i a m e t e r s )
from t h e n e a r e s t downstream d i s t u r b a n c e . I n o r d e r t o meet t h e
sampling r equ i r emen t s of Methods 1 and 5 of t h e F e d e r a l R e g i s t e r ,
V o l . 36, No. 2 4 7 , i t was n e c e s s a r y t o i n s t a l l a s t a c k e x t e n s i o n
on t h e ESP e x h a u s t o u t l e t . F o r t y - e i g h t t r a v e r s e p o i n t s ( 2 4
a long each of two p e r p e n d i c u l a r d i a m e t e r s ) were used a s d e s c r i b e d
i n t h e F e d e r a l R e g i s t e r Method 1. A d d i t i o n a l sampling p o i n t s i n
t h e e x i s t i n g s t a c k a t a lower s i t e were used f o r some of t h e gas
sampling.
b 1 I
1 2
Edge 0 1 r o o f
6 3 . 5 " I.D.
24 24 i ) . . .. . . .. ..
.. . *...
w b s I -1
C R O S S S E C T I O N
~. ! . Sc o f loldiiig Al l Oimenrions in Fcr.1 A r c Approximale
SIDE V I E W
F i g u r e 1. T e s t S i t e - N o . 1 K i l n P r e c i p i t a t o r O u t l e t .
13
i b c
. c i II ci t t € t f b
E B
VI. PROCESS OPERATION & TEST CONDITIONS
Before the test series began, EPA engineers had decided
to conduct tests at the Woodville plant only during periods
in which opacity of visible emissions from the kiln stack
was in the range of 0 to 5 percent. This range had been
described as typical of opacities during operation of the
No. 1 kiln and was judged to be typical of those occurring
in a well-controlled lime-producing plant.
Although plant operations appeared to be normal and
preliminary readings indicated 0 to 5 percent opacity values,
several problems developed during the first day of testing,
July 8,1974. After about 3 hours of testing, PEDCO'S team
of opacity readers stopped the tests at 8:22 p.m. because
opacity values were exceeding.the 5 percent limit. Testing
was resumed at 8:27 p.m. and continued until 9:13 p.m.,
when the "A" field of the kiln's electrostatic precipitator
malfunctioned, probably because of overload. Sampling was
resumed at 9:16 p.m., when the opacity values again dropped
'to the 0 to 5 percent range. The first test was completed
at 9:29 p.m. ..
The second test was started on July 9 at 8:41 a.m.
Opacities of visible emissions ranged between 0 and 5 percent
14
i ' I
Y -i f d i i i c t f f # E ;fs B I i
throughout the entire test sequence. The test was completed
at 12:48 p.m., and because no problems were encountered
in sampling or process operation the emissions were considered
representative of those occurring normally.
After completion of the second test, plant operators
performed a routine cleaning operation, shutting down a
fan on the inlet to the ESP for removal of adhering dust.
The fan was not re-started after cleaning, however, an.d
opacity readings during the afternoon ranged between 10
and 15 percent. The third test, therefore, was not begun
until the following day.
Testing was resumed at 0 : 2 4 a.m. on July 10. Operations
appeared normal except for a heavy load in the kiln, as
evidenced by the ampere meter on the kiln-drive motor.
Opacity readings ranged from 0 to 5 percent. Sampling was
hampered, however, by blockage in the silica gel impinger,
which was replaced several times.
the opacity readers reported an increasing number of 5 percent
readings, with occasional 'puffs' as high as 10 percent.
Observations of the plume were difficult because of cloudy
skies. Test No. 3 was completed at 12:55 p.m.
As testing progressed,
Operating variables for the three test runs are summarized
in Table 5, and sulfur contents of the various 'process streams
are shown in Table 6.
A fourth test, intended to provide values to replace
those obtained in Test No. I, was started at 3:OO p.m. July
1 5
Table 5 . SU.XMARY OF OPERATING VARIABLES
Date Pa r t i cu la t e T e s t N o .
S tone Feed Rate, t on /h ra
O i l R a t e , g a l / h r F i r i n g Zone Temp, O F
Mid K i l n , Temp, OF
Ki ln Feed End Temp, O F
Before ESP Temp, OF Stack Temp, OF
ELECTROSTATIC PRECIPITATOR DATA
"A" F i e l d
Primary c u r r e n t , amps
P r i m a r y v o l t a g e , v o l t s P r e c i p i t a t o r c u r r e n t , amps
"B" F i e l d
Primary c u r r e n t , amps
P r i m a r y v o l t a g e , vo l t s P r e c i p i t a t o r c u r r e n t , amps
7 /8 /74
1
3 2 2
2 6 2 0 - 2 6 5 0
1 4 6 0 - 1 4 6 5
1 0 2 0 - 1 0 4 0
6 8 3 - 7 0 0
6 6 0 - 6 7 5
7 /9 /74
3
3 5 6
2 6 0 0 - 2 6 5 0
1 4 5 0 - 1 4 7 5
1 0 0 0 - 1 0 3 5
6 8 5 - 7 0 0
6 6 0 - 6 9 0
7 / 1 0 / 7 4
5
3 7 5
2 5 9 0 - 2 6 2 0
1 4 7 0 - 1 5 2 0
1 0 5 0 - 1 0 8 0
7 0 0 - 7 2 5
6 7 0 - 7 0 0
3 9 - 5 0 37 -46 4 8 - 6 1
2 5 0 - 2 7 5 2 5 0 - 2 6 5 2 5 0 - 2 7 0
0 .20 -0 .30 0 . 1 9 - 0 . 2 3 0 . 2 0 - 0 . 3 2
4 1 - 5 5 50 -54 5 3 - 6 1
2 4 0 - 2 6 0 2 4 0 - 2 5 0 2 4 0 - 2 5 0
0 .27-0 .35 0 .28-0 .30 0 .32 -0 .37
a ) Obta ined by m u l t i p l y i n g i n d i c a t e d tonnage by (see Appendix D ) .
16 ~
i
ci .I e I i b CI 1 c P f c ci E i I I
1 T a b l e 6 . SULFUR CONTENT OF KILN, FUEL OIL, FEED ROCK, PRODUCT
AND EFFLUENT DUST.
Sample Date - #1 ESP C o l . Dus t #1 ESP C o l . Dus t #1 ESP C o l . Dust
# 2 ESP C o l . Dust # 2 ESP C o l . D u s t # 2 ESP C o l . D u s t #1 S t o n e F e e d #1 Rock Feed
#1 Rock F e e d .
#1 Rock Feed #2 Stone F e e d # 2 Rock Feed
# 2 Rock F e e d
# 2 K i l n P r o d u c t
#1 Lime P r o d u c t
#1 Lime P r o d u c t
#1 Lime Product # 2 Lime P r o d u c t
# 2 Lime P r o d u c t
#1 F u e l O i l
#1 F u e l O i l
# 2 F u e l O i l
# 2 Fuel O i l
# 2 F u e l O i l
#1 F u e l O i l
7/8/74 7/9/74
7/10/74 7/8/74 7/9/74
7/8/74 7/10/7,4
7/9/74 7/10/74 7/10/74 7/8/74 7/9/74
7/10/74 7/9/74 7/8/74 7/9/74
7/10/74 7/8/74
7/9/74 7/10/74
7/8/74 7/9/74
7/10/74 7/8/74
7/10/74
Time
1 8 3 0
1015 0800 2 0 3 0 1255 1 0 3 0 1750 1100 1700 1000 2036 1 2 3 0
1 3 0 0
1 3 0 0
1 7 2 0 0930 1000 2030
1230 0930 1900 1 2 3 0
1 2 3 0
2 0 3 0
1100
- S u l f u r Con ten t % by weight
0.9 1 . 3 2
1 . 2 8
0.78 1.16 1.64 0.02 0.07 0.06 0.07 0.14 0.04 0.04 0.01 0.07 0.04 0 . 0 2
0.06 0.07 1.75 2 . 2 6
1.7 - 0.875
3 . 2 2
2 . 2 6
17
I
i i f
. c 1 E 1 >.
1 0 . Except f o r t h e h e a v i l y loaded k i l n , p r o c e s s o p e r a t i o n s
appeared normal. Because o p a c i t y r e a d i n g s rose t o t h e 15
t o 20 p e r c e n t r a n g e , t e s t i n g w a s s topped a t 4:30 p . m . Cleanup
o p e r a t i o n s l a t e r r e v e a l e d t h a t t h e sampling p robe w a s broken.
The v a l u e s o b t a i n e d i n t h i s t e s t were t h e r e f o r e d i s c a r d e d ,
and f u r t h e r sampling w a s s chedu led f o r t h e f o l l o w i n g day .
On t h e morning of Ju ly 11, however, stack o p a c i t y v a l u e s
were a g a i n r a n g i n g between 5 and 1 0 p e r c e n t . Al though p l a n t
p e r s o n n e l t r ied s e v e r a l v a r i a t i o n s i n k i l n o p e r a t i o n , t h e
h igh o p a c i t y r e a d i n g s p e r s i s t e d th roughou t t h e day and even ing .
A r e a d i n g a t 10:30 p.m. gave v a l u e s between 20 and 25 p e r c e n t .
A t 6:OO a . m . on J u l y 12, o p a c i t y r e a d i n g s s t i l l ranged
between 5 and 1 0 p e r c e n t . P e r s o n n e l of t h e Woodville p l a n t ,
EPA, and PEDCo a g r e e d t h a t t h e k i l n shou ld be shutdown b r i e f l y
for i n s p e c t i o n . Examination o f t h e ESP r e v e a l e d t h a t s e v e r a l
charge p l a t e s were covered w i t h a b o u t 1 i n c h of a s t i c k y
s u b s t a n c e , which p r e v e n t e d t h e d u s t p a r t i c l e s i n t h e e f f l u e n t
from r e c e i v i n g t h e p o s i t i v e c h a r g e and t h u s reduced c o l l e c t i o n
e f f i c i e n c y . It w a s e s t i m a t e d t h a t ' c l e a n i n g o f t h e p l a t e s
would r e q u i r e shutdown of t h e k i l n f o r a week or so. A
shutdown w a s s chedu led f o r t h e week o f J u l y 15 t o allow
Clean ing of t h e ESP, r e b r i c k i n g o f c e r t a i n k i l n s e c t i o n s , ,
and r o u t i n e p e r i o d i c main tenance . F u r t h e r emis 'sions t e s t i n g
w a s t o be conducted s h o r t l y a f t e r resumpt ion of k i l n o p e r a t i o n .
18
V I I . SAMPLING AND ANALYTICAL PROCEDURES
Sampling p rocedures were d e s i g n a t e d by EPA. Analyses of
c o l l e c t e d samples w e r e performed by PEDCo. Appendix H p r e s e n t s
d e t a i l e d sampling and a n a l y t i c a l p rocedures .
V e l o c i t y and Gas Temperature
Gas v e l o c i t i e s were measured w i t h a c a l i b r a t e d t y p e S
p i t o t tube and i n c l i n e d d r a f t gage. V e l o c i t i e s w e r e measured
a t each sampling p o i n t a c r o s s t h e s t a c k d i ame te r t o de te rmine
an average v a l u e acco rd ing t o p rocedures d e s c r i b e d i n t h e
F e d e r a l Reg i s t e r ' - Method 2 .
t h e u s e of a thermocouple .
blolecular Weight
Temperatures were measured w i t h
A 4-hour i n t e g r a t e d sample of t h e s t a c k g a s e s was c o l l e c t e d
d u r i n g t e s t 1 by pumping t h e g a s i n t o a T e d l a r p l a s t i c bag a t
t h e r a t e of approximate ly 0 . 0 0 5 CFM. T h i s bag sample w a s t h e n
ana lyzed w i t h an O r s a t a n a l y z e r f o r CO
i n t h e F e d e r a l R e g i s t e r , Method 3.
Pa r t i cu la t e s
and CO as d e s c r i b e d 2 ' 0 2 t
C o n c e n t r a t i o n s o f p a r t i c u l a t e matter i n s t a c k g a s e s were
measured by Method 5 as d e s c r i b e d i n F e d e r a l R e g i s t e r ?
t r a i n c o n s i s t i n g of a h e a t e d g l a s s - l i n e d p robe , a 3- inch d i a m e t e r
A r i g i d
1) F e d e r a l R e g i s t e r , V o l . 36, N o . 2 4 7 , December 23, 1 9 7 1 . 2 ) F e d e r a l R e g i s t e r , V o l . 3 6 , N o . 1 5 9 , August 17, 1 9 7 1 .
19
i 1
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glass-fiber filter, and a series of Greenburg-Smith impingers
was used for particulate sampling, as shown in Figure 2.
Sampling was conducted under isokinetic conditions by
monitoring stack-gas velocity with a pitot tube and adjusting
the sampling rate accordingly.
The particulate sample was recovered by triple-rinsing
the nozzle, probe, cyclone by-pass, and front half of the filter
holder with acetone into a glass container. The back'half of the
filter holder, impingers, and connecting tubes were rinsed with
distilled water and the washings placed in a glass container with
the impinger contents. These components were then triple-rinsed
with acetone into another glass container. The filter was
placed in a separate container. Blank samples of water and
acetone were also taken.
NO -X
Nitrogen oxides were collected in evacuated 2-liter
flasks containing 25 ml of a dilute sulfuric acid/hydrogen
peroxide absorbing solution.
procedure was as described in Method 7 of the Federal Register
except that the final flask vacuum was read immediately after
sampling.
so -2
The sampling and analytical 1
._ Sulfur dioxide sampling procedures followed chose described
in Method 6. However, due to the low expected concentrations,
1) Federal Register, Vol. 3 6 , No. 247 , December 23, 1971.
20
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larger sampling equipment was used. Flue gas was passed
through a set of Greenburg-Smith impingers at a rate of
approximately 0.8 cubic foot per minute. The first impinger
contained 150 ml of 8 0 percent isopropanol; the second and
third impingers contained 100 ml each of 3 percent hydrogen
per6xide/water solution. After sampling, ambient air was passed
through the train for 10 to 15 minutes. The isopropanol solution
was discarded, and the peroxide solution rinsed into a.glass
container. The hydrogen peroxide solution was titrated with
barium chloride, using a Thorin indicator as described in
Method 6 .
Visible Emissions
Visible emissions were determined according to procedure,
in Method 9. Readings were difficult to determine at times due
to trucks loading and unloading ESP dust and quarry rock in the
vicinity of either the ESP unit or the observer and the light
colored plume against an overcast and partly cloudy sky caused
poor distinction. In additioh, certain ESP rappers set up
a visible emission condition (puffs) that read approximately
5 to 10 percent opacity for about 2 to 3 seconds every cycle.
Sulfur Analysis
Solid samples were analyzed using Standard Methods of
Chemical Analysis of Limestone, Quicklime and aydraded Lime,
C25-67, A.S.T.M. Standards, Part 9, Cement; Lime;’Gypsum, 1972,
American Society for Testing and Materials, Philadelphia, Pa.
22 .
i
Fuel oil samples were analyzed using Standard Method of Test
for Sulfur in Petroleum Products by the Bomb Method, D 129-64,
A.S.T.M. Standards, Part 17, Petroleum Products - Fuels, Solvents, Burner Fuel Oils, Lubricating Oils, Cutting Oils, Lubricating
Greases, Hydraulic Fluids, 1972, American Society for Testing
Materials, Philadelphia, Pa.
I b i
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.
23
i i b r 1 I i i c E i I c E N
'B . I' I I'
APPENDIX A
PARTICULATE RESULTS AND
EXAMPLE CALCULATIONS
Table Al. SUMMARY OF PARTICULATE RESULTS 1
i 'i P
3 - 5 - 1 - 7/8/74 7/9/74 7/10/7 4
1713 0841 8 24 2129 1248
ESP O u t l e t ESP O u t l e t ESP O u t l c
0.375 0.375 0.375
240 240 240
29.48 29.48 29.40
11.26 12.14 11.40
.E874 .E786 .E860
21.66 21.0 19.6
8.0 8.67 11.4
0 0 0
70.34 . . io.33 69.0 ..
74.7 86.4 164
i I
. . - . __
S t i i t i c 1'1-cssui-e oE S t a c k i l l : llq
1 -
30.23
.83
621
48
0.03
29.51
2928
21.992
27619
64393
102.9 -
%Lfa
781.1
1704.6
54.2
0.051
0.111 .
3 -
30.04
.83
669
48
0.03
29.51
3060
21.992
27390
67296
104.5 -
* 718.9
989.9
24.4
0.046
0.064
5 - 30.04
.83
67 4
48
0.03
29.43
3198
21.992
28658
70330
103.6 - -
417.0
889.3
53.1
0.026 . 0.055
. . ---.. : : \ A 1 1 ;:f.J. Table A1 ( con t inued) ‘I
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CALCULATIONS I i ci; 4 1.
1. Volume of d r y 3 g a s sampled a t s t a n d a r d c o n d i t i o n s - 7 0 ° F , 2 9 . 9 2 " Ilg. f t .
1 7 . 7 1 X 2 5 6 . 9 1 1 ( 2 9 . 4 8 + 3.01 - - 1 3 . 6 - -
s td vrn
V o l u m e of water v a p o r a t 7 0 ° F & 2 9 . 9 2 " Hg, F t . 3
( 1 0 8 . 5 + 4 6 0 ) (Tm + 4 6 0 ) = 237 .710
2.
= 0 . 0 4 7 4 X Vw = F t . 3 = ( 0 . 0 4 7 4 ) ( 6 3 6 . 7 ) = 3 0 . 1 8 0 gas
vW
100 x vw %M = gas = 1 0 0 X 3 0 . 1 8 0 = 1 1 . 2 7
237 .710 + 3 0 . 1 8 0 + vw s td . gas 'm
4. Mole f r ac t ion of d r y gas
3. % m o i s t u r e i n s t a c k gas
= 100 - % M = 1 0 0 - 1 1 . 2 7 = .E873 100 100
Md
5. Average molecular w e i g h t of d r y s t a c k gas
M W = ( % C 0 2 . X 44) + ( % 0 2 X 3 2 ) + ( % N X 2 8 ) 2 - ~
100 100 i o 0 = ( 2 1 . 6 6 X . 4 4 ) + (8 X . 3 2 ) + ( 7 0 . 3 4 X . 2 8 )
= 3 1 . 7 9
6. Molecular weight of s t a c k gas
M W = M W d X Md + 1 8 (1 - Md)
(31.79) ( .8873) + ( 1 8 ) (1-.8873) = 30.23
7 . S t a c k v e l o c i t y @ s t a c k c o n d i t i o n s , fpm
= 1062.6c X%P X (Ts +
= 2923
vs P
= (1062.6) ( . 83 ) C.389) (621+460) 1 (29.51) (30.23)
8. S t a c k gas volume @ s t a n d a r d c o n d i t i o n s , SCFM
1 7 . 7 1 x v x A~ x M~ x pS s = (17.71) (2923) (21.992) (.E8731 (29.5 - Qs -
(621 + 460)
= 27576 (Ts + 4 6 0 )
9 . P r c e n t i s o k i n e t i c
1032 X (Ts + 460) X Vm
Vs X Tt X Ps X Md X (D,)
s t d - (1032) (621+460) (237.710) I - %I = I 2 (2923) (240) (29.51) (.E8731 ( .375)2 I
= 102.7
1 0 . P a r t i c u l a t e - p r o b e , c y c l o n e , & f i l t e r , gr/SCF
= 0.0154 X Mf - = (0.0154) (781.1) = 0.051 'an "rn s t d 237.710
I i i ‘ 1 e P t 1 ii c B f 5’ f
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11. P a r t i c u l a t e t o t a l , qr/SCF
M = - = (0.0154) (1704.6) = 0.11 ‘a0 . . I
V m s t d 237.710
12. P a r t i c u l a t e - probe , c y c l o n e & f i l t e r , qr/CF a t s t a c k c o n d i t i o n s
17.71 X Can X P X Ma S
= (17.71) (0.051) (29.51) (.8873) - - ‘at
(621 + 460) = 0.022 (Ts + 460)
13 . P a r t i c u l t 0 3 C c o n d i t .ons
17.71 X Cao X P X Ma S = (17.71) (0.11) (29.51) (.8873) - -
‘au (621 + 460)
(T, + 460) = 0.047
1 4 . P a r t i c u l a t e - probe , c y c l o n e , & f i l t e r , l b / h r .
Caw = 0.00857 X Can X Q, = (.00857) (.051) (27576) = 12.05
.. 15. P a r t i c u l a t e - t o t a l , l b / h r .
Cax = 0.00857 X Cao X R, = (.00857) (0.11) (27576) = 26.0
I I
i
F
i.
f
APPENDIX E
GASEOUS RESULTS AND
EXAMPLE CALCULATIONS
NO; CALCULATIONS
TEST A
I
1. Sample Volume
w h e r e : V = S a m p l e v o l u m e a t s t d . c o n d . , d r y S b a s i s , ml.
= Volume of f l a s k antl v a l v e , m l . Pf = F i n a l a b s o l u t e p r e s s u r e of f l a s k , in.IIcj. P . = I n i t i a l a b s o l u t e p r e s s u r e of f l a s k , i n . HCJ.
Tf = F i n a l a b s o l u t e t e m p e r a t u r e of f1asl:;R.
T . = I n i t i a l a b s o l u t e t e m p e r a t u r e of f l a s k , R.
vO
1
1
Vs = 1 4 5 7 n i l .
2 . PPb1 NO2
" S
w h e r e : C = C o n c e n t r a t i o n of NO ,PPEl . (d ry b a s i s )
M = Mass Of N O i n q a s sample, mg.
V = G a s s a m p l e v o J u m e 0 7 0 F antl 2 9 . 9 2 " I J < I .
2
2
S ~
C = . 2 9 8 . 8 PPM
I' 111 I
3 . L!3S/r117 NO2
M.W. EH = (PPM) (Q,) ( 6 0 G ) h r x 387 E t /lb-mole .- -
I
where: E-R = Emission R a t e in l h s / h r .
PPM= Parts per million N O 2 (dry basis) MW = Molecular weight of NO 4 6 . 0 1 2 '
E R = ( 7 . 1 3 3 ) (PPM) ( O s ) x
ER = ( 7 . 1 3 3 ) ( 2 9 8 . 8 ) ( 27619 , ) x
E17 = 58.9 LBS/€IR
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SO2 CALCULATIONS (Test 2 )
A H (Pbar + 13.6 Vmstd = Vm (Tstd)
(Tm) (Pstd) 1.90
( 180.062) (530) (29.48 + 13.6 Vmstd - ( 566) (29.92)
Vmstd = 166.917 std cu. ft.
- (Vt-Vtb) (N) (Vsoln) (.032) (24.5) (lo6) PPMS02 - (64) (28.316) (Va) (Vmstd)
PPMS02 = ( 28-52] (0.0188 ) (510 ) (.032) (24.5) (lo6) (64) (28.316) (10. ) (166.917)
PPMS02 = 70.8 ppm by volume
cS02 = (7.05~10-~) (Vt-Vth) ( H ) (Vsoln) (Vmstd) (Val
CS02 = (7.05~10-~) ( 28.52) (0.0188 ) ( 510) (166.917 ) (10 )
CS02 = 1.155~10-5 lb/std cu. ft.
Emission rate - (CS02) (Qsstd) (60) -5 Emission rate = (1.155X10 ) (27619 ) (60)
Emission rate = 19.1 lb/hr.
~~~~
SO2 CALCULATIONS ( T e s t 4 )
AH V m s t d = Vm ( T s t d ) ( P b a r + 13.6 I
(Tm) ( P s t d )
( 1 8 1 . 1 1 ) ( 5 3 0 ) ( 29 .48+ 13.6 Vrns td - i i (574 ) ( 2 9 . 9 2 )
Vrnstd = 1 6 5 . 5 4 9 s t d c u . f t . P I
.I i 0 E i
PPMS02 - - ( V t - V t b ) ( N ) (Vso ln ) ( . 0 3 2 ) ( 2 4 . 5 ) ' ( l o 6 ) ( 6 4 ) ( 2 8 . 3 1 6 ) ( V a ) (Vms t d )
PPMS02 = ( 3 - 1 2 ) (0 .0188 ) ( 6 5 0 ) ( . 0 3 2 ) ( 2 4 . 5 ) ( i o 6 ) ( 6 4 ) ( 2 8 . 3 1 6 ) ( 1 0 ) ( 1 6 5 . 5 4 9 )
PPMS02 = 1 0 . 0 ppm by vo lume
CS02 = ( 7 . O ~ X ~ O - ~ ) ( V t - V t h ) ( H ) (Vsoln)
( V m s t d ) ( V a )
( 1 6 5 . 5 4 9 ) ( 1 0 )
CS02 = 1 . 6 2 4 ~ 1 0 - ~ lb/s td cu . f t .
E m i s s i o n r a t e - ( C S 0 2 ) ( Q s s t d ) ( 6 0 )
E m i s s i o n r a t e = (1 .624XlO ) ( 2 7 3 9 0 ) ( 6 0 )
E m i s s i o n r a t e = 2 - 6 7 l b / h r .
-6
i I I I 0 s I I
I I P
1 0 I I U
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i
SO2 CALCULATIONS (TEST NO. 6)
AH (Pbar + 13.6 Vmstd = Vm (Tstd)
(Tm) (Pstd) 1.85
( 180.024) (530) (29.40 + 13.6 Vmstd - (565 ) (29.92)
Vmstd = 166.705 std cu. ft.
PPMS02 = (Vt-Vtb) (N) (Vsoln) (.032) (24.5) (lo6) (64) (28.316) (Va) (Vmstd)
PPMS02 = (17.90 ) (0.0188 ( 590) (-032) (24.5) (lo6) (64) (28.316) (10 l(166.705)
PPMS02 = 51.5 ppm by volume
CS02 = (7.05~10-~) (Vt-Vth) (H) (Vsoln) (Vmstd) (Va)
CS02 = (7.05~10-~) (17.90 )(0.0188 ) (590 ) (166.705 (10 )
CS02 =8.398~10-~ lb/std cu. ft.
Emission rate - (CS02)'(Qsstd) (60) Emission rate = ( 8 .397x10q6 ) (28658 ) ( 6 0 )
Emission rate = 14.4 lb/hr.
i I
i c c e
e e
APPENDIX D
OPERATING RESULTS
L
C
* C W 5 . w - 5 nn
I 1 i c1 E E c i I
b I
EL c ii E li ii i: i
(u - .
E E k b c i ci 1
?- .’
I Stone T c t a l i z e r ) ~ ' ~ ~ ~ - 5- Stone Riite
- r '-. , ,
%i,ing Zone Tempt
- ESP I n l e t Tempt ,
ESP Outlet Tenpt
ESP "A" Field
Primary Current
Prec ip i ta tor Current
ESP "B" Field
3$
t3/t1r
/,/
ainps ILz iE
4J.B
7- - 1 *2
c/G
. . .
t
/
- -. .
- /"
S t o n e Rate #-
Feed Erid K.i.ln 7 m p t
ES? In le t T m p t
Un.i t s
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G a l s . --
a l s / h r .
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1 I Primary Cwrent
Pt-eci p i t a t o r Current
ESP "E" Field
__ I ro: .- /Ob ; 7/11
k 1 d ,Gk.L'/Z x /+fK ty*~> LWXL 4,6i/J/o
CHRONOLOGICAL LIST OF NOTES TIIRQUGIiOUT PROJECT (NOT COVERED BY DAILY PERSONNEL AND LOG S H E E T )
i c E l c li c E
c: c; f c E l I 1
I
Office of (he Vice Presided Phone 849-4311
WOODVILLE. OHIO
August 2 3 , 1 9 7 4
EPA Mutual P l a z a Room 9 2 6 Research T r i a n g l e P a r k , N. C. 27711 '
At tn : M r . Gene R i l e y
Dear S i r :
Herewith e n c l o s e d p l e a s e - f h d c o p l e s o f your r e s e a r c h d a t a s h e e t s , w i t h t h e s t o n e ra te r e c a l c u l a t e d t o a more r e a s o n a b l e f i g u r e . T h i s i n f o r m a t i o n was p laces . i n your column f o r G a s T o t a l i z e r , which I have r e l a b l e d a s
The f a c t o r t h a t I used was S t o n e R a t e T/hr . T h i s f a c t o r t h e s t h e t D t a l inc?icatc$. tonnage
r e a s o n a b l e f i g u r e t o c a l c u l a t e t h e amount of 1 l i m e produced.
A s I i n d i c a t e d o u r o i l t o t a l i z e r gives u s a v e r y good i n d i c a t i o n of t h e t o t a l amount of o i l u s e d , b u t a s a whole I t e n d t o d l s c o u n t t h e hour by hour f i g u r e s .
Yours v e r y t r u l y , d
George Judd Chief C h e n i s t
..
I i i I P I 15 P # f ii I f i fi e L
1 c
APPENDIX E
FIELD DATA
- e-
SCHEihlTIC OF SAidPLING LOCATION
-- '(RA'JEifSE $,,AT LOCATION
IT.O;il OUTSIDE DF NIPPLE DISTANCE 0
C b h c E i ir li E E € c I I
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. , . .... 4 . i I ! . . .. S U I T E 6 . A T I ~ : I N ~ U N SOUA.HE
CINCINNATI . O H I O 4 5 2 4 6 513 /771-4330
ANALYTICAL DATA i
W6nD J l.LLF L I .Vr(^ co. Date 7 -&--I
2 . Sampling l o c a t i o n L ' \ ~ F U \ L ~ W , I e? O C V L a Run. N o . 1 3 . Sample Type sL~l.W~~c Rr i v Y M \ F , r Sample BOX N O . 4 4 . Clean-up Man F- ~ ~ V 0 1 ~ 5
I
MOISTURE MUTE: S \ L I ' ~ ( ) W L WfiS 5l\-Tuem IMP I NGE RS SILICA GEL
c 1 F i n a l Volume -1,58 ML F i n a l N t . 773.79. 9. g. ,558
3 3 . 2 g * /
ML N e t W t . . <>-Jg. g . '9. 3 9 f ' 7 I n i t i a l Volume 300 ML I n i t i a l W t . zoo&. 9.
TOTAL MOISTURE ,7,q1,> g. N e t Volume SSK
92or 3 - k . LABORATORY RESULTS .hpp!? at3 1 2 3 4 . 5 6 7
E C' 5
# k t I E 11 II
i
i
GROSS TARE BLANK
FRONT HALF
Acetone wash o f n o z z l e , p robe , cyc lone ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r h o l d e r .
F i l t e r Number
Water wash of n o z z l e , p robe , cyc lone ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r h o l d e r .
BACK HALF
I m p i n g e r , c o n t e n t s and water wash of imp inge r s , c o n n e c t o r s , and back h a l f o f f i l t e r h o l d e r .
Acetone wash o f i m p i n g e r s , connec tors , and back h a l f of f i l t e r h o l d e r
7
Conta ine r 1. m g
C o n t a i n e r 2 . my
Water 3. m g Con ta ine r
Con ta ine r Ether-Chloroform E x t r a c t i o n 4 . mg
FRONT HALF SUBTOTAL mg
Conta ine r Impinger Water ._ 5 . lllg
Con ta ine r Ether-Chloroform E x t r a c t i o n 6 . mg
Con ta ine r 7 . mg
BACK HALF SUBTOTAL mg
TOTAL WEIGHT mg
,_ .. -. .... ~
i e h I # L
I - 'L;LLJLrJ-tLIuvl I \ 'Ol \ ln,L-_l \ l I A L S U I T E 8 . A T K I N S O N S Q U A R E
C I N C I N N A T I . O H I O 4 5 2 4 6 i 513 1771 .4330
ANALYTICAL DATA
1 1. P l a n t w->yi /L4 & /z Date 7- ?- 77 2 . Sampling l o c a t i o n //e& KILN &st/ d 7 ~ & Run No. 9 3 . Sample Type 3 D., Sample Box No. --
3 1-5 6 b/.' 4 . Clean-up Man J . L . P
MOISTURE 3 P F i n a l W t . q / / J g . 9. 9.
I n i t i a l Volume ,cm ML I n i ti a 1 W t . +'dd 09 . 9 . g . N e t Volume ? I 5 ML N e t W t . F [ g . 9. 9.
2IlK SILICA GEL
b & ML
0 IMPINGERS F i n a l Volume
TOTAL MOISTURE g . 3U6.l
LABORATORY RESULTS 1 2 3 ' 4 . 5 6 1
GROSS TARE BLANK
FRONT HALF
A c e t o n e wash of n o z z l e , p r o b e , cyc lone C o n t a i n e r 1. ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r
h o l d e r .
F i l t e r Number C o n t a i n e r 2 .
Water wash of n o z z l e , p robe , c y c l o n e C o n t a i n e r ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r Water 3 . h o l d e r .
C o n t a i n e r Ether-Chlorof orm E x t r a c t i o n 4 .
FRONT HALF SUBTOTAL
'BACK HALF
Impinger c o n t e n t s a.nd water wash of imp inge r s , connec to r s ' , and back C o n t a i n e r h a l f of f i l t e r h o l d e r . Impinger Water 5.
m9
m 9
m9
lllg
C o n t a i n e r Ether-Chloroform E x t r a c t i o n 6 . m9
Acetone wash of i m p i n g e r s , c o n n e c t o r s , I and back h a l f of f i l t e r h o l d e r C o n t a i n e r 1. m9
1 BACK HALF SUBTOTAL 'nY
TOTAL WEIGHT m9
. . . . ..
I LLL)LU L 4 4 1 I 1 .S.JIUl\ 6 - i . 1 ,--\I SUITE e . ATKINSON S O U A R E
CINCINNATI, OHIO 4524p 5 1 9 /771-433,O
ANALYTICAL DATA
a 1. P l a n t x/z L l h - 4 Date 7-\0-7c( - 2 . Sampling l o c a t i o n < I A ~ A q 6 0 / X k r Run N o . b 3 . Sample Type sox Sample Box No.
4 . Clean-up Man f. E 4 ( i > O W S
'i b
MOISTURE IMPINGERS S I L I C A GEL
$0 3 M L F i n a l W t . 497,&. 9 . 9 .
N e t Volume %Lo 4 ML g . 9 .
F i n a l Vo lume I n i t i a l Volume 600 ML ;;;t;;: W t . +gy¶: 9. 9.
c ybp 60% i:,;TOTAL MOISTURE 9 .
vor LABORATORY RESULTS
1 2 3 4 . 5 6 7
GROSS TARE BLANK
FRONT HALF
1. m q Acetone wash of n o z z l e , p r o b e , c y c l o n e C o n t a i n e r ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r
h o l d e r .
2 . F i l t e r Number C o n t a i n e r
Water wash of n o z z l e , p robe , c y c l o n e C o n t a i n e r Water 3 . mg ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r
h o l d e r . C o n t a i n e r Ether-Chloroform E x t r a c t i o n 4 . mcJ
mY FRONT HALF SUBTOTAL
BACK HALF
Impinger c o n t e n t s and w a t e r wash of imp inge r s , c o n n e c t o r s , and back Con ta ine r h a l f of f i l t e r h o l d e r . Impinger water 5 . lllq
E x t r a c t i o n 6 . mcJ
C o n t a i n e r 7 . mq
BACK HALF SUBTOTAL m 9
C o n t a i n e r Ether-Chloroform
Acetone wash of i m p i n g e r s , c o n n e c t o r s , and back h a l f of f i l t e r h o l d e r
TOTAL WEIGHT mg
i. i il" c. I f c c c e i c f 5 E 1
.
i
h I c li c f 0 1 C Y c E a E h ci
I
i PEDCo - EPlVII3ONMEIVTAL ..........................
C I N C l N N 4 T I . Gt.10 LIZ.,,,
I
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i :I i. 9 11 B c e I! P E 4 I! h il c CI 1 c 1 I
c
F
Projcct N O . 3082-y
PEDCo - ENVIRONMENTAL " " I T L $ ? . .7m1..,*11 . , c , Y L u r
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! e e b I t R r CI 6 c I I I
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LOCATION
i E r-
p_- ... .......... . ..... 3 , - I I~ST NO. DA'I 'I~ LOCATION
APPENDIX F
SAMPLE IDENTIFICATION LOG
I .
E?A I.!uinber Saniole Location Run c o n t e n t s Cornri:ents
SAMPLE IDENTIFICATION LOG _ - .
b 1 .
&j% 1 \ I .
71: . I :
SBi*IPLE IDENTIFICATION LOG
SAMPLE IDENT I F I CAT I ON LOG
--
c c B c G G c c e E 1 I c c
I
I I
APPENDIX G
LABORATORY REPORT
I I
~ U I T L u . ; ~ T K I N S O ~ ' ~ S ~ ) U A N : . CINCINNATI , OHIO 4 5 2 4 6
513 / 7 7 1 - 4 3 3 0
ANALYTICAL DATA
, 1. P l a n t h,/,F,C I, , P , , w e - Date 7/59 /74
2 . Sampling l o c a t i o n &5p &,,f/&f Run No. / :.
3 . Sample Type A r #l>//L, 766 Sample Box No. 2.
ML F i n a l W t . H 7 g . g . 4 - F i n a l Volume I
I n i t i a l Volume z&@ ML I n i t i a l W t . w g . g. 4. N e t Volume 5?Zz ML N e t W t . 447 g . 9. 4 .
TOTAL MOISTURE 6 7 g . LABORATORY RESULTS
1 2 3 4 5 . 6 I
FRONT HALF
Acetone wash of n o z z l e , p r o b e , cyc lone ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r h o l d e r .
F i l t e r Number a//,% Water wash of n o z z l e , p r o b e , c y c l o n e
(bypass ) ; f l a s k , f r o n t h a l f of f i l t e r h o l d e r .
C o n t a i n e r 197 1. e,/ mg
C o n t a i n e r Water 3 . m 9
C o n t a i n e r Ether-Chloroform E x t r a c t i o n 3 . m 9
FRONT HALF SUBTOTAL n/. / mg
BACK HALF
Impinger c o n t e n t s and water wash of imp inge r s , connectors, and back h a l f of f i l t e r h o l d e r .
Acetone wash o f i m p i n g e r s , c o n n e c t o r s , and back h a l f of f i l t e r h o l d e r
C o n t a i n e r 6'99 Impinger 1Jate.r 5 . y/: 2 lug
C o n t a i n e r 700 Ethe r -Ch lo ro fo r6 E x t r a c t i o n 6. 370.5q
C o n t a i n e r &9r 7 . &/,% mg
BACK HALF SUBTOTAL 723,gmq
, ._ ,.. 'L: J I . . .. ." 0 I 'i LJ I . I I ' I i . 8 . , ! I L . .
S U I T E t3 . A T K I N S O N S O U A W L C I N C I N N A T I . OHIO 4 5 2 4 6
! 513 /771-4330
ANALYTICAL DATA
1 . 4 1. P l a n t ~ ~ . / ~ ; / / p . ~ , . ~ , - ~ 4 .
c I c
Date 7-7.-7+
2 . Sampling l o c a t i o n . ,=.%p f- - Run No. -3
4 ; Clean-up Man - JL.A
F i n a l Volume . 5 4 ~ ML F i n a l W t . 6.y-r-5g. 9.. 9. I n i t i a l Volume 2~) ' FTL . I n i t i a l W t g w g . 9. ' g - N e t Volume &A4 ML N e t W t . 98&7 * 9 . g .
3 . Sample Type /& j , A // /&7& ,sample Box N O . 4
MOISTURE IMPINGERS SILICA GEL
TOTAL MOISTURE B s F r;- g . . .
LABORATORY RESULTS 1 2 3 4 5 6~ 7
FRONT HALF
Acetone wash of n o z z l e , p r o b e , cyc lone C o n t a i n e r 75d 1. x+--?&mq ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r
e I h o l d e r .
F i l t e r Number /m//+ Water wash of n o z z l e , probe, cyc lone
( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r h o l d e r .
BACK HALF
Impinger c o n t e n t s and water wash of imp inge r s , c o n n e c t o r s , and back h a l f of f i l t e r h o l d e r .
Acetone wash of impingers , c o n n e c t o r s , and back h a l f of f i l t e r h o l d e r
C o n t a i n e r zc&- 2 . .7c/T:ymg
Con ta ine r Water 3 . my
C o n t a i n e r Ether-Ch l o r o f orm E x t r a c t i o n 4 . ' mg
FRONT HALF SUBTOTAL 7/5.9 mg
Conta ine r 73-g Impinger Water 5 . &?7,d l l l r j
Con ta ine r y e Ether-Chloroform E x t r a c t i o n 6. #;Z/ nig
Con ta ine r 73'7 7 . 757 my
BACK HALF SUBTOTAL 271 0 m y
TOTAL WEIGHT 9-83, 9 "'9
I ,... L 2 L . 1 ... , . - , ~ J ' < . ,I'.L..JIuI\IL..,-I I . - \ L .
SU ITE o . ATKINSON SUUARL- C I N C I N N A T I . OHIO 45246
513 /771-4330 i l 1
!I ANALYTICAL DATA
i . 1. P l a n t Date 7-/& - 74 11 '2 . . Sampling l o c a t i o n P Run No. 5
3 . Sample Type diu I A47 Sample BD'X N O . ' / 1..
4 . Clean-up Man # # *
MOISTURE I M P I N G E R S S I L I C A GEL F i n a l Volume ML F i n a l W t . ,425- g . 9. 9. I n i t i a l Volume a/ M L I n i t i a l W t g . 9. 9. N e t Volume ML N e t W t . Z T 9. 9 - g.
TOTAL MOISTURE A75 9. - LABORATORY RESULTS
1 2 3 4 5 6 7
FRONT HALF U
Acetone wash of n o z z l e , p r o b e , cyc lone Con ta ine r 777 1. /sz. 9 m g ( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r 1 h o l d e r .
F i l t e r Number ,!!~/,$1< Water wash of n o z z l e , p r o b e , cyc lone
( b y p a s s ) , f l a s k , f r o n t h a l f of f i l t e r h o l d e r .
BACK HALF
c r
Impinger c o n t e n t s and w a t e r wash of imp inge r s , c o n n e c t o r s , and back h a l f of f i l t e r h o l d e r .
L
Acetone wash of i m p i n g e r s , c o n n e c t o r s , and back h a l f of f i l t e r h o l d e r
C o n t a i n e r 77& 2 . 29. i m g
Con ta ine r Water 3 . mg
Con ta ine r Ether-Chloroform
4 . mg E x t r a c t i o n
FRONT HALF SUBTOTAL 4 / z & m g
C o n t a i n e r 77-c Impinger Water 5. /m, / r11(3
C o n t a i n e r 776- Ether-Chloroform
C o n t a i n e r 774 7 . /~3.7 mg
BACK HALF SUBTOTAL .+72.'3mg
. . ,
. . I
L:
r r
PEDCo-ENVIRONh\ENrAL SPECIALISTS, INC . MEMORANDUM
10: R . Gerstle DATE: O C t . 2 9 , 1 9 7 4
SUBJECT: W o o d v i l l e Lime
~
cc: Wm. DeWees
F o l l o w i n g are t h e r e s u l t s of a n l a y s i s of t h e r o c k a n d o i l samples
from Woodville Lime.
Sample
#1 ESP C o l D u s t #1 ESP C o l D u s t #1 ESP C o l D u s t # 2 ESP C o l D u s t # 2 ESP C o l D u s t # 2 ESP C o l D u s t #1 S t o n e #1 Rock #1 Rock #1 Rock # 2 S t o n e # 2 Rock # 2 Rock # 2 K i l n #1 L i m e ( '1 1 I #1 Lime #1 Lime # 2 Lime # 2 Lime
#1 K i l n F u e l O i l #1 F u e l O i l # 2 K i l n F u e l O i l # 2 F u e l O i l # 2 K i l n F u e l O i l #1 F u e l O i l
Date - 7/8/74
7 /10 /74 7 /8 /74
7 /10/74 7/8/74
7 /10/74 7 /10 /74
7 /9 /74
7 /9 /74
7/9/74
7/9/74
7 /9 /74 7 /8 /74
7 /10/74 7 / 8 / 7 4 7 /10/74
7 /9 /74
7 /9 /74 7 /8 /74
7 /10/74 7 /8 /74 7/10/74
R e s u l t s ~~ - Time Ef'd (mg S/grams of s a m p l e )
1 8 3 0 740 9 . 0 5 74- 061 -
1015 7 5 2 1 3 . 2 0 8 0 0 76f 1 2 . 8 2030 74 I 7 . 8 1 2 5 5 1 0 3 0 1 7 5 0 1 1 0 0 1.7 0 0 1 0 0 0
1 2 3 0 1 3 0 0 1 3 0 0 1 7 2 0 0 9 3 0 1 0 0 0 2030 1 2 3 0
0 9 3 0 1 9 0 0 1 2 3 0 1 2 3 0 . 2 0 3 0 1 1 0 0
2 0 3 6
7 5 3 1 1 . 6 2 7 0 1 6 . 4
7 93 0 . 7 0 . 6
7 33. 0 . 2
7
7 6 0 0 . 7 7 3 r 1 . 4
761 0 . 4 74 4 0: 4
7 5 0 1 . 0 737 0 . 7 z9 9 0 . 4 26; 0 . 2 7 3 b' 0 . 6 2 6 7 0 . 7
w 6 . 1 7 . 5 4 2 3 9 2 2 . 6 3 c/*ll.- 1 7 . 1 2 767 .> . 8 . 7 5 23 5 3 2 . 1 6 763 2 2 . 5 6
S o l i d s w e r e a n a l y z e d u s i n g S t a n d a r d M e t h o d s of Chemical A n a l y , s i s - of L i m e s t o n e , Q u i c k l i m e , and f l y d r a d e d L ime , C25-67 , A.S.T.M. S t a n d -
a r d s , P a r t 9 , Cement : L ime; Gypsum, 1 9 7 2 , Amer ican S o c i e t y fo r
- -
e
I
TO: R. Gerstle - 2- Oct. 29, 1974
Testing and Materials, Philadelphia, Pa.
Fuel oil samples were analyzed using Standard Method of Test for Sulfur in Petroleum Products & the Bomb Method, D 129-64,
A.S.T.M. Standards, Part 17, Petroleum Products - Fuels, Solvents, Burner Fuel Oils, Lubricating Oils, Cutting Oils, Lubricating
Greases, Hydraulic Fluids, 1972, American Society for Testing
Materials, Philadelphia, Pa.
- - --
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1 1 E E l! c ! 1 r e Q c c I I
?
I I ,
I APPENDIX H
SAMPLING METHODS
_ _
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r I t .
k a I! E r 1
e b I! I! E e! c 1 I
I I I
1
DETERMINATION OF PARTICULATE EMISSIONS
The following method was used in this test program.
Sampling procedures followed those described in the Federal
Register. 1
SAMPLING APPARATUS
The particulate sampling train used in these tests met
design specifications established by the Federal EPA and was
assembled by PEDCo personnel. It consisted of:
Nozzle - Stainless steel (316) with sharp, tapered leading edge and accurately measured round opening.
Probe - Pyrex glass with a heating system capable of maintaining a minimum gas temperature of 25OOF at the exit end during sampling.
Pitot Tube - Calibrated type S attached to probe to monitor stack gas velocity.
Filter Holder - Pryex glass with heating system capable of maintaining minimum temperature of 225'F.
Draft Gage - An inclined manometer made by Dwyer with a readability of 0.01 inches H20 in the 0-1 inch range was used.
Impingers - Four impingers connected in series with ,
glass ball joints. The first, third, and fourth impingers were of the Greenburg-Smith de'sign, modified by replacing the tip with a 1/2 inch I.D. glass tube extending to 1/2 inch from the bottom of the flask. The second impinger was of the Greenburg-Smith design with a standard tip.
Thermometer - Dial type with long stem.
Federal Register, Vol. 36, No. 241, Part 11, December 23, 1971.
c I I
Metering System - Vacuum gauge, leak-free pump, ther- mometers capable of measuring temperature to within 5OF, dry gas meter with 2 % accuracy, and related equipment, to maintain an isokinetic sampling rate and to determine sample volume. The dry gas meter is made by Rockwell and the fiber vane pump is made by Gast.
Barometer - Bourden tube type to measure atmospheric pressures to - + 0.1 inches Hg.
SAMPLING PROCEDURE
After selecting the sampling site and the minimum
number of traverse points, the stack pressure, temperature,
moisture, and range of velocity head was measured according
to procedures described in Method 1 of the Federal Register
(December 23, 1971).
Approximately 200 grams of silica gel were weighed in a
sealed impinger prior to each test. Glass fiber filters*
(3'' diameter) were desiccated for at least 2 4 hours and
weighed to the nearest 0.1 milligram on an analytical
balance. One-hundred ml of distilled water was placed in
each of the first two impingers: the third impinger was
initially empty: and the impinger containing the silica gel
was placed next in series. The train was set up without the
probe as shown in Figure A-1. The sampling train was leak
checked at the sampling site by plugging the inlet to the
filter holder and pulling a 15 inch Hg vacuum. Leakage
rates of less than 0.02 cfm at a vacuum of 15 in. Hg were
recorded in all cases. The probe assembly was then attached,
and crushed ice placed around the impingers. More ice was
added during the run to keep the temperature of the gases
leaving the last impinger at approximately 70°F. - MSA 1106 BH
Y u cz
+A, 0 W L n W
.r cc 0 w 2 m s u a
t- rn
u -2
During sampling, stack gas and sampling train data were
recorded at each sampling point and when significant changes
in stack flow conditions occurred.
rates were set throughout the sampling period with the aid
of a nomograph.
Isokinetic sampling
SAMPLE RECOVERY PROCEDURE
The sampling train was moved carefully from the test
site to the cleanup area.
used in the sample recovery were taken for use as blanks.
Samples of the acetone and water
The sample fractions were recovered as follows:
Container No. 1 - The filter was removed from its holder and placed in a petri dish and sealed.
Container No. 2 - Loose particulate and acetone wash- ings from all sample-exposed surfaces prior to the filter were placed in a glass jar and sealed. Par- ticulate was removed from the probe with the aid of a brush and acetone rinsing.
Container No. 3 - The condensate from the first three Greenburg-Smith impingers was measured within -t 1 ml and placed into a glass jar. Water rinsings from the back half of the filter holder, all connectors, and the first three Greenburg-Smith impingers were placed in this container and the container sealed.
Container No. 4 - Acetone rinsings from the back half of the filter holder, support, all connectors, and the first three Greenburg-Smith impingers were placed in this container and sealed.
Container No. 5 - A minimum of 300 ml of acetone was taken for the blank analysis.
Container No. 6 - A minimum of 300 ml of..distilled water was taken for'a blank.
The silica gel from the fourth impinger was weighed and
recorded. The used silica gel was discarded.
I!
I I
ANALYTICAL PROCEDURES
The following procedures were used and follow the
methods described in the Federal Register of August 17,
1971. 1
Container No. 1 - The filter and any loose particulate matter from this sample container were placed into a tared glass weighing dish, desiccated to a constant weight and weighed to the nearest 0.1 mg.
Container No. 2 - The acetone washings were transferred to a tared beaker and evaporated to dryness at ambient temperature and pressure; desiccated to a constant weight; and weighed to the nearest 0.1 mg.
Container No. 3 - Organic matter from the impinger solution was extracted with three 25 ml. portions each of ethyl ether and chloroform. The extracts were combined into a tared beaker, and evaporated until no solvent remained at about 70'F. The sample was then desiccated to a constant weight and weighed to the nearest 0.1 mg. The remaining water was evaporated by boiling in a tared beaker, and the residue weighed.
Container No. 4 - The acetone washings from the back half of the filter holder, connectors and first three Greenburg-Smith impingers were transferred to a tared beaker; evaporated to dryness at ambient temperature and pressure; desiccated to a constant weight; and weighed to the nearest 0.1 mg.
Container No. 5 - The acetone blank was transferred to a tared beaker, and evaporated to dryness at ambient temperature and pressure. The blank was then desic- cated to a constant weight and weighed to the nearest 0.1 mg.
Container No. 6 - The water blank was evaporated by boilinq in a tared beaker, desiccated to a constant weight; and weighed to the nearest 0.1 mg. corrections were made in proportion to the amount of
Blank
reagent used. ..
Federal ,Register, Vol. 36, No. 159, Part 11, August 17, 1971.
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Il Q I! I! P I!
G G E c c !
i .
4
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I
I
DETERMINATION OF NITROGEN OXIDES IN STACK GAS:
PHENOLDISULFONIC ACID METHOD
INTRODUCTION
The following method was used to determine total oxides
of nitrogen. Samples were collected in evacuated flasks con-
taining a dilute sulfuric acid-hydrogen perox
tion, and the nitrogen oxides, except nitrous
spectrophotometrically at 410 nm.
REAGENTS
de absorbing solu-
oxides were measured
The following reagents were used in this sampling program:
(All chemicals were ACS analytical-reagent grade.)
Water - Distilled - deionized water. - Hydrogen Peroxide ( 3 % ) - 10 ml. of 30 percent H202 was
diluted to 100 ml in a 100 ml volumetric flask with water.
Absorbing Reagent - 2 . 8 ml of concentrated H2S04 was diluted to one liter with distilled water. After mixing well, 6 ml of 3 percent hydrogen peroxide were added. The solution is prepared fresh every two or three days.
in distilled water and diluted to one liter. Sodium Hydroxide (1 N) - 4 0 gm of NaOH were dissolved
Ammonium Hydroxide (concentrated) c
Sulfuric Acid (fuming) - (15-18% SO3)
Phenoldisulfonic Acid Solution - 25 grams of pure white phenol were dissolved in 150 ml of concentrated H2S04 on a steam bath. After the solution cooled, 75 ml fuming sulfuric acid were added. It was then heated to l0O'C for two hours. The reagent was stored in a dark stoppered reagent bottle.
~
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I
Potassium Nitrate Solution (standard) - 0.5495 grams of KN03 were dissolved in one liter of water in a volumetric flask. 100 ml of this solution was diluted to one liter in a volumetric flask. One ml of the final solution was equivalent to 0 . 0 2 5 mg NO2.
SAMPLING APPARATUS
Flasks - Two-liter, Pyrex, round-bottom flask were encased in a simple container with a sleeve and accompanying stopcock valve as shown in Figure A-2.
Vacuum System - The vacuum system consisted of a vacuum pump, capable of producing a vacuum of 3 inches Hg absolute pressure, connected to a 0-36" Hg u-tube manometer.
Thermometer - Dial thermometer, range 25 to 125'F. 5-inch stem.
Probe - Pyrex glass, heated, with a filter to remove par- ticulateatter .
Variable Transformer - Rated at 12 amps, 0 to 140 volts. Spectrophotometer - A Bausch & Lomb Spectronic .70, capable
of measurinq optical density at 410 nm in 0 . 5 inch absorbance cells was used-.
-
SAMPLING PROCEDURES
25 ml of absorbing solution were pipetted into a sample
flask. The flask valve stopper was inserted into the flask
with the valve in the "closed" position. The sampling train
was assembled as shown in Figure A-2 with all valves closed.
The probe was placed at the sampling point. The probe valve
and the pump-manometer valve were turned to their "open" positions
and the probe purged. The probe valve was then closed and the
flask valve opened to its "evacuate" position.- The flask was
evacuated to at least 3 in. Hg absolute pressure. The manometer
reading was taken by turning the pump-manometer valve to the
"manometer" position. The pump was turned off and the system
was checked for leaks by observing any drop in the mercury level.
. .
al L i 7 tn
The initial flask pressure, volume, temperature, and barometric
pressure were recorded on the data sheet. The probe valve was
slowly turned to the "sample" position until a slight drop in
the manometer mercury level was observed. The sample was allowed
to enter the flask for about 3 to 4 minutes. The probe valve
was then closed when there was approximately a one inch mercury
vacuum left in the flask. The final flask pressure and temperature
were then recorded. The flask valve was closed and the flask
contents were shaken for five minutes.
Sample Recovery
The samples were allowed to remain in the flasks for at
least 24 hours. The sample was then transferred to a 250 ml
beaker using a small amount of water.
Analysis
The sample was evaporated to dryness in an oven and then
cooled. Two ml of phenoldisulfonic acid solution were added
to the dried residue and triturated thoroughly with a glass rod.
One ml of water and 4 drops of concentrated sulfuric acid were
then added. The solution was heated on a steam bath for three
minutes with occasional stirring. After cooling, 20 ml of water
were added and mixed well by stirring. Concentrated ammonium
hydroxide was added dropwise with constant stirring until alkaline
to litmus paper. The solution was transferred to a 100 ml volu-
metric flask and the beaker washed three times with 4 to 5 ml
portions of water. The solution was diluted to the mark and
mixed thoroughly.
at 410 nm using the blank solution as a zero. A half inch absor-
The absorbance of each sample was measured
I t -
bance ce l l w a s used.
CALIBRATION PROCEDURES
Flask Volume - The f l a s k and f l a s k va lve were assembled
and f i l l e d w i t h water t o t h e s topcock. The volume o f water was
measured t o + - 1 m l . The f l a s k s were numbered and t h e volume
recorded on each .
Spectrophotometer - Al iquo t s of 0 .0 t o 1 6 . 0 m l of potassium
n i t r a t e s o l u t i o n ( s t anda rd ) was added t o a series of beake r s ,
and 25 m l of absorb ing s o l u t i o n added t o each. Sodium hydroxide
(1N) was added dropwise u n t i l a l k a l i n e t o l i t m u s paper (about
25 t o 35 d r o p s ) . These s o l u t i o n s were t r a n s f e r r e d t o 1 0 0 m l
volumetric f l a s k s and t h e absorbance r ead a t 4 1 0 nm. The ca l i -
b r a t i o n curve was checked p r io r t o each set of samples.
._
i
DETERMINATION OF SULFUR DIOXIDE EMISSIONS IN STACK GASES This method was used to measure sulfur dioxide in stack
the Federal Register', with gases and follows Method 6 of modifications as noted below. SAMPLING APPARATUS
Nozzle - Stainless Steel leading edge.
316) .with sharp, tapered
Probe - Pyrex glass with a heating system capable of maintaining a minimum gas temperature of 225 F at the exit end during sampling.and prevent condensation form occurring.
Pitot Tube - Type S, attached to probe to monitor stack gas velocity.
Filter Holder - Pyrex glass Impingers - Four as shown in Figure A-3. The first
and third are of the Greenburg-Smith design with standard tip. The second and fourth were modified by replacing the standard tip with a 1/2 - inch ID glass tube extending to within one-half inch of the bottom of the impinger flask.
Metering System - Vacuum gauge, leak-free pump, ther- mometers capable of measuring temperature to within 5OF, dry gas meter with 2% accuracy, and related equipment, to maintain an isokinetic sampling rate and to determine sample volume.
c
1. Federal Register, Vol. 3 6 , No. 247 - December 23, 1971.
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a w
al-
3r a 0
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I
m
I + I-
a
v, Ln 4
w
._
Y
4 l- v,
3 V
E .r
m L c,
m E .r 7
n E m VI
m. 0 v, \
0 In N
m
dc a, L 3 m .r
LL
Barometer - Bourden tube type to measure atmospheric pressure to + 0.1 inches Hg. SAMPLING REAGENTS
-
Filters - Glass fiber, MSA type 1106 BH of a suitable size to fit in the filterholder.
Silica Gel - Indicating type , 6-16 mesh. Water - Deionized, distilled. Isopropanol, 80% - Mix 800 ml. of isopropanol with 200
ml. of deionized, distilled water. Hydrogen Peroxide, 3% - Dilute 100 ml. of 30% hydrogen
peroxide to 1 liter with deionized, distilled water.
ANALYTICAL REAGENTS Water - Deionized, distilled. Isopropanol Thorin Indicator - 1 - (O-arsonophenylazo)-2-naphthol-3,
6-disulfonic acid, disodium salt. Dissolve 0.20 gram in 100 ml . distilled water.
Barium Chloride (0.0200N) - Dissolve 2.4431 grams of barium chloride [BaCl21 in 200 ml. distilled water and dilute to 1 liter with isopropanol. Standardize with sulfuric acid.
Sulfuric Acid Standard (0.02N)- Standardize to + - 0.0002 N against 0.01N NaOH which has previously been standardized against primary standard potassium acid phthalate.
SAMPLING PROCEDURE One sampling point of average velocity was chosen ._
which was more than 2 feet from the inner walls of the stack. The train was assembled as follows: 150 ml. of 80% isopropanol in the first impinger, 100 ml. of 3 %
hydrogen peroxide in both the second and third impingers,
I I 1 .
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a 0 0 c ! ! I 1 e I] e c t I I
I I
1 l
and about 200 grams of weighed silica gel in the fourth impinger. A portion of the reagents were retained for use as a blank. The train was assembled without the probe and was leak checked at the sampling site by plugging the inlet of the first impinger and pulling a 15-inch Hg vacuum. A leakage rate not in excess of 0.02 cfm at a vacuum of 15 inches Hg was recorded in all cases. attached and the probe heating system turned on. The probe heater setting was adjusted during sampling to prevent any visible condensation. Crushed ice was placed around the impingers and more ice was added during the run to keep the temperature of the gases leaving the last impinger to 70'F or less.
The probe was then
For each run, the data were recorded at startup, on completion of the test and at 15 minute intervals. Sampling was begun by positioning the probe at the sample point. at a rate of approximately 0.8 cfm for a 240 minute period.
The pump was then started and sampling proceeded
At the completion of the test, the probe was removed from the stack and the train was pruged for 20 minutes by drawing ambient air through the system.
SAMPLE RECOVERY The solutions from the second and third impingers
were transferred to a Wheaton bottle. These impingers and their connecting glassware were rinsed with deionized distilled water and other washings added to the same container. The isopropanol from the first impinger and filter were discard6d.
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ANALYTICAL PROCEDURES The volume of the sample was recorded. A 10 ml
aliquot of sample was pippetted into a 100 ml flask. 40 ml of isopropanol and 2 to 4 drops of thorin indicator were added. The sample was then titrated with barium chloride to a pink end point. Each titration was repeated with a second aliquot of sample. The blanks were titrated in the same manner as the samples.
Erlenmeyer
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APPENDIX I
TEST LOG
CHRON‘OLOGICAL LIST OF NOTES THROUGHOUT PROJECT (NOT COVERED BY DAILY PERSONNEL AND LOG SHEET)
CHRONOLOGICAL L I S T OF NOTES THROUGHOUT PROJECT (NOT COVERED BY DAILY PERSONNEL AND LOG SHEET)
CHRONOLOGICAL L I S T O F NOTES THROUGHOUT P R O J E C T (NOT COVERED BY DAILY PERSONNEL AND LOG S H E E T )
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APPENDIX J
RELATED REPORTS
(Supplied by EPA)
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RELATED REPORTS
I Because of the process and control equipment problems
that were encountered, two additional test series were
performed at the Woodville Lime and Chemical Company. The
first test series began on May 21, 1974, and is discussed in
EPA Report No. 74-LIM-3A. The last test series performed
started on August 5 , 1974, and is presented in EPA’s Report
No. 75-LSM-8.
