-------
2-1
2.0 SUMMARY OF RESULTS
2.1 COMPOSITION OF OFF GAS STREAMS
The hydrocarbon composition of the three process off gas streams
and the emissions from the limestone pits at Union Carbide's LAB process
were quite similar. The major hydrocarbons were ethyl benzene, n-decane
and n-undecane. There were also substantial amounts of various decane and
undecane isomers as well as n-dodecane. Benzene was barely detectable in
all samples.
The average concentrations of hydrocarbons present in the several
off gas streams are summarized in Table 2.1 along with the percent of the
total hydrocarbon contributed by each component. The saturates are combined
by carbon number to simplify the data analysis. The data given are averages
of the data for four runs which are presented in Table 6.8. The relatively
small differences in run-to-run composition of the hydrocarbon fraction
justify the use of averages as representative of the composition at each
sampling point during the test program.
2.2 BENZENE EMISSIONS AND CONTROL EFFICIENCY
The average benzene concentrations at each sampling point are given
in Table 2.2 along with the equivalent mass of benzene per kg LAB produced.
and the apparent benzene removal efficiency in the pit system. The benzene
concentrations at each point exhibited a significant decrease from Run A
(9/18) to Run D (9/20). The complete results for benzene analysis are
presented in Table 6.9.
-------
2-2
TABLE 2.1
AVERAGE HYDROCARBON COMPOSITION BY CARBON NUMBER
Compound
C^, Butane Isomers
Cg» Ethyl Benzene & Xylenes
Cg, Nonane Isomers
, Decane Isomers
' Undecane Isomers
> Dodecane Isomers
TOTAL
ppra (Corrected for Carbon Number)
Point 1 Point 2 Point 3 Point 4
0
647
132
1083
547
163
2572
774
687
82
557
160
40
2300
439
64
64
787
.262
63
1679
576
1478
105
894
362
70
3492
C,, Butane Isomers
Cg» Ethyl Benzene & Xylenes
Cg, Nonane Isomers
C,Q, Decane Isomers
Cji, Undecane Isomers
Dodecane Isomers
Volume Percent of Hydrocarbon Fraction
0 34 27 14
28 30 4 39
4442
42 25 47 27
20 7 16 15
6 2 4 .5
-------
2-3
Table 2.2
AVERAGE BENZENE CONCENTRATIONS
ppm mg Benzene/kg LAB Benzene Removal Efficiency
Point 1 7.53 3.07
Point 2 5.95 2.56
Point 3 5.88 4.91
Point 4 1.65 0.69
-------
3-1
3.0 PROCESS DESCRIPTION
Union Carbide's Institute, West Virginia plant produces Alkyl 11
and 12 which are linear alkyl benzenes (LAB). The synthesis of LAB is done
in three operations: chlorination, alkylation, and product recovery.
Anhydrous hydrogen chloride gas is produced as a by-product from both the
chlorination and alkylation steps. At the time of Scott's test program, the
hydrogen chloride off gas was disposed of in limestone pits. Figure 3.1 il-
lustrates the system schematic and the materials flow through these operations.
3.1 CHLORINATION
The first step in Union Carbide's synthesis of LAB is the chlori-
nation of an n-paraffin feed stock which consists primarily of C-.Q-C..,
normal alkanes. The feed stock is brought into contact with a metered
stream of anhydrous chlorine gas which results in the following reaction:
n-RH + C12 n-RCl + HC1
The paraffin feedstock is supplied in excess and therefore the
chlorine conversion is essentially 100%. Hydrogen chloride gas is formed
as a reaction by-product in equimolar amounts to the chlorine feed.
The chlorinated reaction products along with unreacted hydro-
carbons makes up the product' stream of the chlorinator. The HC1 gas
produced from the chlorination reaction is removed from the reactor.
3.2 ALKYLATION
The chlorinated paraffin stream from the chlorinator is mixed
with benzene in the presence of an aluminum chloride catalyst. The resulting
Friedel-Crafts reaction produces a mixture of alkylated benzene products
which are discharged to a product recovery system. The primary reaction
occurring is:
A1C13
n-RCl + «$H n-R«5 + HC1
-------
3-2
Chlorine
Gas
Paraffin
Liquid
Paraffin
Chlorination
System
->
HC1 Gas
,
Chloroparaffin
J;C1
s
Limestone
Water
HC1 Gas
Limestone
for
Compressor
Water
Crude
Chloroparaffin
Liquid
Paraffin - Secycle
A1C13
Slurry
Benzene
LiquidA
Reactor
System
Benzene - Recycle
-,^,^
Crude Product
>
Water
CO 0)
XXI
rH J3
03 o
U OT
4) 4)
e e.
0) C.
N ft
QJ ij
P3 CO
m C.
u-i c.
V- W
eg u
PL, w
Water
Catalyst
4r
Product
FIGURE 3.1 BLOCK FLOW DIAGRAM, LAB PROCESS SHOWING
LIQUID AND GAS SAMPLING POINTS.
-------
3-3
The HC1 liberated by the reaction along with low molecular weight
reaction products is vented to a compressor and is then combined with the
HC1 stream from the chlorinator.
3.3 PRODUCT RECOVERY
The discharge from the alkylator contains alkyl benzene, unreacted
n-paraffins, benzene, and aluminum chlorine catalyst. This is contacted with
water to deactivate and remove the catalyst and scrub any dissolved HC1. The
unreacted benzene is stripped and combined with the benzene feed stream. The
unreacted n-paraffins are stripped and returned to the paraffin feed. Crude
product LAB remains.
3.4 LIMESTONE PITS
Limestone pits are used by Union Carbide to control the acidic
emissions of several processes. The LAB HC1 emissions wera controlled this
way at the time of this program. One pit was reserved exclusively for the
emissions of the LAB process during this test program. The acidity built
up high enough to require part of the stream to be sent to a second pit
during test D.
The limestone pits consist of four underground concrete tanks
with open tops at ground level in which an excess of crushed limestone rock
is maintained washed by a constant stream of water. The pits are approxi-
mately 18 feet deep. The .reaction in the case of HC1 emissions is: 2HC1 +
CaCO, CaCl2 + H20 + CO;-. Fresh water and waste gas are admitted at the
bottom of the tanks. The primary products are CO- which is allowed to vent
drectly to atmosphere and waste water containing CaCl^ which is run from
the surface of the tanks to the sewer.
3.5 PROCESS FLOW AND SCHEDULE
The LAB unit operating schedule is continuous once the process is
started. It requires two to three days to bring it up to equilibrium from
a cold start. Maintenance shut downs are scheduled long in advance approxi-
mately once per year.
The process flow is based on the chlorine feed rate which is
metered.
-------
4-1
4.0 SAMPLING AND ANALYSIS
The sampling and analysis program involved the collection of
simultaneous one-hour integrated bag samples at four locations on the HC1
venting system. Four sets of samples were collected and analyzed for total
hydrocarbons, benzene, and other dominant organic species immediately
following each sample run. The analyses were conducted by FID and gas
chromatograph in Scott's mobile laboratory parked at the plant. Analyses
were also conducted for HC1 or CO on the integrated samples, for pH,
organic content and dissolved solids on the limestone pit effluent, and
for dissolved HC1 on the chlorinated paraffin feed and the crude product.
4.1 LOCATION OF SAMPLING POINTS
The four locations sampled by integrated bags and the three liquid
sampling points are illustrated on Figure 3.1. The gas sampling points
were the off gas from the chlorinator, the off gas from the alkylator, the
combined off gas streams, and the off gas from the pit.
Sample Point 1 - Chlorinator
HC1 produced in equimolar amounts to the chlorine feed was vented
to the limestone pits. This vent line was under a pressure of from 17 to
18 psi and was approximately 100°F. It was sampled from a 1/2" valve
located 15 feet above grade.
Sample Point 2 - Alkylator
The vent from the alkylator contained HC1 in equimolar amounts
to the chlorine feed. This stream passed, through a compressor before venting
to the pits. It was sampled on the high pressure side of the compressor
from a 1/2" valve located on the first platform of the LAB unit. The pressure
ranged from 20 to 22 PSI and the temperature was between 80 and 95°F.
Sample Point 3 - Combined Streams
The HC1 off gas streams from both the chlorinator and the alkylator
were combined before being run to the pits. This combined stream was sampled
at a point near grade level from a 1/2" valve. The pressure at this point
was around 14 PSI and the temperature was approximately 100°F.
-------
4-2
Sample Point 4 - Pit Emissions
One of the four limestone pits was selected for sampling during
the program. This pit was isolated from other plant waste streams, and most
of the emissions from the LAB unit were run into it. Gaseous emissions were
collected from the pit by covering most of the open grating with polyethylene
sheeting and positioning a sample line directly above the surface of the
liquid.
Samples of the pit liquid effluent were collected from an overflow
well immediately adjacent to the pit. A plunge bottle sample was collected
every 15 minutes during each sample run. These were combined and submitted to
the Union Carbide laboratory for pH analysis and then resealed and returned
to Scott's Plumsteadville laboratory for organic and total solids analyses.
Process Samples
Samples were taken by Union Carbide technicians of the chlorinated
paraffin feed and the crude product at the mid point of each sampling run.
These were analyzed by Union Carbide's lab for dissolved HC1.
4.2 SAMPLE COLLECTION
Integrated Bags
The integrated bag sampling technique was based on EFA Method 110,
"Determination of Benzene from Stationary Sources". It involved air-tight
20 gallon steel wide mouth drums into which 100 liter Tedlar bags were placed.
For the HC1 samples, the process stream pressures were sufficient to supply
a steady flow of sample into the Tedlar bags. The drum used for sampling
the pit emissions was partially evacuated prior to sampling.
Each drum was fitted with a shut off valve, a vacuum gauge, and
an inert flow meter calibrated for HC1. This was connected to the sample
point with a short length of Teflon tubing. Mounted on the process sampling
points were stainless shut off valves, inert diaphram pressure gauges and
stainless dial thermometers. The drums were marked so that each could be
dedicated to a single sample point.
-------
4-3
Sample collection was accomplished by first purging the Tedlar
bags with nitrogen and checking by FID for contamination. The clean bags
were sealed in the drums and subjected to vacuum of 15 PSI to check for
leaks. The sampling units to be used on the HC1 streams were then back
filled with metered amounts of nitrogen to provide known dilutions in the
resulting samples. The exact dilution ratios were measured after sampling
by injecting 20 cc from each bag into water and titrating with standard
0.1N NaOH. The drum for the sampler designated for the pit sample was
partially evacuated to approximately 16 psi vacuum. Infiltration into
the sampled area of the pit by ambient air was measured in each sample by
analyzing for CC^ and 62 by Orsat.
Each sample was connected to its respective sample point by a
short length of Teflon tubing. Technicians were assigned to each location
so that all sampling could be started and stopped at the same times.
During the runs, the sample pressures and temperatures were recorded at
regular intervals, and the sampling rates were adjusted to maintain con-
stant rates. At the conclusion of each sampling run, the samplers were
returned to Scott's mobile laboratory and the Tedlar bags removed for
analysis.
Pit Overflow Water
Over-flow water was sampled with a Bacon bomb. This device con-
sists of a stainless chamber with a scalable closure at the bottom. It can
be lowered into a liquid and filled below the surface. For this project,
samples were taken approximately one foot below the surface. Four samples
were taken during each run. They were combined and sealed in Teflon lined
glass jars. Union Carbide laboratories performed pH analyses on each sample.
"They were then returned to Scott's Plumsteadville lab for organic and
dissolved solids analyses.
-------
4-4
4.3 SAMPLE ANALYSIS
Total Hydrocarbon Analysis
The integrated sample bags were analyzed on a Beckman Model 108
total hydrocarbon analyzer. This was calibrated with a standard mixture of
1.02% propane in air. Hydrocarbon-free air was used to zero the instrument.
Analyses were performed before each sampling run to determine the background
contamination level of each integrated bag sampling unit and after each
sampling run to determine the total hydrocarbon content of each sample.
Gas Chromatography
The Tedlar bag samples were analyzed for individual hydrocarbons
and benzene using a Shimadzu - GC - Mini 1 Gas Chromatograph equipped with
dual flame ionization detectors. Samples for injection into the chromato-
graph were extracted from the Tedlar bags through a rubber septum into a
100 cc gas sampling syringe.
The chromatograph was equipped with dual heated gas sampling loops.
Each of these was connected to a column inside the oven. The columns were
connected to separate FIDs and read out on recorders. For each analysis,
the oven was programmed from 208C to 160°C at a rate of 4°C/minute for ten
minutes. Then the programming rate was increased to 10°C/minute. Upon
reaching 160°C, it was held isothermally until no more peaks eluted.
The columns were:
A. 0.3m x 3.2mm stainless steel packed with 20% SP 2100/0.5%
Carbowax 1500 on 100/120 mesh Supelcoport (D-4536)
B. 1.83m x 3.2mm stainless steel packed with 5% SP 1200/1.75%
Bentone 34 on 100/120 mesh Supelcoport.
A Chromatopac E1A Shimadzu Data Processor was used to measure peak areas on
Column A.
For the samples containing HC1 gas, a pre-injection neutralization
device was connected to the sampling loops on the GC. This was constructed
following information supplied by Dr. J. E. Knoll, EPA - SS/QAB/EMSL/RTP
-------
4-5
(Memo of August 16, 1978). It consisted of a 4" x 1/4" stainless container
filled with a one to one mixture of acid washed celite and s.oda lime heated
to 225°C. This temperature was arrived at experimentally as the temperature
at which no benzene adsorption was apparent using standard benzene samples.
The mixture was changed after every five injections. All field calibrations
of the chromatograph were passed through the neutralization device.
The total analysis time for each sample was approximately twenty
minutes. The calibration gases were 1.02% propane in nitrogen and 150 ppm
benzene in air.
To determine the relative response and linearity of this instrument
for benzene and propane, a series of laboratory calibrations were run before
the field program. The first calibration runs were made to establish fuel
and air ratios which would give comparable response factors for benzene and
propane. These settings were found to be: air at 240 cc/min, fuel at
40 cc/min, and carrier at 40 cc/min. Other calibration runs were made to
prove the linearity of the instrument for both propane and benzene. Benzene
was checked at 49.3 ppm and 3003 ppm. Propane was checked at 82 ppm, 330 ppm,
1.02% and 10%. On the basis of these studies, the 1.02% propane standard was
utilized in the field in conjunction with the 150 ppm benzene standard.
The accuracy of the gas chromatographic techniques used in this
program was tested by EPA through the use of Audit Samples. Three unknowns
were presented to Scott's chemist for analysis in the field laboratory.
These were analyzed by first transferring each to a Tedlar bag. A sample
of each was extracted from the bag and injected into the chromatograph.
Each Audit Sample was analyzed three times. Scott's analyses averaged 4.5%
higher than the stated concentrations. The results of the audit survey are
included as Appendix 2.
HC1 Emissions
The flow rate of HC1 was determined from Union Carbide's records
for chlorine consumption during the test period. Two additional factors
were also taken into account. The dilution ratio of sample to pre-filled
-------
4-6
nitrogen was determined by titrating gas samples out of each integrated bag.
The HC1 lost through dissolution in the product streams was -analyzed by
Union Carbide laboratories.
The dilution ratio was determined by extracting a 20 cc gas sample
from each integrated sample which contained HC1. This was slowly injected
into 50 cc of distilled water. It was then titrated with standard 0.1N
NaOH against phenolphthalein indicator. This procedure was done twice and
the results averaged to yield the dilution ratio of HC1 to nitrogen.
The HC1 lost through dissolution in the product streams was
determined from process samples taken at approximately the mid-point of each
run by Union Carbide technicians from the product stream of both the chlori-
nator and the alkylator. These were transmitted to Union Carbide's laboratory
for analysis of dissolved HC1.
cp_2_
The pit samples were drawn from the head space over the limestone/
water mixture in the pit. The density of CO? in comparison with air caused
the pit emissions to accumulate in this area. Air infiltration was possible,
so each integrated sample was analyzed for C02 and 02 contents by Orsat. The
percentage of noii-CO- gas in each sample was interpreted as the degree of
dilution of the sample.
Temperature and Pressure
Temperature and pressure at each sampling point on the HC1 vent
streams were recorded at regular intervals during each sampling run. The
pressures were measured with 0-30 PSI oil filled bourdon gauges isolated by
Teflon diaphragms. Temperatures were taken with dial thermometers at points
2 and 3 and with a chrome-alumel thermocouple at point 1. In each case, the
temperature measurement was taken on the withdrawn sample rather than on the
flowing stream. This was felt to be fairly accurate despite the low sampling
rate because of the closeness of the stream temperature to ambient and to
the temperature conduction of the sampling manifolds. The latter were
insulated with asbestos tape prior to sampling.
-------
4-7
Pit Water Samples
The combined water samples collected from the pit overflow well
were returned to Scott's Plumsteadville laboratory for analysis of total
solids and benzene. Total solids were determined by evaporating a known
volume to dryness and weighing the residue.
The organic components of the pit water samples were determined
by gas chromatography. The volume of each sample was measured and then
extracted with 50 ml methylene chloride. The polyethylene sample container
was also extracted with the same methylene chloride to remove any absorbed
organics. A 1 ul aliquot of each extract was analyzed by gas chromatography
using the SP-2100 column under the same temperature program as in the field
program. A 0.478 ug/tnl standard of benzene in methylene chloride was used
to calibrate the results.
-------
5-1
5.0 GAS CHROMATOGRAPHY
The gas chromatographic analysis of a process stream such as Union
Carbide's LAB process which has not previously been the subject of detailed
analysis presents the possibility that peaks for benzene or other components
of interest will be obscured by peaks due to unknown components. This
problem is difficult to overcome when the analyses are being performed in
a mobile laboratory at a remote field site. In this test program two pre-
cautions were taken to minimize this problem. First, preliminary samples
of the process streams were analyzed at Scott's Plumsteadville laboratory
prior to the field phase of the program. Second, the gas chromatograph
used in the field was equipped with two columns having different retention
characteristics. During the field test program, each sample was analyzed
simultaneously using two columns each connected to separate flame ionization
defectors, electrometers and strip chart recorders.
The two gas chromatography columns described in Section 4.3 were
selected on the basis of the expected sample composition. The SP-2100 column
has been used by Scott for the separation of benzene from other hydrocarbons
in numerous previous programs, and extensive retention time documentation
had been developed for this column. The Bentone column is specified in EPA
Method 110 for Determination of Benzene from Stationary Sources.- It is used
where the separation of xylene isomers is also desired. The characteristics
of this column in comparison to the SP-2100 is to delay the elution of aro-
matics with respect to the aliphatic compounds.
Analysis of the off gas samples collected several weeks before the
field test program determined that benzene concentrations were around 25 ppm
after correcting for dilution. These analyses were considered to be approxi-
mations, however, due to the corrosive nature of the HC1 balance gas in each
sample. The predicted concentrations for benzene of 1 to 3% were definitely
not indicated by the preliminary sample analysis. Plant personnel also
predicted low benzene readings, but they acknowledged wide swings in process
conditions which were not readily controllable. Thus, in setting up for
-------
5-2
this field program it was decided to prepare for a benzene concentration
from 100 to 1000 ppm. Higher concentrations could be readily analyzed by
additional dilution of the samples.
The actual field analyses showed much lower benzene concentrations
than expected. The highest concentration was approximately 15 ppm and some
samples contained less than 1 ppm. The analyzed concentrations in the dilu-
tion sampling systems were 20% of these values. The effect of these low
concentrations on the field analytical system was to severly reduce the
precision of the results for benzene. Higher precision could have been
obtained only by doing a separate benzene analysis on each run under
different chromatographic conditions which would not have produced infor-
mation on the other components in the samples. Neither the time nor the
equipment was available for this during the field program.
Table 5.1 shows the benzene concentrations for each run from
both the SP-2100 and the Bentone columns. These figures are in ppm benzene
and were calculated directly from peak height on the recorder charts. The
variations in concentration can be due to the inaccuracy inherent in the
estimation of peak heights that are only 1 to 2% of full scale or to the
effect of unrecognized trace compounds eluting with benzene. Nevertheless,
Table 5.1 does verify that minimal benzene concentrations were present on
the LAB process at the time of these tests.
Figures 5.1 through 5.8 are reproductions of the actual chromato-
graphs obtained on the two columns utilized on this program. Unlike the
chromatograms used in the analysis, these have been run without attenuation
by estimating at the beginning the greatest peak height. For this reason,
benzene does not always appear as a peak. Its position; however, is indicated
on each figure.
-------
TABLE 5.1
COMPARISON OF BENZENE ANALYSES MADE ON SP-2100 AND BENTONE GC COLUMNS
ppm C
Run
Sample Point
SP-2100
Bentone
A
1
14.1
12.0
2
13.2
3
11.6
8.2
4
5.4
2.2
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1
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3.4
2
8.5
1.1
3
7.3
4.5
4
0.5
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2
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0.6
3
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4
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1
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-------
5-6
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-------
5-7
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0)
|
!
1
1
' 1 1 .
i : ! !
i ' '
! ! .
'
1 ~
' =
I
1 : 1 i
1 i
I . . i
1 . ,
!
g- .
i . .
- .
; . .
H.
<-J
1
i
! ' : ,
; ;
i
i
i ;
b /'
, i '
i
; !
1 :
' '
' (
03 .
1 -
..
^
i
i
«X
r'
I
I
t
.
;
1
f
i
i '
i
1
^_
o^>
,
4-' M i CJ A 'Jl
1
1 .
? ' P
-
i \
|
CD
,
! -
, '
' '
CD
!
«
C) \ *J ) CD
i
)
!0
FIGURE 5.4
SAMPLE 4B, BENTONE COLUMN 128X (? 102 ATTENUATION
-------
5-8
FIGURE 5.5
SAMPLE IB. SP-2100 COLUMN
2X (3 IQ2 ATTENUATION
-------
5-9
SAMPLE 2B, SP-2100 COLUMN
4X @ 1CH ATTENUATION
-------
5-10
FIGURE 5.7
SAMPLE 3B, SP-2100 COLUMN
2 AT
2X @ 1CK ATTENUATION
-------
5-11
FIGURE 5.8
SAMPLE 4B, SP-2100 COLUMN
32X @ 102 ATTENUATION
-------
6-1
6.0 DATA SUMMATION
Four runs were made each consisting of simultaneous samples at
four test points on the LAB process. The test points have been designated
Numbers 1 through 5 as shown on Figure 3.1. The runs have been designated
Letters A through D. Thus each analytical datum is referenced by a number
and a letter. For example 1A refers to the sample taken at the chlorinator
'off gas line on September 18, 1978.
The date and times of each run were as follows:
A September 18, 1978 1515-1615
B September 19, 1978 1005-1105
C September 20, 1978 0730-0830
D September 20, 1978 1120-1220
The sample locations were:
1 Chlorinator off gas
2 Alkylator off gas
3 Combined off gas
4 Pit emissions
5 Pit effluent
6.»1 FIELD TEST DATA
Table 6.1 lists the data collected in conjunction with each
integrated sample. Sample point temperature and pressures were averaged
from readings taken during each run. The percentages of HC1, CO- and 0-
were determined from titrations and the Orsat readings respectively. The
hydrocarbon measurements were made on the FID analyzer.
The percent dilutions of each HC1 sample were calculated from the
volume of 0.01N NaOH required to neutralize 20 cc of sample. Assuming each
mole of HC1 gas occupies 24 liters at ambient conditions, the following
equation was used to calculate the percentage of HC1 in each sample.
-------
6-2
TABLE 6.1
FIELD SAMPLING DATA
Total
Run Location
A
B
C
D
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
Temperature
°C
38
27
34
(27)*
36
29
27
(31)
26
27
24
(24)
38
31
30
(32)
Pressure
psig
17.6
22.0
14.9
(29.61)
18.2
21.2
13.9
(29.72)
17.5
20.9
13.7
(29.65)
18.4
21.6
14.2
(29.62)
HC1 C02 02 Solids Hydrocarbons
% % % pH ' % % by Volume((
15,60
14.16
16.68
92 2
1.2 8.947
22.26
18.66
21.84
86 3
1.6 5.771
27.36
26.67
28.29
93 2
1.2 8.326
21.16
19.74
22.83
97 1
5.2 8.106
0.23
0.08
0.10
0.44
0.15
0.13
0.12
1.15
0.11
0.17
0.12
1.11
0.25
0.13
0.14
0.86
*Temperatures and pressures in parentheses are ambient conditions in °C
and inches mercury respectively.
-------
6-3
Normality NaOH x Volume NaOH x 24 x 100 = %
Volume HC1
for 20 cc gas samples and 0.01N NaOH:
1.2 Volume NaOH = %
6.2 PROCESS DATA
Union Carbide supplied average LAB production data for the three
day period of this program. These data consisted of average, minimum and
maximum chlorine feeds and the instrument error associated with them and
the average, minimum and maximum LAB production rates and their accuracy.
In addition, Union Carbide took samples of the chlorinated paraffin steam
and the crude product, analyzed them for dissolved HC1 and calculated the
HC1 flow at each sample point.
Table 6.2 shows the theoretical average, minimum and maximum HC1
flows at each sample point based on Union Carbide's data. Table 6.3 shows
the actual HC1 flows calculated by Union Carbide for each sample point.
The percentages of variance in Table 6.3 are based on the difference at
Points 1 and 2 with half of Point 3. Since Point 3 totals all lie within
the range of theoretical HC1 flows, the variance equals the degree of HC1
dissolution and degassing as described in Union Carbide's letter in Appendix A.
6.3 COMPOSITION OF HYDROCARBONS IN HC1 VENT SYSTEM
The composition of hydrocarbons in each of the integrated gas
samples was determined by gas chromatography. The results of these analyses
are shown on Tables 6.4 through 6.7. The concentrations shown are ppm as
propane and have been adjusted for the dilution in the sample container.
Table 6.8 shows the volume percentages of each carbon number group of compounds.
-------
6-4
TABLE 6.2
UNION CARBIDE PRODUCTION DATA
September 18 through 21, 1978
Kg HCl/Kg Crude LAB
Maximum
Average
Minimum
Points 1 &
0.2084
0.1992
0.1908
TABLE 6.
HYDROGEN CHLORIDE
2 Point 3
0.4169
0.3984
0.3817
3
FLOW RATES
Kg HCl/Kg Crude LAB
Run
A
B
C
D
Point 1
0.1908
0.1916
0.1833
0.1826
Point 2
0.2019
0.2002
0.2062
0.1996
Point 3 Variance (%)
0.3927 2.8
0.3918 2.2
0.3895 5.9
0.3822 4.4
-------
6-5
TABLE 6.4
COMPOSITION OF HYDROCARBON VAPOR AT THE CHLORINATOR VENT LINE
Sample Point #1
ppm Cg
Compound Run A Run B Run C Run D
Isobutane
N-Butane
Unknown 184
Benzene 28 30 1 2
Cg Saturate 110
Cg Saturate 214
Cg Saturate
Cg Saturate 301 50 77 105
Cg Saturate 201 101 54 136
Ethyl Benzene* 1760 1262 1026 2560
0-Xylene 271 18 60
N-Nonane 193 34
C10 Saturate 580 173 141 209
C10 Saturate 234 195
C10 Saturate 594 277 205 438
C10 Saturate 865 497 239 628
N-Decane 4045 1694 921 2504
C^ Saturate
GH Saturate
N-Undecane
Cj_2 Saturate
Unknown
N-Dodecane
Total
Total
(From THC Analyzer)
^Includes trace amounts of M- and P-Xylene
1018
1621
830
251
13116
14700
379
1013
128
136
6171
6700
176
331
188
32
3391
4000
603
2882
169
872
11168
11800
-------
6-6
TABLE 6.5
COMPOSITION OF HYDROCARBON VAPOR AT THE ALKYLATOR VENT LINE
Sample Point #2
ppm C<]
Compound
Isobutane
N-Butane
Unknown
Benzene
Cg Saturate
Cg Saturate
Cg Saturate
Cg Saturate
Cg Saturate
Ethyl Benzene*
0-Xylene
N-Nonane
C^g Saturate
CIQ Saturate
C-J_Q Saturate
Cin Saturate
Run A
1130
15
(26)
705
86
44
283
71
341
387
Run B
1011
45
17
159
158
1981
92
194
270
Run C
1033
3
22
4-3
143
160
2573
49
139
244
209
Run D
895
1
125
122
1931
110
284
345
N-Decane 1327 1153 840 1146
C-i, Saturate
Cu Saturate 198 195 59 268
N-Undecane 575 341 193 511
C12 Saturate 74 84 290
Unknown
N-Dodecane 88 69 25 88
Total 5276 5759 5819 6116
Total 5700 7000 6400 6600
(From THC Analyzer)
Benzene concentration in paranthesis from Bentone column analysis
*Includes trace amounts of M- and P-Xylene
-------
6-7
23
N-Decane 2337
C]j_ Saturate
C-Q Saturate 184
N-Undecane 898
C12 Saturate 137
Unknown
N-Dodecane 116
Total 4384
Total 6000
(From THC Analyzer)
14
1941
283
641
220
55
4830
5500
TABLE 6.6
COMPOSITION OF HYDROCARBON VAPOR AT THE COMBINED VENT LINES
Sample Point #3
ppm G.J
Compound
Isobutane
N-Butane
Unknown
Benzene
Cg Saturate
Cg Saturate
Cg Saturate
Cg Saturate
Cg Saturate
Ethyl Benzene*
0-Xylene
N-Nonane
C^Q Saturate
C]_g Saturate
CIQ Saturate
C^g Saturate
172
33
266
17
36
36
151
370
6
195
97
55
208
149
399
57
116
76
98
164
312
54
166
181
104
147
248
530
1294
209
466
169
36
3588
4200
1923
310
851
187
88
5373
6100
*Includes trace amounts of M- and P-Xylene
-------
6-8
TABLE 6.7
COMPOSITION OF HYDROCARBON VAPOR IN THE VENT FROM THE LIMESTONE PIT
Sample Point #4
ppm Co
Compound
Isobutane
N-Butane
Unknown
Benzene
CQ Saturate
CQ Saturate
CQ Saturate
Co Saturate
CQ Saturate
Ethyl Benzene*
0-Xylene
N-Nonane
CJLO Saturate
C^Q Saturate
C1Q Saturate
C]_Q Saturate
N-Decane
C11 Saturate
^11 Saturate
N-Undecane
C^ Saturate
Unknown
N-Dodecane
Total
Total
Run A
37
11
9
766
76
19
173
233
951
18
249
1353
95
543
4533
4800
Run A
37
11
Run B
1493
24
1
42
Run C
913
17
1
43
Run D
585
(D
47
60
21
9
766
76
19
173
233
951
18
249
1353
95
543
4533
4800
345
5613
164
71
448
698
812
2452
20
216
1006
36
69
13557
13400
388
5823
155
65
398
572
655
1892
143
598
17
31
11871
11900
147
3045
125
219
353
454
1609
27
351
1434
65
265
8700
8900
(From THC Analyzer)
Benzene concentration in paranthesis from Bentone column analysis
*Includes trace amounts of M- and P-Xylene
-------
TABLE 6.8
COMPOSITION OF HYDROCARBON VAPORS IN LAB SYSTEM BY CARBON NUMBER
ppm (Corrected for Carbon Number)
Compound
C. , Butane Isomers
CQ, Ethyl Benzene
and Xylene
Cg, Nonane Isomers
CJQ, Decane Isomers
^11 » Undecane Isomers
Cj^» Dodecane Isomers
TOTAL
C^, Butane Isomers
Cg, Ethyl Benzene
and Xylene
Cg, Nonane Isomers
CJQ, Decane Isomers
C-.,, Undecane Isomers
C, «, Dodecane Isomers
A
0
762
340
1895
720
270
3987
0
19
8
47
18
7
Point 1
B C
0 0
480 385
62 44
851 452
380 138
66 55
1839 1074
Volume
0 0
26 36
3 4
46 42
21 13
4 5
D
0
960
80
1134
950
260
3384
Point 2
A
859
297
15
723
211
22
2127
Percent of
0
29
2
33
28
8
40
14
1
34
10
1
B C
792 775
743 983
106 123
507 430
146 69
36 27
2330 2407
Hydrocarbon
34 32
32 41
5 5
22 18
6 3
2 1
D
671
724
82
566
212
73
2328
Point 3
A B
456 425
106 36
80 85
868 809
295 252
63 69
1868 1676
Fraction
29
31
4
24
9
3
24 25
6 2
4 5
46 48
16 15
3 4
C
439
44
19
583
184
51
1320
33
3
1
44
14
4
D
435
68
73
886
317
69
1848
Point 4
A B
28 1138
316 2166
9 168
407 1323
442 339
160 26
1362 5160
24
4
4
48
17
4
2 22
23 42
1 3
30 26
32 . 7
12 1
C D
697 439
2242 1189
185 56
1055 791
202 494
12 83
4393 3052
16 14
51 39
4 1
24 26
5 16
0 3
0\
I
-------
6-10
6.4 CALCULATED BENZENE DATA
Table 6.9 shows the concentrations of benzene at each sample point
compared to the process data for this production of LAB. In addition, the
percent efficiencies of the pits as a benzene control device are shown. The
calculations are shown in Section 7.0.
6.5 ORGANIC CONTENT OF PIT WATER SAMPLES
The pit samples were extracted with some methylene chloride
and analyzed for organic content by gas chromatography. A standard of
0.478 vg/yl was used for comparison. Table 6.10 shows the results of the
analysis.
-------
6-11
TABLE 6.9
CALCULATED BENZENE DATA
Sample Point Benzene Benzene Benzene
gm HC1 CM HCL
mg
Efficiency
Number
1A
2A
3A
4A
IB
2B
3B
4B
1C
2C
3C
4C
ID
2D
3D
4D
ppm
14.1
13.2
11.6
5.4
14.8
8.5
7.3
0.5
0.4
1.5
2.5
0.4
0.8
0.6
2.1
0.3
mg/CM HC1 mg/CM CO,,
45.0
42.1
37.0
8.6 17.2
47.2
27.1
23.3
0.8 1.6
1.28
4.79
7.98
0.64 1.28
2.55
1.91
6.70
0.48 0.96
Kg LAB
190.8
201.9
392.7
191.6
200.2
391.8
183.3
206.2
389.5
182.6
199.6
382.2
Kg LAB
0.128
0.135
0.263
0.128
0.134
0.262
0.123
0.138
0.261
0.122
0.134
0.256
Kg LAB
5.76
5.68
9.73
2.26
6.04
3.63
6.10
0.21
0.16
0.66
2.08
0.17
0.31
0.26
1.72
0.12
%
77
97
92
93
-------
6-12
TABLE 6.10
ORGANIC CONTENT OF PIT OVERFLOW WATER
Ug/ral
Run
A
B
C
D
Benzene
<0.05
<0.05
<0.05
<0.05
Ethyl
0,
0.
0.
0.
Benzene
19
37
32
11
Dec an e
1.
6.
3.
3.
43
28
63
11
Undecane
4
16
9
7
.62
.51
.09
.45
Dodecane
3.
13.
6.
6.
51
21
25
12
-------
7-1
7.0 SAMPLE CALCULATIONS
Run A has been used as an example.
7.1 CONCENTRATION OF BENZENE IN THE PROCESS OFF GAS STREAMS.
1. Analysis results: Point 1 = 14.1 ppm benzene
Point 2 » 13.2 ppm benzene
Point 3 = 11.6 ppm benzene
2. Conversion to mg benzene () /cubic meter (CM) HC1.
molecular weight, gm mole . _ _
PPm - 24745 - = mg/CM @ 25°C, 1 atm.
Pt. 1, 14.1 24^45 45.0 mg /CM HC1
Pt. 2,13.2 2^845 = 42.1 mg $/CM HC1
Pt. 3, 11.6 24-^4-5 " 37.0 mg z/ j
oni q
Pt. 2 ," 1 x 0.0224 x ^22. = Q.135 CM HCl/kg LAB
_3b. 5 // J
jqo 7 298
Pt. 3 x o-°224 x = °-263 ^ HC1/k§ LAB
-------
7-;
4. 'Conversion of tng <{)/CM HC1 to rag /kg LAB
mg (j>/CM HC1 x CM HCl/kg LAB = mg /kg LAB
Pt. 1 45.0 x 0.128 5.76 mg /kg LAB
Pt. 3 37.0 x 0.263 = 9.73 mg <|>/kg LAB
7.2 BENZENE EMISSIONS TO THE ATMOSPHERE FROM THE PITS
1. Analysis results: Point 4 = 5.4 ppm benzene
2. Conversion to mg /CM C02 = 8.6 mg (j>/CM HC1
3. Average HC1 flow to pits (Table 6.3)
Plant Data: Point 3 = 392.7 gm HCl/kg LAB
392.7 gm HCl/kg LAB - 0.263 CM HCl/kg LAB
4. Benzene released from the pits
mg /CM HC1 x CM HCl/kg LAB = mg /kg LAB
8.-6 x 0.263 = 2.26 mg */kg LAB
-------
APPENDIX A
UNION CARBIDE LETTER OF OCTOBER 5, 1978
HC1 FLOW RATES
-------
UNION CARBIDE CORPORATION
CHEMICALS AND PLASTICS
P. O. BOX 2831, CHARLESTON, W. VA. 25330
INSTITUTE PLANT October 5, 1978
United States Environmental Protection Agency
Office of Air Quality Planning and Standards
Research Triangle Park, North Carolina 27771
Attention: Mr. Winton E. Kelly
Dear Mr. Kelly:
Attached is the data from the testing of the linear Alkylbenzene facility
at Institute, West Virginia. The data does not conform to the pattern which
I would have expected. I have run other analyses on a different part of the
system and that data confirms the original analysis which were completed while
you were here.
The data is in pounds hydrogen chloride per pound of product which flowed
past the sample points P-l and P-2. Of course, the flow rate at P-3 would be
the sum of the two points. As you can see all of the dissolved hydrogen chloride
is absorbed in the chlorination system and, in fact, degassed somewhat in the
alkylation system. The differences in liquid flow rate were taken into account.
If you or Scott Environmental have any questions concerning the data,
please contact me.
Very truly yours,
Ronald A. Tenney
RAT/cam
Attachment
-------
ATTACHMENT 1
Hydrogen Chloride Rate Past P-l Sample Point
Sample Date Rate
EPA-1 9-18-78 0.1908 pounds HCl/pound AB
EPA-2 9-19-78 0.1916 pounds HCl/pound AB
EPA-3 9-20-78 0.1833 pounds HCl/pound AB
EPA-4 9-20-78 0.1826 pounds HCl/pound AB
Hydrogen Chloride Rate Past P-2 Sample Point
Sample Date Rate
EPA-1 9-18-78 0.2019 pounds HCl/pound AB
EPA-2 9-19-78 0.2002 pounds HCl/pound AB
EPA-3 9-20-78 0.2062 pounds HCl/pound AB
EPA-4 9-20-78 0.1996 pounds HCl/pound AB
pH Water Sample From Pit
Sample Date pH
EPA-1 9-18-78 1.2
EPA-2 9-19-78 1.6
EPA-3 9-20-78 1.2
EPA-4 9-20-78 5.2
-------
APPENDIX B
EPA AUDIT SAMPLE REPORT
-------
4
FIELD AUDIT REPORT
PART A - To be filled out by organization supply unit cylinders (RTI)
1. Organization supplying" audit sample(s) and shipping address
Research Triangle Institute, P. 0. Box 12194
Research Triangle Park, North Carolina 27709
2. Audit supervisor, organization, and phone number (EMB Technical
)
"Vtinton E. Kelley I Jj
Manager) I ^
JM/I
3. Shipping instructions - Name, Address, Attention _
_ Viinton E. Kellev _
_ Environmental Protection Agency. MD-13 _
_ Research Triangle Park, NC 27711 _
4. Guaranteed arrival date for cylinders Ready for pickup on 9/1/78
5. Planned shipping date for cylinders To be picked up by WEE. before 9/11/78
6. Details on audit cylinders for last analysis
Low Cone. High Cone.
a. Date of last analysis 9/1/78 9/1/78 9/1/78
b. Cylinder number B-1117 B~742 BAL 111
c. Cylinder pressure, PSI 2200 1750 725
Benzene in Benzene in Benzene in
d. Audit gas(es)/balance gas Nitrogen Nitrogen Nitrogen
e. Audit gas(es) ppm 98 294 331
f. Cylinder construction Steel Steel ..Aluminum
-------
5
PART B - To be filled out by audit supervisor
1. Organic chemical manufacturing process
2. Location of audit 2^/i/gw Cash'c/e. (!?rp, J^sVrf UJ, \jf^_
3. Name of individual audit and organization
£6.
4. Audit results
e. RTI concentration,' ppm
(Part A, 6d)
(I) (IT)
Low Cone. High Cone.
Cylinder Cylinder
a. Cylinder number S-IU7 AAL.
b. Cylinder pressure before ^fc. ; !j|
audit, psi
c.. Cylinder pressure after *te. M
audit, psi
d. Audit date and measured
concentration, ppm
Date
Analysis #1 _
Analysis #2 V/iS/7? /oV (1\ 3ff?./.ft) 3*3 ff)
Analysis #3
.^ (Tl)
-------
f. Audit accuracy*
Analysis #1 + 4.Q? % +C>'.5 7. 46.7$%
'Analysis #2 f-fr.'Q % 4 ?.
Analysis £3 47.ovf ?.
* Percent accuracy = Measured ConcRH Cone. x 1QO
g. Problems detected (if any)
^-v i
.(Xj - ,
-------
APPENDIX C
INTEGRATED BAG DATA SHEETS
-------
FIELD DATA
INTEGRATED DAG SAMPLER
. ( 7 3 /
Project No
Method/Type Sample f~r t, L
Run No. T\.
Can No.
Location
Date
Time f ^ /S"
Temp. Ambient
Baro. Press.
Flowmeter Setting
Sample Time Start t *] / 5
Stop
Point
Number
Sampling
Time
Flow
Setting
Tei.iperature
Sample
Pressure
eat
.V?
UL
0
n,
bo
y
d
Comments:
/J-.
. 0) A/.
Scott £n\/ircnm«ntcJ Technclosy Inc
-------
Point
Number
FIELD DATA
INTEGRATED 2AG SAMPLER
Project No
. /7-V
Date
Method/Type Sample
Run No. A
^fT^
Can No.
//t/T
Time / 5V T
Location
Temp. Ambient
Baro. Press.
^x /
/
Flowmeter Setting
Sample Time Start / ) /^
Stop
Sampling
Time
1
ft to
///r
Flow
Setting
Temperature
Sample
Pressure
22.0
. 0
22.0
ents: f~f
<$)
^ 5*1 __/
?) v^V rv^L
,/J ft? A*-^
Scott Environrnentai
o.ol
7^7
inc
* 1 (. 2. o
H
/4.|6
-------
FIELD DATA
INTEGRATED SAG SAMPLER
Project No.
Date
Method/Type Sample
Run No.
Can No.
Time
3 /&
3
Location
^ -
Temp. Ambient
Baro. Press.
Flowmetsr Setting
Sample Time Start
,' / v
stop
Point
Number
Sampling
Time
Flow
Setting
Temperature
Sample
Pressure
3//S.
100
/oo
*>*>&
W.
oc
loo
rf-l
, of A)
Scott Environmental Technology Inc
-------
FIELD DATA
INTEGRATED SAG SAI1PLER
Project No. V )-*»
Method/Type Sample
Run No.
Can No.
Date
Time
. *-f
U/S
90
Location
Temp. Ambient
Baro. Press.
Flowmeter Setting
Sample Time Start
Stop
Iff)?-
Point
Number
Sampling
Time
Flow
Settins
Temperature
Sample
Pressure
.V?
Comments:
Scott Environn>ental Tschncksgy Ire
-------
FIELD DATA
INTEGRATED SAG SAMPLER
Project No.
Date
Method/Type Sample
Run No.
Can No.
Time
0
Location
Temp. Ambient
Baro. Press. 2- /< ~7
Flowmeter Setting
Sample Time Start
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Scott Envircximental Technobsy inc
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FIELD DATA
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Scot: Environmental Technolosy Inc
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FIELD DATA
INTEGRATED 3AG SAMPLER
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(7)
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Scott Environmental Technolosy Inc
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FIELD DATA
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Project No. 10*1^
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Run No.
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Date
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Scott Environmental Techno/c^y Inc
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FIELD DATA
INTEGRATED SAG SAMPLER
Project No. | /
Date
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FIELD DATA
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Project No.
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Date
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Scott Environmental TechnoJosy !nc
-------
Point
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FIELD DATA
INTEGRATED SAG SAMPLER
Project No.
Date
Method/Type Sample
Run No. C.
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Time
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Scott Environmental TecirfegY
-------
FIELD DATA
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Project No. .'> S I-f$
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Date
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Scott EnvironmentaJ Technolosy Inc
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FIELD DATA
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Project No. ("7
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Scort Environnnentai Techndosy Inc
-------
FIELD DATA
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Project No.
.'73
Date
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20/76
Run No.
Can No.
Time
Location
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3
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7
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Comments:
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-------
Project No.
FIELD DATA
INTEGRATED 2AG SAMPLER
Date
Method/Type Sample
Run No. J>^
Can No. H
Time
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Temp. Ambient __^
Flowmeter Setting f*Y'
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Scott Environmental Technology Inc
-------
5-4
SAMPLE IB, BENTONE COLUMN 16X fi 10- ATTENUATION
-------