United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 79-CKO-21
May 1979
Air
oEPA
BaPCoke Ovens
Analysis of Coke Oven
Quench Tower
Water and Coke Samples
-------
ANALYSIS OF COKE OVEN QUENCHING
TOWER WATER AND COKE SAMPLES
(BENZO-ct- PYRENE)
.
Tony E. Egg! es ton
Contract No. 68-02-2812
Work Assignment No. 46
EPA Technical Manager: Daniel G. Bivens
Prepared for:
Emission Measurements Branch
U.S. Environmental Protection Agency
Research Triangle Park, N.C. 27711
ENVIRONMENTAL ENOINEERINQ DIVISION
P.O. Box 13000
Research Triangle Park, North Carolina 27709
-------
CONTENTS
Page
Introduction 1
Benzo-o-Pyrene Analytical Procedure
Sample Preparation
Total Suspended and Dissolved Particulates Analytical Procedures
Recovery Efficiency and Spiking
Determination of Detection Limits
Appendix
-------
INTRODUCTION
A series of sets of samples collected from the coke quenching process
were received by the Environmental Engineering Division of TRW, Inc. for
the purpose of conducting analysis for Benzo-a-Pyrene. Water samples, coke
samples and sludge samples were received from four (4) coke oven quench
towers. The samples collected at each site consisted of:
3 - water samples fa 1,000 ml each)
1 - quench sump sludge sample (vlOO grams each)
2 - coke samples (% 500 grams each).
The sampling locations are shown on Figure 1. All samples collected
represented towers using clean makeup water, except at Lorain. Samples
taken at the two quench towers at Lorain included one tower which used clean
makeup water (denoted by C) and one tower which used dirty makeup water
from the byproducts plant (denoted by D).
The liquid samples (S-|, $2 and $3) were grab samples taken during a
quench. The sludge sample ($4) was dredged from the quench tower sump. Hot
coal samples ($5) were small pieces of coke that fell out of the hot car
during a push. These.samples were then cooled by pouring distilled water
over them. Cool coke samples (85) were taken from the same car as samples
$5, after quenching.
Water and sludge samples were collected in glass bottles (light protec-
ted) with teflon cap liners. Some coke samples needed to be quenched
immediately after sampling so they were sprayed with distilled water before
placement in sample bottles.
Some of the water samples contained suspended coke particles (i.e., all
except makeup water). Each water sample (except makeup water) was filtered
and both portions (filtered solids and water) were analyzed for BaP. Sludge
samples were treated similarily.
For all solids (coke, sludge, filtered solids) the BaP analysis results
are reported in yg of BaP per gram of dry solids. Results for liquid
-------
s
I Coke In
Coke Out.
. I '
J
₯
SS/SS/S/SSSS
\
L
(§)
1
I
( ->6 j Sump
Return
0 Water
- Indicates Sampling Point.
Spray
JFeed Water
' 1
© '
i
^ i (. )
j Clean
I Water
Sludge
Figure 1. Diagram of quench tower streams t:o be sampled during site visits.
2.
-------
samples (or filtrates) are reported in yg of BaP per ml of sample, along
with the dry filterable solids content expressed in mg per ml.
Results of the analyses are shown in Table 1. The samples were analyzed
using fluorescence spectrophotometry. Armco Sample $4 (sludge) is reported
as a liquid as this was the condition of the sample upon arrival and analysis.
3.
-------
-TABLE 1. BENZO-a-PYRENE RESULTS
TEST
SITE
ARMCO
FORD
FAIRFIELD
Sampl
numbe
Sample' Location . .
Clean makeup water
Spray feed water
Sump return water
Sludge
Coke in
Coke out
Clean makeup water
Spray feed water
Sump return water
Sludge
Coke in
Coke out
Clean makeup Water
Spray feed water
Sump return water
Sludge
Coke in
Coke out
Si
S2
S3
S4
S5
SB
si
S2
S3
S4
V
S6
Sl
s2
S3
S4
S5
S6
e Concentration BaP
P
Liquid Solid
yg/ml* yg/ml*
0.0060
0.0065 0.0068
0.0010 0.0052
0.0005
0.0022
0.0053 0.0302
0.0044 0.0195
0.0028
0.0025 0.0068
0.0020 0.0024
Total
yg/ml*
0.0060
0.0133
0.0062
0.0005
0.0022
0.0355
0.0239
0.0028
0.0093
0.0044
1 Total
suspended
Total solids (TS
yg/g + mg/ml
0.0370
0.1085
0.15
0.65
0.0818
0.2929
2.5
0.14
0.78
0.0232
>
j. 0.1206
i «
0.61
0.10
0.1^
Detection Total
limit dissolved
S) solid liq. solids
yg/g yg/ml. mg/ml
0.2
0.2
0.1.
0.1
0.2
0.2
0.1
0.1
0.1
0.2
0.2
0.1
0.1
0.1
0-002
0.002
0.002
0.002
0.002
0.002 0.1766
0.002 0.1630
0.002
0,002 0.1486
0.002 0:1526
Detection Cone of
limit BaP in solid
(TDS) yg ug/g
0.001
0.001 183.73
. 0.001 47.93
0.001
0.001 369.19
0.001 66.58
0.001
0.001
0.001
0.001
0.001 293.10
0.001 19.90
0.001
0.001
0.001
* units expressed in yg of BaP per ml of sample
+ units expressed in yg of BaP per gram of dry solids
-------
TABLE 1 (concluded)
TEST
SITE
LORAIN
LORAIN
Sample Location
Clean makeup water
Spray feed water
Sump return water
Sludge
Coke in
Coke out
Clean makeup water
Spray feed water
Sump return water
Sludge
Coke in
Coke out
Sample
number
YC5
S2"C5
s3-c5
S4-C5
VC5
VC5
srDi
S2"D1
VDi
S4"D1
S5"D1
S6'D1
Concentration BaP
Liquid
yg/ml*
0.0026
0.0252
0.0164
0.0380
0.0396
0.0076
Solid
vg/ml*
0.0055
0.240
0.0500
0.4000
0.0655
0.7100
Total
yg/ml*
0.0081
0.0492
0.0664
0.4380
0.1051
0.7176
1
Total
vg/g +
4
<0
<0
34
<0
<0
.0
.1
.1
.2
.1
'I1
ij
Total Detection
suspended limit
solids (TSS)solid liq.
mg/ml yg/g yg/ml _
0.0882
0.2924
0.475
0.5265
0.002
0.2 0.002
0.2 0.002
0.1
0.1
0.1
' 0.002
0.2 0.05
0.2 0.1
0.1
0.1
0.1
Total
dissolved
solids
, mg/ml
0.9864
0.9842
2.655
1.7404
Detection ' Cone of
limit BaP in solid
(TDS) yg yg/g
0.002
0.002 27.21
0.002 171.00
0.002
0.002 137.89
0.002 1348.53
*units expressed in yg of BaP per ml of sample .
+units expressed in yg of BaP per gram of dry solid
-------
BENZO-a-PYRENE ANALYTICAL PROCEDURE
The procedure for BaP analysis was by means of fluorescence spectro-
photometry. The equipment used for this analysis was the Aminco Model SPF-
125 Spectrophotofluorometer with 7mm lightpath cell. This instrument
accurately measures concentrations of BaP as low as 0.0001 ppm. The wave-
length settings were 378 nm excitation and 403 nm emission with respective
slitwidth openings of 1mm and 5mm. This instrument becomes extremely
substance specific at very narrow slit width, as used.
Solid fractions and sludge samples were extracted using cyclohexane.
The extraction procedure placed the solid or sludge into a single thickness
pre-extracted cellulose extraction thimble. The thimble was then placed in
a soxhlet apparatus and extracted for eight hours at five to six cycles per
hour. All this was done either behind a yellow light-safe screen or under
a yellow safe light. At the end of the extraction the"extract volume was
recorded, and the extract was stored in an amber bottle at 4°C until the
analysis was performed. The thimble was checked with a black light to
confirm complete extraction.
A set of standards were prepared for each range (high, medium, and low
concentrations) by serial dilutions. Each set was analyzed for linearity
by continual measurement throughout the day's testing. Since BaP is light
sensitive, standards and sample aliquots are discarded after analysis with
the samples kept in closed, dark containers. Lastly, a spiking procedure .
was used to determine recovery efficiencies on solid and filtered samples.
All samples and extracts were analyzed without any concentration procedures.
No major problems were encountered with the fluorescence spectrophoto-
metric procedure for BaP analysis. This method is preferred over the thin
layer chromatographic (TLC) method for low level BaP analysis, as the TLC
method had only 0.01 the sensitivity of direct liquid measurement.
The benzora-pyrene method used was tailored to these samples. The
method originally chosen was intended to be a thin layer chromatography
6.
-------
separation and measurement by scanning in-situ with a scanning attachment
for the fluorescence spectrophotometer. .
The TLC method lacked the sensitivity required for the analyses. The
sampled were to be pre-concentrated using Kuderna-Danish concentrators with
a nitrogen stream flowing over them. However, most of the samples would not
reduce.in a reasonable time (i.e., some samples took several weeks to reduce
their volume by 50% while others would not reduce within two weeks, .even ,
with formation of an azeotrope by addition of ethanol). It was found by
reviewing the literature that no compound expected to be present in these
samples had similar excitation/emission spectrum'to benzo-a-pyrene. Previous
analyses by GC/MS on similiar samples were the basis of the compounds to be
considered as interferences. In addition, a general compendium of poly-
organic materials and other organic compounds showed no similar spectrum.1
It was, therefore, decided to go to a direct in-situ method as previously
described.
SAMPLE PREPARATION
Upon receipt each sample was individually inspected to determine its
make-up. In the case of the makeup water samples (SI) no solids were
visible and therefore the samples were analyzed as received. In the case of
those samples having suspended solids the sample were measured volumetrically
and an aliquot taken which was first filtered, the filter materials then
being dried and weighed to determine total dissolved solids and the
remaining liquid portion was brought to dryness to determine gravimetrically
the dissolved solids. From the samples received in the solid state, '. ,
including all of the sludge samples with the exception of sample S4 from
ARMCO, an aliquot was extracted and the BaP concentration measured in the
solvent to determine the concentration in that aliquot. Sample S4 from
ARMCO was an aqueous sludge sample and was therefore treated as a liquid.
Due to its being a very thick liquid, a volumetric aliquot was taken and
placed in an extraction thimble and extracted as a solid, and its values
are reported in micrograms of BaP per ml of liquid extracted.
Fluorescence and Phosphorescence Data Compendium,
Donald L. Helman, American Instrument Co., 1977.
7.
-------
TOTAL SUSPENDED AND DISSOLVED ANALYTICAL PROCEDURES
Total suspended solids were determined by filtration of a known volume
of liquid after thorough agitation of the sample. The pre-weighed filter
was then re-weighed after drying to determine the amount; of solids collected.
Dissolved solids were determined by taking the filtered liquid from the
total suspended solids determination and evaporating to dryness in a tared
container. The residue was then weighed to determine total dissolved solids.
RECOVERY EFFICIENCY AND SPIKING
A series of samples were spiked to determine the recovery efficiency of
the method. The initial attempts at spiking produced results ranging from
negative values to 38% recovery efficiency. It was determined that the
spiking method as well as the storage at room conditions were inadequate.
The spiking attempts were rerun using a direct mixture for liquids. The
spiking solution was spread over the filter or solid particulate matter
using a fine tip syringe to uniformly distribute the spiking solution over
the sample. These were allowed to dry in the absence of light and under
refrigeration, The spiking took place under yellow-chrome light. This
second series of spikes produced recovery efficiencies ranging from 80 to
83 percent recovery. The samples, along with the results, are shown in
Table 2.
DETERMINATION OF DETECTION LIMITS
Upper and lower detection limits show minor variation daily and are
determined by a group of standards prepared for each range with the highest
and lowest standards overlapping the next higher or lower range. An
illustration:
Range
O)
r
CO
O
in
1%
10%
100%
. 8.
-------
TABLE 2
RECOVERY EFFICIENCY
SAMPLE DESIGNATION
ARMCO
Coke in
Coke out
Blank1
ARMCO
Sludge
Coke in
Coke out
Blank
AMOUNT SPIKED*
Ivg)
10
10
10
10
10
10
10
AMOUNT RECOVERED
tug)
0
3.8
8.2
8.0
8.3
8.1"
9.1
%
EFFICIENCY
0
38
82
80
83
81
91
*in each case, the BaP consentration of the sample relative to the spike was less
than 1%, and is excluded from the calculation
Results questionable due to storage at room conditions. See discussion.
9.
-------
The extracted samples were prepared from either the solid or sludge samples
of the T.S.S. (total suspended solids) filter. It is impossible to analyze
the filtered sample without first going through the extraction procedure as
a liquid phase is necessary for this analytical method.
10.
-------
APPENDIX
Sequence of Events
Recorder Charts for Samples
BaP Calibration Curves
Calculations
11.
-------
SEQUENCE OF EVENTS
Received Samples (Site: date) Armco: 6/14/79
Ford: 8/10/79
Fairfield: 8/24/79
Lorain: 8/30/79
Extracted Samples (Site: date) Armco: 6/18/79 - 6/28/79
Ford: 8/13/79 - 8/22/79
Fairfield: 8/28/79 - 9/06/79
Lorain: 9/07/79 - 9/14/79
Sample Analysts (Site: date) Armco: 7/13/79
(Completion) Ford; 8/24/7g
Fairfield: 9/12/79
Lorain: 9/20/79
Draft Report 10/31/79
-------
RECORDER CHARTS FOR SAMPLES
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BaP CALIBRATION CURVES
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CALCULATIONS
Benzo-a-pyrene
1) Prepare a standard curve
2) Read as analyzed concentration from curve
3) Correct by dilution factor or for sample
size extracted.
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