vIEPA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 86-CAD-1
November 1986
Air
Cadmium
Screening
Study Test Report
Cadmium Refining
Industry
Amax Zinc
Company, Inc
East St. Louis,
Illinois
-------
NESHAP Development
Cadmium Emission Testing At The
AMAX Zinc Company, Inc
Primary Zinc Smelter
East St Louis, Illinois
June 1986
EPA Contract No. 86-02-4337
ESED Project No. 80/42
Work Assignment No. 1
CAD-1 E. St. Louis, IL
TRC Project No. 3497-E81-90
Prepared for:
Michael Toney, EPA/EMB
Task Manager
Prepared by:
John H Powell
Work Assignment Manager
Richard A Pirolli
Project Engineer
December 1986
-------
TABLE OF CONTENTS
SECTION PAGE
1.0 INTRODUCTION 1
1.1 Background 1
1.2 Summary of Process 1
1.3 Applicability of EPA Reference Test Methods .... 2
1.3a EPA Method 5 Configurations For Cadmium
1.4 Measurement Program Summary 3
1.4a Baghouse Outlet 3
1.5 Report Sections 4
2.0 SUMMARY AND DISCUSSION OF RESULTS 5
2.1 Method 5 Configuration (w/filter) Modified for Cadmium 5
2.la Cadmium Emissions 5
2.1b Stack Conditions 8
2.2 Method 5 (w/out filter) Modified For Cadmium. ... 8
2.2a Cadmium Emissions 8
2.2b Stack Conditions 8
2.3 Particle Size Distribution 11
2.4 Visible Emissions 11
2.5 Trace Metals 11
3.0 PROCESS DESCRIPTION AND OPERATIONS (PROVIDED BY MRI). 20
3.1 Process Equipment 21
3.2 Control Equipment 22
4.0 DESCRIPTION OF SAMPLE LOCATION 21
4.1 Cadmium and Particle Size 21
4.2 Visible Emissions Observation Locations 21
4.3 Cadmium Product Composite Sample 25
5.0 SAMPLE AND ANALYTICAL PROCEDURES 26
5.1 EPA Method 5 (w/filter) Modified for Cadmium. ... 26
5.2 EPA Method 5 (w/out filter) Modified for Cadmium. . 30
5.3 Particle Size Distribution Sample Collection. ... 32
5.4 Cadmium Dust Analyses 35
6.0 QUALITY ASSURANCE 36
-11-
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LIST OF FIGURES
FIGURE PAGE
2-1 Particle Size Distribution - Baghouse Outlet 15
2-2 Summary of Visible Emissions - Baghouse Outlet (Test 1) ... 16
2-3 Summary of Visible Emissions - Baghouse Outlet (Test 2) ... 17
2-4 Summary of Visible Emissions - Baghouse Outlet (Test 3) ... 18
2-5 Summary of Visible.Emissions - Baghouse Outlet (Test 4) ... 19
4-1 Process and Sampling Points . . 22
4-2 Sample and Velocity Traverse 23
4-3 Observers Location - Visible Emissions 24
5-1 Modified EPA Method 5 Cadmium Sampling Train 27
5-2 Modified EPA Method 5 Cadmium Comparison Sampling Train ... 31
5-3 Particle Size Distribution Sampling Train 33
LIST OF TABLES
TABLE PAGE
2-la English Units - Summary of Controlled Cadmium Emissions
Method 5 Train with Filter 6
2-lb Metric Units - Summary of Controlled Cadmium Emissions
Method 5 Train with Filter 7
2-2a English Units - Summary of Controlled Cadmium Emissions
Method 5 Train without Filter . . 9
2-2b Metric Units - Summary of Controlled Cadmium Emissions
Method 5 Train without Filter 10
2-3 Particle Size Data Summary 12
2-4 Summary of Visual Emissions 13
2-5 Trace Metals 14
-111-
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APPENDICES
A EXAMPLE EQUATIONS AND CALCULATIONS
A.I Cadmium
B FIELD DATA SHEETS
B.I Modified Train With Filter
B.2 Modified Train Without Filter
C SAMPLING LOGS
C.I Daily Summary Log
C.2 Sampling Task Logs
C.3 Sample ID Log
C.4 Chain of Custody Forms
C.5 Crew Chief Field Operation Log
C.6 Recovery Sample Sheet
D VISIBLE EMISSIONS
D.I Observer Certification
D.2 Visible Emissions Field Data Sheets
E CALIBRATION DATA
E.I Summary of Equipment Used During Testing
E.2 Orifices, Dry Gas Meter
E.3 Nozzles
F SAMPLING AND ANALYSIS PROCEDURES
F.I EPA Method 5 Modified for Cadmium
F.2 EPA Method 9 (Visible Emissions)
G LABORATORY ANALYSIS DATA
G.I Cadmium
G.2 Anderson Cascade Impactor
H PARTICULATE
-IV-
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PREFACE
The work described herein was conducted by personnel from TRC
Environmental Consultants, Inc., Midwest Research Institute (MRI), the United
States Environmental Protection Agency Emission Measurement Branch (EPA/EMB)
and AMAX Zinc Co. in East St. Louis, Illinois.
The scope of work was issued under EPA Contract 68-02-4337, Work
Assignment 1. The work was performed under the supervision of John H. Powell,
TRC Work Assignment Manager, and Richard A. Pirolli, TRC Field Team Leader.
Mark Turner of MRI monitored process operations. MRI was responsible for
preparing Section 3 of this report, which deals with process descriptions and
operations. Raymond Ehrhard, Environmental Engineer for AMAX, provided
invaluable assistance and guidance to TRC, EPA and MRI in the performance of
the test program. Michael Toney, Office of Air Quality Planning and Standards
(OAQPS), Emission Measurement Branch, EPA, served as Task Manager and was
responsible for coordinating the test program.
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1.0 INTRODUCTION
1.1 Background
Section 112 of the Clean Air Act of 1977 charges the administrator of the
United States Environmental Protection Agency with the responsibility of
establishing National Emission Standards for Hazardous Air Pollutants (NESHAP)
that may significantly contribute to air pollution. When promulgated, these
standards of performance are to reflect the degree of emission limitation
achievable through application of the best demonstrated emission control
technology. Emission data collected from controlled sources in the cadmium
industry may provide a portion of the data base used by EPA to develop a
NESHAP.
EPA Industrial Studies Branch (ISB) selected AMAX Zinc Co. in East St.
Louis, Illinois, as a site for an emission test program because it is
considered to employ process and emission control technology representative of
modern cadmium oxide manufacturing plants. The test program was designed to
develop controlled emission factors for Cadmium Oxide production.
TRC Environmental Consultants, Inc. was retained by the EPA Emission
Measurement Branch (EMB) to perform emission measurements at the AMAX Zinc Co.
in East St. Louis, Illinois. Testing was performed on the cadmium oxide
baghouse outlet. This report has been prepared in accordance with EPA
Contract No. 68-02-4337 under the provisions of Work Assignment No. 1.
Midwest Research Institute (MRI), the NESHAP contractor, was responsible
for coordinating the overall test program with AMAX personnel and for assuring
that process and control equipment operating conditions were suitable for
testing. Related process data were monitored and recorded by MRI.
1.2 Summary of Process
CONFIDENTIAL
-i-
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1.3 Applicability of EPA Reference Test Methods
EPA is required to publish a national reference test method for each
regulated source category and pollutant for which a National Emission
Standards for Hazardous Air Pollutants (NESHAP) is established. Reference
test methods are usually specified by a state regulatory agency during the
State Implementation Planning process and may be different from national
reference test methods.
The purpose of establishing a national reference test method is to ensure
that emission data collected from a specific source is representative of that
source and comparable to data collected at other designated sources. The
primary purpose of this test program was to collect emission data using
standardized test methods which will allow the data to be evaluated to develop
a NESHAP. Two modified configurations of EPA Method 5 were identified to
measure emissions from cadmium oxide production. These methods are described
in detail in Section 5.
1.3a EPA Method 5 Configuration For Cadmium
Cadmium emissions were measured by two different configurations of EPA
Mthod 5. In the first configuration a flexible line was placed between the
filter and impingers. In the second, the filter was eliminated from the train
and flexible line was used to connect the probe to the first impinger. In the
first configuration, five percent Nitric Acid was placed in the first two
impingers, and the second five percent in the first three.
-2-
-------
It should be noted that the flexible line was used because of a
particularly difficult sampling location and would not normally be a component
of a cadmium sampling train.
Five percent Nitric acid is used as the impinger solution because metals
are readily soluble in Nitric acid and also Nitric acid increases capture
efficiency.
1.4 Measurement Program Summary
The measurement program was conducted at the AMAX Zinc Co. in East St.
Louis, Illinois during the week of June 16, 1986. Tests were performed at the
cadmium oxide furnace baghouse outlet.
All emission testing was performed by TRC. MRI personnel monitored
process operating conditions. Michael Toney of EMB observed the test program.
1.4a Baghouse Outlet
Preliminary Measurements
Preliminary testing was performed on June 16, 1986 to determine volumetric
flowrate and stack gas moisture content. An integrated gas sample was also
taken to determine concentrations of C02, 02, and CO, which were found to
be ambient. Stack diameter and the sampling port configuration were confirmed
at this time.
Method 5 (configuration) modified for cadmium
Eight Method 5 tests modified for cadmium were performed, four on June 17
and four on June 18, 1986. One of the test on June 17, 1986 was invalid due
to a leak in the sampling train.
Particle size distribution test
One particle size distribution test was performed on June 18, 1986 using
an Anderson Mark IV Cascade Impactor.
-3-
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Method 9 - Visible emissions
Visible emissions from the baghouse outlet were observed concurrently with
each Method 5 modified for cadmium test.
Cadmium Dust
Samples of cadmium dust from the baghouse were drawn from the baghouse
every half-hour during each emission test.
1.5 Report Sections
The remaining sections of this report present the Summary and Discussion
of Results (Section 2), Process Description and Operations (Section 3),
Description of Sampling Locations (Section 4), Sampling and Analytical
Procedures (Section 5), and Quality Assurance (Section 6). Methods and
procedures, field and laboratory data, and calculations are presented in
various appendices as noted in the Table of Contents.
-4-
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2.0 SUMMARY AND DISCUSSION OF RESULTS
A summary of all emission measurements and collected data is presented in
this section. Section 2.1 presents cadmium results collected with the Method
5 train (with filter) modified for cadmium and a complete breakdown and
discussion of parameters. Cadmium results collected with the Method 5 train
(without a filter) modified for cadmium are presented in Section 2.2. Section
2.3 presents the particle size distribution and Section 2.4 summarises the
visible emission observations. Section 2.5 presents results of the trace
metals and baghouse dust analyses.
The cadmium results indicate that there was no significant difference
between the sampling train with filter than the train without filter.
2.1 Method 5 (configuration) Modified For Cadmium
A total of four tests were conducted using the Method 5 train (with
filter) modified for cadmium. The second test was discarded due to an
unacceptable isokinesis of 134%. The first test had an isokinesis of 114% but
it was decided to keep the test. All other tests were acceptable with
100± 10 percent isokinesis. All tests had an acceptable leak rate of
<0.02 cfm.
2.la Cadmium Emissions
Tables 2-la (English Units) and 2-lb (Metric Units) present a summary of
measured cadmium emissions from the baghouse outlet using the Method 5 train
with the filter.
The average total cadmium concentration was 1.55x10"2 gr/DSCF (35470
ug/NM3) and ranged from 1.15x10"2 gr/DSCF (26350 u/NM3) to
1.76x10"2 gr/DSCF (40440 ug/NM3). All significant amounts of cadmium
concentrations and emission rates were found in the front half of sampling
train.
-5-
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TABLE 2-la (English Units)
Summary of Controlled Emissions
Method 5 Train with Filter
AMAX Zinc Co.
Baghouse Outlet
TEST NO
DATE
TIME
Sample Conditions
Volume (DSCF)1
Front Half Catch (ug)
Back Half Catch (ug)
Total Catch (ug)
Isokinesis (%)
Stack Conditions
1A
6/17/86
0900-1106
67.61
77200
42.1
77242
114.2
3A
6/18/86
1115-1322
52.86
39500
25.2
39525
104.6
4A
6/18/86
1420-1635
54.73
61400
9.6
61410
102.5
AVG
—
—
—
—
—
Temperature (°C) 233
Cadmium Emissions
Front Half
Concentration (gr/DSCF) 1.76x10
Back Half
Concentration (gr/DSCF) 9.61x10
Total Cadmium Emissions
Concentration (gr/DSCF) 1.76x10
227
-2
-6
- 2
230
1.15xlO~2 1.73xlO~2
7.36xlO"6 2.71xlO"6
229
1.55x10
6.56x10
-2
-6
1.15x10"
1.73x10
- 2
1.55x10
-2
1 Standard Conditions: 29.92 in Hg @ 68°F
-6-
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TABLE 2-lb (Metric Units)
Summary of Controlled Emissions
Method 5 Train with Filter
AMAX Zinc Co.
Baghouse Outlet
TEST NO
DATE
TIME
1A
6/17/86
0900-1106
3A
6/18/86
1115-1322
4A
6/18/86
1420-1635
AVG
Sample Conditions
Volume (NM3)1
Front Half Catch (ug)
Back Half Catch (ug)
Total Catch (ug)
Isokinesis (%)
Stack Conditions
Temperature (°C)
Cadmium Emissions
Front Half
Concentration (ug/NM3)
Back Half
Concentration (ug/NM3)
Total
Concentration (ug/NM3)
1.91
77200
42.1
77242
114.2
112
40420
22.04
40440
1.50
39500
25.2
39525
104.6
108
26330
16.80
26350
1.55
61400
9.6
61410
102.5
110
39610
6.19
39620
110
35450
15.01
35470
Standard Conditions: 760 mm Hg @ 20°C
-7-
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2.1b Stack Conditions
Stack temperature during this test series averaged 229°F and ranged from
233°F to 227°F.
2.2 Method Configuration 5 (w/out filter) Modified For Cadmium)
A total of four tests were conducted using the Method 5 train (without
filter) modified for cadmium. The second test was deleted due to an
unacceptable leak rate of >0.02 cfm. All other tests were acceptable with a
leak rate of <0.02 cfm and 100±10 percent isokinesis.
2.2a Cadmium Emissions
Table 2-2a (English units) and Table 2-2b (Metric units) present a summary
of measured cadmium emissions from the baghouse outlet.
The total average cadmium concentration was 1.62x10 "2 gr/DSCF (37000
ug/NM3) and ranged from 1.45x10"2 gr/DSCF (33220 ug/NM3) to
1.61x10"2 gr/DSCF (36940 ug/NM3).
2.2b Stack Conditions
Stack exhaust gas temperature during this test series averaged 236°F and
ranged from 241°F to 230°F.
-8-
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TABLE 2-2a (English Units)
Summary of Controlled Emissions
Method 5 Train w/o Filter
AMAX Zinc Co.
Baghouse Outlet
TEST NO
DATE
TIME
Sample Conditions
Volume (DSCF)1
Front Half Catch (ug)
2nd Impinger Catch (u)
3rd&4th
Impinger Catch (ug)
Total Catch (ug)
Isokinesis (%)
Stack Conditions
IB
6/17/86
0900-1106
64.63
49400
7070
4330
60800
109.2
3B
6/18/86
0834-1215
66.03
52600
9920
6560
69080
109.4
4B
6/18/86
1420-1636
62.40
40800
31100
378
72278
107.6
AVG
—
—
—
—
—
—
Temperature (°F) 230
Cadmium Emissions
Front Half (Probe Wash & 1st Impinger)
Concentration (gr/DSCF)1.18x10 z
241
1.23x10"
2nd Impinger
Concentration (gr/DSCF) 1.69x10
3rd&4th Impinger
Concentration (gr/DSCF) 1.03x10
Total Cadmium Emissions
Concentration (gr/DSCF) 1.45x10
-3
- 3
- 2
2.32x10
- 3
1.53x10
1.61x10
-3
238
1.01x10"
7.69x10"
-2
9.35x10
1.79x10
-5
-2
236
1.14x10
-2
3.90x10"
8.84x10"
1.62x10
-2
1 Standard Conditions: 29.92 in Hg @ 68°F
-9-
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TABLE 2-2b (Metric Units)
Summary of Controlled Emissions
Method 5 Train w/o Filter
AMAX Zinc Co.
Baghouse Outlet
TEST NO
DATE
TIME
IB
6/17/86
0900-1106
3B
6/18/86
0834-1215
4B
6/18/86
1420-1636
AVG
1.83
49400
7070
4330
60800
109.2
110
Sample Conditions
Volume (MM3)1
Front Half Catch (ug)
2nd Impinger Catch (ug)
3rd&4th
Impinger Catch (ug)
Total Catch (ug)
Isokinesis (%)
Stack Conditions
Temperature (°C)
Cadmium Emissions
Front Half (Probe Wash & 1st Impinger)
Concentration {ug/NM3)26990
2nd Impinger
Concentration (ug/NM3) 3860
3rd&4th Impinger
Concentration (ug/NM3) 2370
Total Cadmium Emissions
Concentration (ug/NM3) 33220
1.87
52600
9920
6560
69080
109.4
116
28130
5300
3510
36940
1.77
40800
31100
378
72278
107.6
114
23050
17570
220
40840
113
26060
8910
2030
37000
Standard Conditions: 760mm Hg @ 20°C
-10-
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2.3 Particle Size Distribution
Table 2-3 presents particle size data summary from the baghouse outlet.
Figure 2-1 presents a graph of particle size to cumulative percent less than
cut diameter. Table 2-3 includes sampling time, sample volume, effective cut
diameter, size range and percent in size range.
Particle size data show that 26.0% of the particles are in the 0.68 to
1.11 urn size range, 21.3% in the 2.25-3.53 urn range and 18.5% of the
particles are in the 1.11-2.25 urn size range. Figure 2-1 indicates that the
particle size distribution is unimodal.
2.4 Visible Emissions
A summary of visible emission observations from the baghouse outlet is
presented in Table 2-4. Average opacities are presented for 6 minute time
periods during each test. The average opacity was 3% for tests 1, 2 and 4 and
5% for test 3. These 6-minute average opacities are presented graphically in
figures 2-2 through 2-5.
2.5 Trace Metals
One sample and blank per set of tests, baghouse dust and lab blanks were
analyzed for trace metals by A.A. Barium, chromium, copper, iron, lead,
magnesium, manganese, mercury, nickel and zinc were analyzed. Mercury was
analyzed for the train without the filter but not for the train with the
filter. Mercury was not analyzed for the train with the filter because of the
difficult digestion procedure. The baghouse dust and road dust was also
analyzed for cadmium. Table 2-5 presents a summary of the trace metals
results. All sample train results were corrected for field and/or laboratory
blanks. Trace metals for the sample train blanks were high, possibly due to
the nitric acid rinse of the nozzles.
-11-
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TABLE 2-3
Particle Size Data Summary
Baghouse Outlet
AMAX Zinc Co.
June 18, 1986
SAMPLING TIME: 90 MINUTES
SAMPLE VOLUME: 46.50 DSCF
ho
I
STAGE
PS&O
1
2
3
4
5
6
7
Backup
EFFECTIVE
CUT DIAMETER
>11.16
7.06
5.19
3.53
2.25
1.12
0.680
0.457
<0.457
SIZE
RANGE (p)
>11.16
7.06-11.16
5.19-7.06
3.53-5.18
2.25-3.53
1.12-2.25
0.680-1.12
0.457-0.680
<0.457
STAGE
SAMPLE (Mg)
0.07
0.69
4.69
6.72
9.63
8.34
11.71
1.50
1.77
45.12
% IN
SIZE RANGE
0.15
1.5
10.4
14.9
21.3
18.5
26.0
3.3
3.9
CUMULATIVE % LESS
THAN CUT DIAMETER
99.8
98.3
87.9
73.0
51.7
33.2
7.2
3.9
—
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Table 2-4
Sunmary of Visible Emissions
Baghouse Outlet
AMAX Zinc Co.
East St. Louis, Illinois
TEST NO 1
6/17/86
0900-1116
SIX MINUTE AVERAGE
TIME PERIOD OPACITY (%)
0909-0915
0915-0921
0921-0927
0927-0933
0933-0939
0939-0945
0945-0951
0951-0957
0957-1003
1003-1009
1009-1015
1015-1021
1021-1027
1027-1033
1033-1039
1039-1045
1045-1051
1051-1057
1057-1103
1103-1109
AVG
4
5
5
4
6
3
4
4
3
3
3
3
2
2
1
2
1
2
1
fi
3
TEST NO 2
6/17/86
1308-1520
SIX MINUTE
TIME PERIOD
1308-1314
1314-1320
1320-1326
1326-1332
1332-1338
1338-1344
1344-1350
1350-1356
1356-1402
1402-1408
1408-1414
1414-1420
1420-1426
1426-1432
1432-1438
1438-1444
1444-1450
1450-1456
1456-1502
1502-1508
1508-1514
1514-1520
AVG
AVERAGE
OPACITY (%)
4
5
4
4
3
1
2
1
3
2
0
3
4
3
1
4
5
4
3
3
2
1
3
TEST NO 3
6/18/86
0828-1328
SIX MINUTE AVERAGE
TIME PERIOD OPACITY (%)
0828-0834
0834-0810
0840-0846
0846-0852
0852-0858
0858-0904
0904-0910
0910-0916
0916-0922
0922-0928
0928-0934
0934-0940
0940-0946
STOP TEST
110-1116
116- 122
122- 128
128- 134
134- 140
134- 140
1140- 146
1146- 152
1152- 158
1158-1204
1204-1210
1210-1216
1216-1222
1222-1228
1228-1234
1234-1240
1240-1246
1246-1252
1252-1258
1258-1304
1304-1310
1310-1322
1322-1328
AVG
4
1
5
5
5
5
4
4
5
5
5
5
4
5
5
5
5
8
8
7
7
5
6
4
1
0
3
5
5
5
5
5
2
2
5
5
5
TEST NO 4
6/18/86
1420-1644
SIX MINUTE
TIME PERIOD
1420-1426
1126-1432
1432-1438
1438-1444
1411-1450
1450-1456
1456-1502
1502-1508
1508-1514
1514-1520
1520-1526
1526-1532
1532-1538
1538-1544
1544-1550
1550-1556
1556-1602
1602-1608
1608-1614
1614-1620
1620-1626
1626-1632
1632-1638
AVG
AVERAGE
OPACITY (%)
0
0
3
1
0
3
1
0
2
2
3
2
4
5
4
4
1
2
5
4
4
3
5
3
-------
TABLE 2-5
TRACE METALS
AMAX ZINC CO
BAGHOUSE
JUNE 1986
SAMPLE
ROAD
DUST
HN03
BLANK
LAB
BLANK
TRACE METAL
Barium (pg)
Cadmium1
Chromium (ug)
Copper (ug)
Iron (ug)
Lead (ug)
Magnesium (pg)
Manganese (ug)
Mercury (ug)3
Nickel (ug)
Zinc (ug)
7850ug/g
nd>25
nd<25
nd<5.0
nd<4.0
0.131ug/ml
nd<23
0.023ug/ml
nd<4.0
nd<7.0
0.276ug/ml
nd<5.0
nd<4.0
nd<7.0
nd<23
2.7
nd<4
nd<7.0
nd<0.9
1 Cadmium considered major metal refer to Tables 2-1 and 2-2
2 nd = Non Detected
3 Mercury was not analyzed due to the difficult digestion procedure for the
train with filter
-14-
-------
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FIGURE 2-
PARTICLE SIZE DIS1
BAGHOUSE OU1
AMAX ZINC C(
June 18, 19!
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TEST 1 - 6/17/86
I
0909 0927
0945
1003
1021
1039
1058
1116
TIME
Figure 2-2. Summary of Visible Emissions form Baghouse Outlet
Amax Zinc Co., E. St. Louis, Illinois
-16-
-------
20
TEST 2 - 6/17/86
£T 15
et
O_
o
C3
et
10
o
1308
J~L
1326 1344 1402 1420 1438 1456
TIME
1514
1532
Figure 2-3. Summary of Visible Emissions from Baghouse Outlet
Amax Zinc Co., E. St. Louis, Illinois
-17-
-------
20
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TEST 3 - 6/18/86
5
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0828 0846 0904 0922 0940 0958 1110 1128 1146 1204
TIME
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1222 1240 1258
i I
1310 1328
Figure 2-4. Summary of Visible Emissions from Baghouse Outlet
Amax Zinc Co., E. St. Louis, Illinois
-------
20
15
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TEST 4 - 6/18/86
n
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1420 1438 1456
1514 1532
TIME
1550 1608 1626 1644
Figure 2-5. Summary of Visible Emissions from Baghouse Outlet
Amax Zinc Co., E. St. Louis, Illinois
-19-
-------
3.0 PROCESS DESCRIPTION AND OPERATIONS (Provided by MRI)
CONFIDENTIAL
3.1 Process Equipment
CONFIDENTIAL
3.2 Control Equipment
CONFIDENTIAL
-20-
-------
4.0 DESCRIPTION OF SAMPLING LOCATION
This section presents a description of each sampling location. Figure 4-1
presents a schematic layout of the cadmium oxide process and identifies all
sampling locations.
4.1 Cadmium and Particle Size
The cadmium oxide baghouse outlet was sampled in the 19-inch diameter duct
which exits the top of the baghouse, enters the I.D. fan and exits through a
stack. Sample ports are located 90° apart on the duct section preceding the
fan 12 diameters downstream of a bend and 1.8 diameters upstream of the ID
fan. Point A in figure 4-1 presents this location.
In accordance with EPA Method 1, sampling was performed at 12 traverse
points through the two sample ports simultaneously. Figure.4-2 presents the
sample port configuration and a cross section of the duct showing the exact
distance of each sampling point from the duct wall.
Each Method 5 test lasted 120 minutes (10 minutes traverse point). The
particle size test was run for 90 minutes. Particle size sampling was
performed at an average point of flow in the stack.
4.2 Visible Emissions Observation Locations
A certified visible emissions observer read at the exhaust opacity at the
cadmium oxide baghouse stack for a period of 2 hours during each test. Sample
Point C in Figure 4-1 depicts the exhaust point.
The observers location was determined in accordance with EPA Method 9 and
considering obstructions and traffic problems in the area.
The Method 9 data reduction was calculated by taking 6 minute averages for
the entire length of the test. Location of the observer can be found in
Figure 4-3.
-21-
-------
SAMPLE
POINT C
CADMIUM OXIDE BAGHOUSE
-*•
SAMPLE
POINT A
• SAMPLE
POINT B
Figure 4-1. Process and Sampling Points
AMAX Zinc Co., Sauget, 111.
-22-
-------
Environmental
EPA Method 1 Sample and Velocity Traverse
•-C O
F
-•Jrm EPA/AMAX ZINC CO. Total
, pr»Hnn CADMIUM OXIDE BAGHOUSE Numbf
Diameters Up;
Diameters Dov
rMINIMUM NUM
A
Duct Diam
0.5
>o - 1
IGURE 4-2
Traverse Points Req
>r of Ports 2
;tr»»m... -L2_ Points Ppr pprt
jnctrpam 1.8 Travf
BER OF TRAVERSE POINTS FOF
NO NONPARTICULATE TRAVERSE
eters Upstream from Flow C
(Distance A)
1.0 - 1.5
i i i i
HIOHCN NUM»IN it ron
RICTAMQULAA ITACU ON OUCTI
10-
K) - --PARTICULATE
24 of 25 f
'0 -
I 20
6
Jrse ( Horizontal or
\ PARTICULATE U_
:s
Hsturbance /
2.0
i i
-A-/OIITVWANCI
A
-| - :- tin
I
J_ 1 OIITUMANCE
-
\
*—
1Q I 16 *TACKDIAMITiR>e.l1mlJ«UJ
10- ^NC
I
1 . 1
)NPARTICULATE
VTACK OlAMETtH -
1 1 1 1
12
I 8 or 9
-
CJOTOO.n m (1214UJ
1 1
23456789
Duct Diameters Downstream from Flow Disturbance
(Distance B)
v LOCATION OF TRAVERSE POINTS IN CIRCULAR STACKS
Point
Number
On A
Diameter
. 1
2
3
4
5
6
7
8
9
10
11
12 :
(Percent of stack diameter from
inside wall to traverse point)
Number Of Traverse Points On A Diamet
46 8 10 12
6.7 4.4 3.2
25.0 14.6 10.5
75.0 29.6 19.4
93.3 70.4 32.3
85.4 6*7.7
95.6 80.6
89.5
96.8
2.6 2.
er
1
8.2 6.7
14.6 11.8
22.6 17..7
34.2 25.0 .
65.8 35.6
77.4 64.4
85.4 75.0
91.8 82.3
97.4 88.2
93.3
97.9
for Stationary Sourc
uirpH 12
Vertical) HORIZONTAL
iS
]
_i
1
1
°eq * L+W'=
r
36'
Sample i r
Port :>
240"
t*
/
CROSS-SECTIONAL LAYOUT
FOR RECTANGULAR STACKS
Total
Traverse Points Matrix
9 3x3-
12 4x3
16 .4x4
20 5x4
25 5x5
'TRAVERSE POINT LOCATIONS
No.
1
2
3
4
5
6
7
8
9
10
11
12
Distance Nippl
From Wall Size
0.9
2.9
5.9
14. I
17.1
19-
e • Total
Distanc
:
t
-23-
-------
PIGMENT
1
1
1
1
BUILDING
I
NJ
SUN
TEST 3
•4
TEST 1
Figure 4-3 Observers Location
Visible Emission
Amax Zinc Co
Baghouse Outlet
June 1986
-------
4.3 Cadmium Product Composite Sample
A sample of the baghouse dust was collected at Sample Point B as shown in
Figure 4-1. Samples were collected at half hour intervals during each test
run. All half hour samples were then mixed into one representative sample.
The resulting composite was returned to TRC and analyzed for trace metals by
GFAA using a Parr Bomb digestion with nitric acid.
-25-
-------
5.0 SAMPLING AND ANALYTICAL PROCEDURES
This section presents descriptions of sampling and analysis procedures
which were employed during the emission testing conducted at the AMAX Zinc
Company facility in East St. Louis, IL.
A combination of EPA Methods 1, 2, 3, 4, 5 (modified for Cadmium), and 9
were used to measure cadmium emissions from the Cadmium Oxide Baghouse
exhaust. In addition, one Andersen cascade impactor sample was taken to
determine particle size distribution.
A composite sample of cadmium product was analyzed for trace metals using
a Parr Bomb digestion and graphite furnace atomic absorption (GFAA).
5.1 EPA Method 5 with filter (Modified for Cadmium)
Cadmium sampling was performed by using two configurations of the Method 5
sampling train1. The first is shown schematically in Figure 5-1 and
consists of a nozzle, probe, filter with glass frit, a flexible Teflon
umbilical line, four impingers, vacuum pump, dry gas meter, and an orifice
flow meter. One modification of the standard EPA Method 5 train consists of
placing flexible Teflon tubing between the filter and the impingers. This
modification makes the sampling eguipment much easier to handle. A second
modification is the use of 5% nitric acid in first two impingers . The
sampling train was calibrated before and after this test program. This method
is based on the proposed methodology presented in Appendix F.
1 Code of Federal Regulations 40, Part 60 Appendix A, July 81
-26-
-------
i
ro
16
I
©
14
16
;6* ^
/—^ — . i ,J
STACK WALL-
1
13
LEGEND
1 - NOZZLE
2 - PROBE
3 - FILTER HOLDER
4 - HEATED FILTER BOX
5 - IMPINGER ICE BATH
6 - UMBILICAL CORD
7 - VACUUM GAUGE
8 - MAIN VALVE TO PUMP
9 - PUMP
10 - BYPASS VALVE
11 - DRY GAS METER
12 - ORIFICE AND MANOMETER
13 - PITOT TUBE AND MANOMETER
14 - THERMOCOUPLE READOUT
15 - FLEXIBLE TEFLON SAMPLE LINE
[6 - THERMOCOUPLES
17 - IMPINGER OUTLET TEMPERATURE
Figure 5-1. Modified EPA Method 5 cadmium sampling train
(August 18, 1977 Federal Register)
-------
A nozzle was attached to a stainless steel glass-lined probe which was
heated to prevent condensation. Whatman EPM-1000 fiberglass filter paper
supported in a 4 1/2 inch glass filter holder with a glass frit was used as a
particulate collection medium. Filters was desiccated and pre weighed. A
visual inspection for irregularities in the filter material was conducted.
The filter assembly was enclosed in a heated box to keep the filter
temperature at approximately 150° F (±10), which is approximately the same
as the stack temperature. A thermocouple, located inside the back half of the
filter holder, monitors the gas stream temperature to ensure proper filter
temperature.
Four impingers immersed in an ice bath were attached to the back end of
the filter holder with a flexible Teflon tube. The first two impingers each
contained 100 ml of 5% nitric acid, the third was empty and the fourth
contained 200 grams of silica gel to remove any remaining moisture. Impinger
outlet temperatures were kept between 50°F to 80°F.
Flexible tubing, vacuum gauge, needle valve, leakless vacuum pump, bypass
valve, dry gas meter, calibrated orifice and inclined manometer complete the
sampling train. A check valve was not used in the TRC sampling train.
A nomograph was used to quickly determine the orifice pressure drop
required for any pitot velocity pressure and stack temperature in order to
maintain isokinetic sampling conditions. Sampling flow was adjusted by means
of the bypass valve. Before and after each particulate test run the sampling
train was leak checked. Sample time was 120 minutes per run.
Test data recorded at ten minute intervals for each sampling point
included: test time, sampling duration at each traverse point, pitot pressure,
stack temperature, dry gas meter volume and inlet-outlet temperatures, probe
temperature, and orifice pressure drop.
-28-
-------
Due to the large negative static pressure in the duct, sampling trains
were started and stopped prior to stack entry and stopped after stack exit.
This procedure mitigated any effects of suction on the sampling media.
Sample Recovery
Sample recovery was performed in a clean, wind-free area to avoid sample
contaimination. A 22 foot by 8 foot high-cube truck provided shelter. The
following fractions were recovered:
Container No. 1
Container No. 2
Container No. 3
Container No. 4
The glass fiber filter was removed from its holder and
deposited in an inert petri dish and then sealed.
The probe, nozzle and front-half of the filter holder was
rinsed and brushed three times with 5% HN03 into a 500 ml
glass sample jar with a Teflon-lined lid.
The Teflon line was drained into the first impinger. The
first three impinger's volumes were determined
gravimetrically to the nearest 0.5g. The contents were then
deposited into a 1000 ml glass sample jar with a Teflon
lined lid. The back-half of the filter holder, the Teflon
line, and the first three impingers were each rinsed three
times with 5% HN03, measured then added into the 1000 ml
sample jar.
The silica gel was be returned to its original container and
weighed to the nearest 0.5g.
Sample Analyses
' Sample analyses was performed in TRC Environmental Laboratories in East
Hartford, CT. The sample fractions were analyzed as follows:
Container No.1
Container No.2
Container No. 3
Container No. 4
The filter was desiccated and weighed for particulate. The
filter was digested, extracted and then analyzed for cadmium
by graphite furnace atomic absorbtion. One set of samples
was be analyzed for trace metals.
Nozzle and probe rinse was dryed and weighed, then brought
back to solution with HN03. The solution was extracted
and analyzed as Container No. 1.
The solution was analyzed as Container No. 2.
The silica gel was weighed to the nearest 0.5g.
-29-
-------
Trace metals standards purchased from J. T. Baker Standards, which are NBS
traceable, were used for all trace metals analyses. Samples were concentrated
or diluted in order to bring the analysis range into the center of the Atomic
Absorption linearity curve. All samples were analyzed in triplicate as a
measure of precision. A complete discription of the analytical procedure can
be found in the Appendix of this test report.
The trace metals analyzed for are:
Barium
Chromium
Coppe r
Iron
Lead
Magnesium
Manganese
Nickel
Zinc
5.2 EPA Method 5 (without filter) Modified for Cadmium
A second Method 5 sampling train for simultaneous cadmium testing was used
as a method development tool to determine the best sample train component
arrangement for cadmium. This sampling train is shown in Figure 5-2. This
train consisted of a heated probe (150° + 10°F) and five impingers. The first
three each contained 100 ml of 5% HN03. The fourth was empty and the last
contained 200 grams of silica gel. No filter was present in this train so any
particulate captured was collected in the impinger solutions.
Impinger outlet temperatures did not exceed 80°F. Data was recorded as
previously described in Section 5.1.
Sample Recovery
Sample recovery was performed in the location described in Section 5.1.
-30-
-------
i
U)
13
STACK WALL
LEGEND
1 - NOZZLE
2 - PROBE
3 - IMPINGER ICE BATH
4 - UMBILICAL CORD
5 - VACUUM GAUGE
6 - MAIN VALVE TO PUMP
7 - PUMP
8 - BY-PASS VALVE
9 - DRY GAS METER
10 - ORIFICE AND MANOMETER
11 - PITOT TUBE AND MANOMETER
12 - STACK TEMPERATURE READ OUT
13 - THERMOCOUPLES
Figure 5-2. Modified EPA Method 5 Cadmium Sampling Train
(modified for cadmium sampling method comparison)
-------
Container No. 1 The probe and nozzle were rinsed and brushed three times
with 5% HMOs into a 1000 ml glass sample jar with a
Teflon-lined lid. The first impinger was weighed to
determine moisture gain and the contents deposited in the
jar. The impinger was then rinsed three times with 5%
measured and added into the sample jar.
Container No. 2 The second impinger was weighed to determine moisture gain
and the contents deposited into a 500 ml glass sample jar
with a Teflon-lined lid. The impinger was then rinsed three
times with 5% HN03 measured and added into the jar.
Container No. 3 Impingers 3 and 4 were combined and treated as Impinger 2.
Container No. 4 The silica gel was weighed to the nearest 0.5 g to determine
moisture gain.
Sample Analyses
Containers 1 through 3 was analyzed for cadmium and trace metals by GFAA
as described in Section 3.1.
5.3 Particle Size Distribution Sample Collection
The particle size distribution sampling train is shown schematically in
Figure 5-3. The train consisted of a nozzle, Andersen right-angle inlet
pre-separator, Andersen Mark III cascade impactor, probe, flexible umbilical
line, impinger, vacuum pump, dry gas meter, and orifice flowmeter. Reeve
Angel 934AH fiberglass substrates are used as the sample collection media in
the impactor. One impinger in an ice bath was connected to the probe by a
flexible umbilical tube. The impinger contained silica gel to remove sample
stream moisture prior to the gas meter. A vacuum gauge, needle valve,
leakless vacuum pump, bypass valve, dry gas meter, calibrated orifice, and
inclined manometer complete the sampling train.
Before each particle size sample collection run, the assembled sampling
train was leak checked. The accpetable leak rate was less than 0.02 cfm at 5
inches of mercury vacuum. A nomograph was used to determine the orifice
-32-
-------
CASCADE
IMPACTOR
ASSEMBLY
1
VACUUM
TUBING
THERMOMETER
«Ss
t^-
PITOT TUBE
STACK WALL HEATED
PROBE
1
PITOT ,J
MANOMETER \
THERMOMETERS
ORIFICE
1
ss
4
(
ICE BATH
• (rl
-
J
X
VALVE
<>. VACUUM GAUGE
^ 9 I
VACUUM
LINE
IMPINGER UITil
SILICA GEL
MAIN
VALVE
AIR TIGHT
PUMP
DRY GAS
METER
Figure 5-3. Particle size distribution sampling train.
-------
pressure drop required to maintain isokentic sampling conditions at the sample
point velocity and temperature. Sampling time of 90 minutes was observed.
At the conclusion of the sampling time period, the sample flow was shut
off and the pre-separator/impactor assembly carefully removed from the duct
and maintained in a horizontal position. The nozzle and outlet ends were then
sealed with Parafilm® and the assembly kept vertical and carefully
transported to the clean-up area.
Sample recovery performed in the same area described in Section 5.1. The
recovered sample fractions are identified as follows:
• Container No. 1: Acetone wash from the nozzle, pre-separator,
interconnecting coupling, and impactor inlet throat.
• Container No. 2
through 8: Individual substrates and back-up filters in their
respective containers.
The following analyses was performed on these samples:
• Container No. 1: Transfer the acetone washing to a tared beaker and
evaporate to dryness at ambient temperature and
pressure. Desiccate and dry to a constant weight.
Report results to the nearest 0.1 mg.
• Containers No. 2
through 8: Transfer the filter, and any loose particulate
matter from the sample container to a tared glass
weighing dish, desiccate the dry to a constant
weight. Report results to the nearest 0.1 mg.
A calculator program developed by TRC is used to calculate volume sampled
at standard conditions, particulate concentration (grains/DSCF), flowrate
(ACFM), viscosity, mean free path, and cutoff diameter per stage.
-34-
-------
5.4 Cadmium Dust Analyses
Samples of cadmium dust from the baghouse were drawn during each test for
trace metals and particle size distribution analyses. One 500 ml glass sample
jar with a Teflon-lined lid was filled at half-hour intervals during each
emission test. These samples were composited for one set of trace metals
analyses. A complete outline of analytical procedure can be found in
Appendix F.
Trace Metals Analyses
One dust sample was digested in nitric acid in a Parr Bomb and then
analyzed for trace metals by GFAA. The sample was broken into nine aliquots
individually analyzed as a measure of precision. The following summarizes
principal Trace Metals for analyses for this test program:
Barium
Chromium
Coppe r
Iron
Lead
Magnesium
Manganese
Nickel
Zinc
-35-
-------
6.0 QUALITY ASSURANCE
TRC's quality assurance program for source emission measurement is
designed so that the work is done by competent, experienced individuals using
properly calibrated equipment and approved procedures for sample collection,
recovery and analysis with proper documentation in various appendicies as
noted in the Table of Contents.
Specific details of TRC's quality assurance program for stationary air
pollution sources may be found in the Quality Assurance Handbook for Air
Pollution Measurement Systems, Volume III (EPA-600/4-7-027b).
At the beginning of each day, an organizational meeting was held to orient
personnel to the day's activities, to discuss results from the previous day,
and to determine if any special considerations are appropriate for the day's
work.
Method 5
TRC's measurement devices, pitot tubes, dry gas meters, thermocouples,
probes and nozzles are uniquely identified and calibrated with documented
procedures and acceptance criteria before and after each field effort.
Records of all calibration data are maintained in TRC files. Samples of these
calibration forms are presented in Appendix.
All Method 5 sampling was 100 ± 10 percent isokinetic. Filter outlet
temperatures were maintained at 150±10°F.
Clean-up evaluations were performed on each initial set of glassware prior
to collecting field samples.
The Method 5 sampling train with the glass fiber filter had a clean-up
sequence as follows:
Blank 1
Run 1
Blank 2
Run 2
. Blank 3
Run 3
Blank 4
-36-
-------
The Method 5 sampling train without the glass fiber filter had a clean-up
sequence as follows:
Blank 1
Run 1
Run 2
Run 3
Blank 2
All blank sample recovery was conducted identicaly to sample recovery
procedures outlined in Section 5 of this test plan.
Blanks of all solution used during the test program (HN03) Filter media
was collected and analyzed.
In summary, the evaluation tests shall be designed to precondition the
sample collectors, to establish blank background values, and to educate the
clean-up personnel in specific sample recovery procedures.
All sample recovery was performed by a one person clean-up crew.
Appropriate sample recovery data was recorded on the sample identification
log, sample handling log, chain of custody form, and analytical data forms as
presented in Appendix C.
Recovered samples were secured in padlocked, shock-proof, steel containers
for storage and shipment for analysis.
All preparation and analysis of Method 5 samples will be performed by
TRC. TRC will adhere to the standards of quality assurance as set forth in
Quality Assurance Handbook for Air Pollution Measurement Systems, Volume III
(EPA-600/4-7-027b) and the Handbook for Analytical Quality Control in Water
and Wastewater Laboratories. (EPA-600/4-79-019, March 1979).
Method 9
-37-
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