SEPA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
May 1987
Air
Chromium
Electroplaters
Test Report
Consolidated Engravers
Corp.
Charlotte, North Carolina
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February 4, 1988
FINAL REPORT
STACK TESTING FOR TOTAL CHROMIUM
AND HEXAVALENT CHROMIUM EMISSIONS
FROM CHROME PLATING TANKS
EPA Contract No. 68-02-4346
Work Assignment 01
Technical Directive 2
Test Site
Consolidated Engravers Corporation
Charlotte, North Carolina
Prepared for:
U.S. Environmental Protection Agency
Emission Measurement Branch
Research Triangle Park., North Carolina 27711
Prepared by:
PEER Consultants, P.C.
4134 Linden Avenue, Suite 202
Dayton, Ohio 45432
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TABLE OF CONTENTS
SECTION Page
1.0 INTRODUCTION 1
2.0 PROCESS 4
2.1 Process Description 4
2.2 A1r Pollution Control 5
2.3 Process Conditions During Testing 9
3.0 SUMMARY OF RESULTS 13
3.1 INTRODUCTION 13
3.2 HEXAVALENT AND TOTAL CHROMIUM EMISSIONS
RESULTS 13
3.3 CHROMIUM DISTRIBUTION 19
3.4 PROCESS SAMPLE ANALYSIS 23
3.5 WASHDOWN WATER ANALYSIS 23
4.0 SAMPLE LOCATIONS AND TEST METHODS USED 32
4.1 MIST ELIMINATOR INLET 32
4.2 MIST ELIMINATOR OUTLET 36
4.3 HEXAVALENT AND TOTAL CHROMIUM SAMPLE EXTRACTION
AND ANALYSIS 38
4.4 PROCESS SAMPLES 41
4.5 WASHDOWN WATER 41
5.0 PROJECT QUALITY ASSURANCE 42
REFERENCES 46
APPENDICES
A Process Monitoring Data A-l
B Analytical Methods for Total Chromium
and Hexavalent Chromium B-l
111
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APPENDICES Page
C Field Data Sheets C-l
D Calculations D-l
E Laboratory Results E-l
F Sampling, Sample Recovery and Analytical
Procedures F-l
G Equipment Calibration Data G-l
H Project Participants H-l
I Particle Size Sampling and Sample Recovery
Procedures 1-1
1v
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LIST OF TABLES
Number Page
2-1 Average Operating Conditions Recorded During Each
Emission Test Run 10
2-2 Total Current Supplied to the Plating Tanks During
Each Emission Test Run 12
3-1 Test Schedule for Cr+* and Cr Emissions at
Consolidated Engravers Corporation, Charlotte,
North Carolina 14
3-2 Summary of Sample and Flue Gas Conditions
(Consolidated Engravers Corporation, Charlotte,
North Carolina) 15
3-3 Summary of Cr+6 and Total Cr Emission Data
(Consolidated Engravers Charlotte, North Carolina) . 16
3-4 Summary for Cr+* and Total Cr Removal Efficiencies
at Consolidated Engravers Corporation, Charlotte,
North Carolina 20
3-5 Summary of Net Gains from Gravimetric Analysis
of Particle Samples ... 1 22
3-6 Summary of Total Net Chromium Gains
by Chemical Analysis 22
3-7 Summary of Inlet Distribution Data 25
3-8 Summary of Outlet Distribution Data 26
3-9 Summary of Results From the Laboratory Analysis of
of Plating Tank Solution 31
3-10 Summary of Results From Laboratory Analysis of
Hashdown Hater From the M1st Eliminator 31
4-1 Summary of Traverse Point Locations .... 35
5-1 Equipment Used 1n the MM 13B Sampling Program .... 44
5-2 Summary of Blank Analysis 45
5-3 Summary of Analytical Results From Duplicate
and Spiked Samples 45
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LIST OF FIGURES
Number Page
1-1 . Process Diagram 3
2-1 Diagram of Horizontal-flow Chevron-Blade M1st
Eliminator With a Single Set of Blades 6
2-2 Diagram of Capture and Control System for
Two Hard Chromium Plating Tanks Tested at
Consolidated Engravers 7
2-3 Diagram of Overlapping-type
Chevron-blade Design 8
3-1 Determination of Stage Outpoint Diameter 24
3-2 Graphical Presentation of Inlet Chromium
Distribution (Chemical Analysis) 27
3-3 Graphical Presentation of Inlet Chromium
Distribution (Gravimetric Analysis) 28
3-4 Graphical Presentation of Outlet Chromium
Distribution (Chemical Analysis) 29
3-5 Graphical Presentation of Outlet Chromium
Distribution (Gravimetric Analysis) 30
4-1 Flow Diagram for the Chromium Plating Tanks 1 and 2
at Consolidated Engravers Facility 33
4-2 Orthogonal Sketch of Inlet Sampling Location .... 34
4-3 Orthogonal Sketch of Outlet Sampling Location .... 37
vi
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SECTION 1.0
INTRODUCTION
The U.S. Environmental Protection Agency (EPA) 1s currently evaluating
whether air emissions of chromium and other potentially toxic metals should
be regulated. Chromium emissions are not Included 1n the New Source
Performance Standards (NSPS) for stationary sources or the National
Emissions Standards for Hazardous A1r Pollutants (NESHAP).
As part of this study, the EPA 1s evaluating uncontrolled emissions from
hard chromium plating operations. The purpose of these tests 1s to
characterize the emission rate and size distribution of uncontrolled
emissions of hexavalent chromium (Cr*6) and total chromium (Cr) from a
representative Industrial operation. Consolidated Engravers Corporation of
Charlotte, North Carolina, was the selected site at which these tests were
performed. The Consolidated Engravers facility was chosen because 1t 1s a
captive shop that performs hard chromium electroplating of Industrial
rolls. Based on operating parameters such as current, voltage, plating time
and chromic add concentration, the plating tank could be considered typical
of other hard chromium plating operations. The results from the
Consolidated Engravers Test Program will be used to characterize the
uncontrolled emissions from hard chrome plating operations and to revise or
confirm uncontrolled emission factors for this type of process developed
during another phase of the test program.
In an effort to obtain this data, tests were conducted at the Consolidated
Engravers Corporation, Charlotte, North Carolina, plant on May 11 through
15, 1987, under contract to the Emission Measurement Branch (EMB) of the
EPA's Environmental Standards and Engineering Division. Test team members
were PEER Consultants, P.C., located 1n Dayton, Ohio; Pacific Environmental
Services, Inc., (PES), located 1n Cincinnati, Ohio; and Midwest Research
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Institute (MRI) located 1n Raleigh, North Carolina. Triplicate tests using
the Modified Method 13B (MM 13B) sampling train and the Andersen 8-stage
Impactor were performed on the exhaust gas stream at the Inlet and outlet of
the mist eliminator servicing chromium plating Tanks 1 and 2.
Chromium emissions from both tanks are vented to a chevron-blade mist
eliminator that Is equipped with a single set of overlapping-type, chevron-
blade baffles and 1s Installed on the roof of the plant. Figure 1-1
represents a process diagram. The results of these tests were used to
determine Cr*6 and total Cr emissions. In addition to the emissions
sampling, samples were taken of the chromium plating solution from each
plating tank at Intervals during each emission sample run and analyzed for
Cr*6 and Cr.
The remainder of this report describes the process and Its operation 1n
Section 2.0; Section 3.0 presents a summary and discussion of results;
Section 4.0 describes the sampling locations and test methods while quality
assurance 1s discussed 1n Section 5.0. Appendix A presents process
monitoring data summary; Appendix B presents analytical methods for Total
Chromium and Hexavalent Chromium; Appendix C presents the field data sheets
for each test; Appendix D presents the calculations; Appendix E contains
laboratory and analytical results; Appendix F contains sampling, sample
recovery and analytical procedures; Appendix G contains equipment
calibration data; Appendix H presents a 11st of project participants and an
activities log and Appendix I contains particle size sampling and sample
recovery procedures.
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SECTION 2.0
PROCESS DESCRIPTION
2.1 PROCESS DESCRIPTION
The Consolidated Engravers plant located In Charlotte, North Carolina,
manufactures and refurbishes Industrial rolls for the packaging and textile
Industries. The plant operates six hard chromium plating tanks. Hard
chromium plate 1s applied to the Industrial rolls as the final, finishing
stage to provide a wear-resistant surface and protection from corrosion.
The facility tested consists of two hard chromium plating tanks that are
controlled by a chevron-blade mist eliminator with a single set of blades.
The tanks are operated from 8 to 10 hours per day, 5 days per week, 51 weeks
per year. The chromic add consumption for the two tanks 1s about 63
kilograms (140 pounds) per month.
Based on size; operating parameters such as current, voltage, and
plating time; and chromic add concentration of the plating bath, the tanks
are typical of other hard chromium plating tanks used 1n the electroplating
Industry. Tank 1 1s 1.52 meters (m) (5.0 feet [ft]) long, 0.7 m (2.3 ft)
wide, and 1.8 m (6.0 ft) deep and holds about 1,780 liters (ft) (470
gallons [gal]) of plating solution. Tank 2 1s 1.8 m (6.0 ft) long, 0.7 m
(2.5 ft) wide, and 1.8 m (6.0 ft) deep and holds about 2,350 ft (620 gal)
of plating solution. The chromic add concentration of the plating baths 1s
210 grams per liter (28 ounces per gallon) of solution. The normal
operating temperature of the plating baths ranges from 43°C (110°F)
to 54°C (130°F). Both tanks are equipped with a circulating water
cooling system.
Tank 1 contains two work stations each of which 1s equipped with a
3,000-ampere rectifier. Tank 2 1s equipped with one 5,000-ampere
rectifier. Typically, one Industrial roll 1s plated for about 45 minutes In
each tank; however, two Industrial rolls can be plated at a time 1n each
tank. The operating voltage and current for each roll typically ranges from
10 to 15 volts and 1,200 to 1,600 amperes, respectively. About 13
micrometers (0.5 mil) of chromium plate 1s applied to each roll plated.
4
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2.2 AIR POLLUTION CONTROL
The ventilation system and chevron-blade mist eliminator were
manufactured and Installed by Ouall Industries. Inc., 1n January 1987 to
control chromic add and emissions from the two hard chromium plating tanks
tested. A diagram of the capture and control system for the two tanks 1s
presented In Figure 2-1.
Both tanks are equipped with double-sided lateral exhaust hoods. The
hood on each side of Tank No. 1 has one slot that 1s 1.5 m (4.8 ft) long and
8.9 centimeters (cm) (3.5 C1n]) wide. The hood on each side of Tank 2 has
three slots. Each slot 1s 0.4 m (1.3 ft) long and 5.1 cm (2.0 1n.) wide.
Exhaust gases from both tanks are ducted together and vented to a
horizontal-flow chevron-blade mist eliminator. The mist eliminator contains
a single set of overlapping-type blades and 1s located on the roof of the
plating shop. Diagrams of the mist eliminator and overlapping-type blades
are presented 1n Figures 2-2 and 2-3, respectively. The overlapplng-type
blade design changes the direction of the gas flow four times, causing
chromic add droplets to Impinge on the blades by 1nert1al force. The
overlapping edges of the blades act as collection troughs that provide a
central location for droplet collection and facilitate drainage of the
droplets Into the collection sump at the bottom of the mist eliminator. The
blades are spaced about 3.20 cm (1.25 1n) apart. The blade section 1s 1.1 m
(3.6 ft) 1n height and width and 20 cm (8 in.) In depth.
Design parameters of the mist eliminator Include a gas flow rate of
226 standard cubic meters per minute (ma/m1n) (7980 standard cubic feet
per minute [fta/m1n]). gas stream velocity through the blade section of
about 190 meters per minute (m/m1n) (620 feet per minute [ft/m1n], and
pressure drop of 0.19 kllopascal (kPa) (0.75 Inch of water column
[1n. w.c.]). During emission testing, the gas flow rate averaged 154 actual
m*/m1n (5,450 actual ft8/m1n), the gas velocity was about 130 m/m1n
(425 ft/m1n), and the pressure drop averaged 0.05 kPa (0.20 1n. w.c.).
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ROOF
(f
II
MOISTURE
EXTRACTOR
MIST
ELIMINATOR
1)
II
ROOF
HOODS
LEGEND;
AIRFLOW t
WATERFLOW
HOODS
TANK NO. I
TANK NO. 2
Figure 2-1. Diagram of capture and control system for two hard chromium
plating tanks tested at Consolidated Engravers.
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Spray Nozzto
Wash Down
Gta Stream
». Controlled
Qas Stroam
Drain
Figure 2-2. Diagram of horizontal-flow chevron-blade mist eliminator
with a single set of blades.
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MIST-LADEN
GAS
STREAM
BLADES
(COLLECTION
TROUGH)
CONTROLLED
GAS
STREAM
DROPLETS TO COLLECTION SUMP
Figure 2-3. Diagram of overlapping-type chevron-blade design.
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A moisture extractor 1s Installed 1n the stack to control chromium
emissions that may be drawn through the mist eliminator. The mist
eliminator and moisture extractor are equipped with a spray washdown
system. The washdown water 1s drained Into a 340-ft. (90-gal) holding tank
and then Into the plating tanks to make up for plating solution evaporation
losses. The mist eliminator and moisture extractor are washed down one or
two times per day depending on the amount of plating solution makeup needed.
2.3 PROCESS CONDITIONS DURING TESTING
Three emission and three particle size distribution tests were conducted
at the Inlet and outlet of the mist eliminator to characterize uncontrolled
emissions and the performance of the mist eliminator. Inlet and outlet
testing was conducted simultaneously. The emission tests were conducted for
180 minutes each. The first particle size distribution test was conducted
for 190 m1n, the second test for 180 m1n, and the third test for 240 m1n.
Process operating parameters such as the voltage, current, and plating
solution temperature were monitored and recorded during each test.
Descriptions (dimensions and surface areas) and plating time of each
Individual roll plated also were recorded during each test. Process data
sheets documenting the process and control device operating parameters
during emission testing (test run Nos. 1-1 through 1-3 and 0-1 through 0-3)
and particle size distribution testing (PSI-1 through PSI-3 and PSO-1
through PSO-3) are presented 1n Appendix A. The average operating
conditions recorded during each emission test run are presented 1n Table 2-1.
Grab samples of the plating solution 1n each tank and the mist
eliminator washdown water were taken to determine the concentration of
chromic add 1n the plating baths and washdown water, respectively. Grab
samples of the plating solution 1n each tank were taken at the beginning.
middle, and end of each test run to obtain a composite sample for each
tank. The mist eliminator was washed down with about 230 ft (60 gal) of
water each morning before testing began. Grab samples of the mist
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TABLE 2-1. AVERAGE OPERATING CONDITIONS RECORDED DURING EACH
EMISSION TEST RUN
Test run No. Tank
Inlet/outlet No.
Temp, of
Work- Operating Operating plating
station voltage, current, solution.
No. volts amperes *C (°F)
1-1/0-1
1-2/0-2
1-3/0-3
1
1
2
1
1
2
1
1
2
1
2
1 and 2
1
2
1 and 2
1
2
1 and 2
15.5
13.0
10.0
15.5
13.0
9.8
12.6
11.4
9.8
1.600
1,250
2,050
1,460
1,270
2,210
1.265
1.250
2.170
68 (155)
68 (155)
55 (132)
62 (144)
62 (144)
58 (136)
67 (152)
67 (152)
55 (132)
10
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eliminator washdown water were taken from the holding tank after the mist
eliminator was washed down. The analytical results for each sample are
presented 1n Section 3.0 of this report.
Industrial rolls used 1n the textile and packaging Industries were
chromium plated during testing. Typically, the time required to plate one
roll 1n each work station ranged from 45 to 60 minutes. Dummy rolls were
plated during testing when the workload was Insufficient to operate the two
tanks at full capacity. Two dummy rolls were plated 1n Tank 1 during all of
run Nos. 1 and 3 and for 72 minutes of run No. 2, and one dummy roll was
plated In Tank 2 for 38 minutes of run No. 3. Two dummy rolls were plated
1n Tank 1 during all three particle size distribution tests.
During testing, the bath temperature of both plating tanks was somewhat
higher than normal. The temperature of Tank 1 ranged from 54°C (130°F) to
greater than 71°C (160°F), and the temperature of Tank 2 ranged from
50°C (122°F) to 64°) (148°F). The cooling systems for the tanks
were unable to maintain the normal operating temperatures when the tanks were
operated at full capacity. Although the bath temperatures were higher than
normal, the higher temperatures did not adversely affect the plating process.
The MM13B runs were shut down approximately 15 to 20 minutes to change
test ports. The first particle size distribution test (PSI-l/PSO-1) was
Interrupted for 12 minutes because of a low process workload and the second
and third particle size tests (PSI-2 and PSI-3/PSO-2 and PSO-3) were not
Interrupted.
The total amount of current supplied to the tanks during each emission
test run 1s calculated in ampere-hours and included in Appendix A. A tabular
summary of the total current values Is presented in Table 2-2.
11
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TABLE 2-2. TOTAL CURRENT SUPPLIED TO THE PLATING TANKS DURING EACH
EMISSION TEST RUN
Test run No.
Inlet/outlet
1-1/0-1
Tank No.
1
1
2
TOTAL
Work-
station No.
1
2
1 and 2
Total current,
ampere-hours
Inlet
4.829
3,724
6.471
15.024
Outlet
4.839
3,731
6.513
TtSsi
1-2/0-2
1
1
2
TOTAL
1
2
1 and 2
3,948
3.550
6.579
14,077
4,032
3.555
6.576
14,163
1-3/0-3
1
1
2
TOTAL
1
2
1 and
3,791
3.730
6.591
14,112
3,784
3,722
6.590
12
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SECTION 3.0
SUMMARY OF RESULTS
3.1 INTRODUCTION
Table 3-1 presents the testing schedule along with the sample and
analytical parameters. The samples collected from the triplicate MM 13B
tests performed at the Inlet and outlet of the mist eliminator, and the
plating solution samples from Tanks 1 and 2 were analyzed for Cr and
Cr*6. The size distribution samples were analyzed only for total Cr.
The Cr*' analysis was performed using the procedures outlined 1n
"Determination of Hexavalent Chromium Emissions From Stationary Sources."
This method 1s presented 1n Appendix B. The total Cr concentration was
determined by the Inductively Coupled Argon Plasmography (ICAP) Analytical
Procedures. This procedure 1s outlined 1n Method 3050 of the EPA manual,
SN-846 "Test Methods for Evaluating Solid Waste," and 1s also presented 1n
Appendix B of this report. The results of these analytical procedures are
presented 1n the remainder of this section.
3.2 HEXAVALENT AND TOTAL CHROMIUM EMISSIONS RESULTS
Table 3-2 summarizes pertinent sample and flue gas data for the chromium
tests, and Table 3-3 presents the Cr*6 and total Cr emissions results.
Sample volumes are expressed 1n dry normal cubic meters (dNm3) and dry
standard cubic feet (dscf) . Volumetric flow rates are corrected to
standard conditions (20°C and 760 mm Hg [68°F and 29.92 Inches Hg]
and zero percent moisture) and are expressed as dry normal cubic meters per
minute (dNm'/mln) and dry standard cubic feet per minute (dscfm).
Concentrations of Cr*' and total Cr are expressed 1n milligrams per
dry normal cubic meter (mg/dNm8) and grains per dry standard cubic foot
(gr/dscf).
13
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TABLE 3-1. TEST SCHEDULE FOR CR+6 and Cr EMISSIONS AT CONSOLIDATED
ENGRAVERS. CHARLOTTE. NORTH CAROLINA
Run No.
1-1
0-1
IPS-1
OPS-1
1-2
0-2
IPS-2
OPS-2
1-3
0-3
IPS-3
OPS-3
Samole Parameter
Date/Time Size
(1987) MM 13B Distribution
5/12
0952 -
5/12
0955 -
5/12
1427 -
5/12
1429 -
5/13
0925 -
5/13
0928 -
5/13
1327 -
5/13
1329 -
5/14
0845 -
5/14
0848 -
5/14
1232 -
5/14
1234 -
1309 X
1312 X
1749 X
1751 X
1245 X
1248 X
1657 X
1659 X
1200 X
1203 X
1632 X
1634 X
Analytical Parameter
Cr+6 Oiphenylcarbazide Total Cr Gravimetric
Colorimetric Method ICAP Analysis
X X
X X
X
X
X X
X X
X
X
X X
X X
X
X
X
X
X
X
X
X
14
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TABLE 3-2. SUMMARY OF SAMPLE AND FLUE GAS CONDITIONS (CONSOLIDATED ENGRAVERS CORPORATION, CHARLOTTE, NORTH CAROLINA)
Samel e Parameter
Run No.
1-1
1-2
1-3
0-1
0-2
0-3
IPS-1
IPS-2
IPS-3
OPS-1
OPS-2
OPS-3
Date
(1987)
5/12
5/13
5/14
5/12
5/13
5/14
5/12
5/13
5/14
5/12
5/13
5/14
Sample
Location
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Sample
dNM3
3.82
3.54
3.81
3.83
3.80
4.01
2.72
3.27
3.59
2.71
3.25
3.75
Volume
dscf
134.899
125.009
134.472
135.409
134.305
141.618
96.002
115.377
126.915
95.556
114.921
132.559
Percent
I sold ne tic
101.6
94.4
100.0
103.1
100.9
102.7
101.8
108.2
105.1
106.8
105.9
106.6
Volumetric
Flow Rate
dNnrVmin
143
142
145
142
144
149
•
•
«
•
*
*
dscf /ml n
5.038
5.026
5.105
5,028
5.095
5.277
•
*
•
*
•
•
Flue Gas Conditions
Temper-
ature
OF «c
81
79
73
84
83
76
*
*
*
*
*
•
27
26
23
29
28
24
Moisture
Content X
2.26
2.25
2.02
2.25
2.06
1.89
*
*
•
•
*
•
Static
Pressure
In. H20
-3.7
-4.1
-3.7
-0.39
-0.39
-0.39
*
•
•
*
•
*
This parameter not measured during size distribution run
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TABLE 3-3. SUMMARY OF Cr+* AND TOTAL CR EMISSION DATA (CONSOLIDATED ENGRAVERS, CHARLOTTE, NORTH CAROLINA)
Concentration
Run No.
1-1
1-2
1-3
Average
0-1
0-2
0-3
Average
Date
(1987)
5/12
5/13
5/14
5/12
5/13
5/14
Sample
Location
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Cr*
mg/dNm3
1.815
1.731
1.746
1.764
0.0885
0.2237
0.1346
0.1493
gr/dscf
0.00079
0.00075
0.00076
0.00077
0.00004
0.00010
0.00006
0.00007
Total
«g/dNm3
1.449
0.937
0.419
0.935
0.092
0.143
0.118
0.118
Cr
gr/dscf
0.00063
0.00041
0.00018
0.00041
0.00004
0.00006
0.00005
0.00005
Mass
Emission Rate
Cr+6
kg/h
0.0155
0.0148
0.0152
0.0152
0.0008
0.0019
0.0012
0.0013
Ib/h
0
0
0
0
0
0
0
0
.0342
.0326
.0333
.0333
.0017
.0042
.0026
.0028
Total Cr
kg/h
0.0124
0.0080
0.0036
0.0080
0.0008
0.0012
0.0011
0.0010
Ib/h
0.0273
0.0177
0.0080
0.0177
0.0017
0.0027
0.0023
0.0022
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Mass emissions rates are expressed 1n kilograms per hour (kg/hr) and pounds
per hour (Ib/hr). Each sample was recovered In a polyethylene bottle and the
sample consisted of the rlnseate from the nozzle and probe combined with the
1mp1nger solutions and the rlnseate from all connecting glassware.
As reported 1n Table 3-2, dry gas meter volumes were consistent and ranged
from 3.540 to 3.820 dNm3 (125.009 to 134.899 dscf) for the Inlet MM 13B
runs and 3.803 to 4.011 dNm1 (134.305 to 141.618 dscf) for the outlet
MM 13B runs. The 1sok1net1c variation ranged from 94.4 to 101.6 percent for
the Inlet and 100.9 to 103.1 percent for the outlet, all within the acceptable
range of 90 to 110 percent. The sample volume and 1sok1net1c variation for
the size distribution sampling 1s also summarized 1n this table. The field
data sheets for this sampling program are presented 1n Appendix C. The
calculations for the emission rates and size distribution data are presented
1n Appendix D.
3.2.1 M1st Eliminator Inlet
At the mist eliminator Inlet the average volumetric flowrate at standard
conditions was 143 dNm3/m1n (5056 dscfm). Flue gas temperatures ranged
from 23 to 27°C and averaged 25°C (73 to 81°F and averaged 78°F).
The moisture content of the gas stream averaged 2.18 percent for the Inlet.
The static pressure was checked during the collection of preliminary data
and recorded using a 0- to 10-1nch H 0 manometer during each test. The
static pressure was measured from the negative side of the pi tot tube and
measured 3.7 to 4.1 Inches H 0. Analysis of the gas stream composition
was not performed because by the nature of the process, 1t was emitting
essentially air. The molecular weight was .assigned a value of
29.0 Ib/lb-mole.
The Cr*' concentration of the gas stream at the Inlet to the mist
eliminator ranged from 1.731 to 1.815 mg/dNm* (0.00075 to 0.00079 gr/dscf) and
averaged 1.764 mg/ dNm8 (0.00077 gr/dscf) for the three tests. The
average mass emission rate for Cr+6 was 0.0152 kg/hr (0.0333) Ib/hr.
17
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The total Cr concentration ranged from 0.419 to 1.449 rag/dNm8 (0.00018 to
0.00063 gr/dscf) and averaged 0.935 mg/dNm3 (0.00041 gr/dscf). The
average mass emission rate for Cr was 0.0080 kg/hr (0.0177 Ib/hr).
The total mass of Cr*6 that was captured 1n the sample trains during
each test was 6.93 mg for Run 1-1, 6.13 mg for Run 1-2 and 6.65 mg for
Run 1-3. The mass of total Cr contained 1n the sample train for these runs
was 5.54 mg, 3.32 mg and 1.59 mg, respectively. Note that the Cr*6
concentration 1n the samples Is higher than the total Cr concentration. Due
to the fact that two different analytical methods were used. I.e.,
colorlmetrlc for Cr*6 and ICAP for total Cr, the analytical results are
slightly different. In Section 5.0 of this report 1t 1s demonstrated that the
percent recovery of Cr*6 1n the colorlmetrlc method exceeds that of the
ICAP method for total Cr. In that sense, the coloHmetry 1s more "accurate"
than ICAP. In any case, the data Indicate that the majority of Cr 1n these
samples 1s 1n the form of Cr*6. The calculation sheets for the Cr*6
and total chrome concentrations and emission rates are presented 1n
Appendix D.
3.2.2 M1st Eliminator Outlet
At the mist eliminator outlet, the average volumetric flow at standard
conditions was 145 dNm3/min (5133 dscfm). Flue gas temperatures ranged
from 24 to 29°C and averaged 27°C (76 to 84°F and averaged 81°F).
The static pressure was checked during collection of preliminary data and
recorded using a 0- to 10-1nch H 0 manometer during each test. The
static pressure was measured from the negative side of the pltot tube and
measured 9.91 mm of H20 (0.39 Inches of H20). The molecular weight
was assigned a value of 29.0 Ib/lb-mole, because the process was emitting
essentially air.
The Cr*6 content of the gas stream at the outlet to the mist elimin-
ator ranged from 0.09 to 0.22 mg/dNm8 (0.00004 to 0.00010 gr/dscf) and
averaged 0.15 mg/dNm3 (0.00007 gr/dscf) for the three tests. The
average mass emission rate for Cr*6 was 0.0028 Ib/hr. The total Cr
18
-------
concentration ranged from 0.092 to 0.143 mg/dNm3 (0.000040 to
0.000063 gr/dscf). The average mass emission rate for Cr was 0.0010 kg/hr
(0.0022 Ib/hr).
The total mass of Cr*6 that was captured 1n the sample trains during
each test was 0.339 mg (7.48 x 10~7 Ib) for Run 0-1, 0.851 mg
(18.80 x 10"7 Ib) for Run 0-2, and 0.544 mg (12.00 x 10"7 Ib) for Run
0-3. The mass of total Cr contained 1n the sample train for these runs was
0.352 mg (7.80 x 10~7 Ib), 0.546 mg (12.00 x 10~7) and 0.472 mg
(10.40 x 10~7 Ib), respectively. Note that the Cr*6 concentration 1n
the samples 1s higher than the total Cr concentration. Such apparent
discrepancies are due to the fact that two different analytical methods are
used, namely colorlmetrlc for Cr*6 and ICAP for total Cr. In Section 5.0
of this report 1t 1s demonstrated that the percent recovery of Cr*6 1n the
colorlmetrlc method exceeds that of the ICAP method for total Cr. In that
sense, the col crimetry 1s a more "accurate" method. The data Indicate that
the majority of Cr 1n these samples 1s 1n the form of Cr*6. Table 3-4
represents a summary of Cr*6 and total Cr removal efficiency of the mist
eliminator according to the results of this test.
3.3 CHROMIUM DISTRIBUTION
Triplicate chromium distribution measurements were made at the Inlet and
outlet location following each MM 13B run. The samples were collected using
the Andersen Mark III, 8-stage Impactor. The Impactor was modified such that
Stages 1, 4, 7 and backup were the first four stages. All remaining
Stages 0, 2, 3, 5 and 6 were assembled to follow these four in order to
provide for correct spacing within the Impactor unit. This procedures 1s
discussed 1n more detail 1n Section 4.3.2. These tests were designed to
characterize total Cr emissions by size fraction. The Cr distribution was
determined by gravimetric analysis of the filters and stage rinses with the
addition of the masses calculated from the chemical analysis of the filters
and stage rinses. To determine the average net gain on the filter stages, the
net gain from the cutpolnts were combined by stage for each sample location.
The stage rinses for each cutpolnt were combined, by stage, for each sample
19
-------
TABLE 3-4. SUMMARY FOR Cr+' AND TOTAL Cr REMOVAL EFFICIENCIES AT CONSOLIDATED
ENGRAVERS CORPORATION, CHARLOTTE, NORTH CAROLINA
Run Date Sample Cr*6 Emission Cr6 Removal Total Cr Emission Total Cr Removal
Nq. (1987) Location Rate (Ib/hr) Efficiency Rate (Ib/hr) Efficiency
1-1 5/12 Inlet 0.0342 95.OX 0.0273 93.4X
0-1 5/12 Outlet 0.0017 0.0017
1-2 5/13 Inlet 0.0326 87.IX 0.0177 84.7X
0-2 5/13 Outlet 0.0042 0.0027
1-3 5/14 Inlet 0.0333 92.2% 0.0080 71.3X
0-3 5/14 Outlet 0.0026 0.0023
Average 91.4X 83.IX
20
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location, and those samples were evaporated to determine the total weight gain
of each designated stage. The total gain was calculated by summing the
average net gain from the stage filter and the net gain of the respected stage
rinse evaporations. The data are presented 1n Table 3-5.
The stage filters from each of the three Inlet samples, were combined by
stage cutpolnt, digested and then analyzed for total chromium concentration
using the ICAP Method. Similarly, the stage rinses were combined and an
aliquot of each stage Hnse was also analyzed using the ICAP method. The
outlet samples were analyzed by the same technique. These data are presented
1n Table 3-6. The results from the filter analysis were reported 1n
milligrams. The results from the stage rinse analysis were reported 1n
mg/ft. The mass of total chromium 1n stage rinses was calculated by
multiplying the reported concentration (mg/fl,) by the sample volume
(liters). This calculation yielded the total milligrams collected 1n the
stage rinse. Hence, the mass of chromium from the filter analysis was added
to the mass of chromium 1n the stage rinse. This calculation yielded the
total mass of chromium collected In each stage cutpolnt.
It must be noted that the analytical results presented, both gravimetric
and chemical methods, do not Include the results from the analysis of the
nozzle rinse. These data are not presented because it 1s suspected that as
the gas stream enters the nozzle, chrome "particles" Immediately adhere to the
exposed Inside surfaces of the nozzle and the cone section of the Impactor.
There 1s no reason to suspect that such adhesion would be size dependent, so
1t was assumed that the size distribution of the particles captured at the
nozzle 1s the same as that passing Into the Impactor stages. The nozzle rinse
data are therefore not Included with the first stage so as to not bias the
size separation data. The gas stream that enters the subsequent sections of
the Impactor would be divided by size fraction and considered representative
of the Cr distribution 1n the full gas stream. For example, 1f 70 percent of
the chrome 1n the gas stream was collected 1n the nozzle and cone section, the
size distribution of the remaining 30 percent would be representative of the
distribution characteristics of the chrome 1n the gas stream as a whole.
21
-------
TABLE 3-5. SUMMARY OF NET GAINS FROM GRAVIMETRIC ANALYSIS
OF PARTICLE SIZE SAMPLES
Stage
INLET - RUNS 1
1*
4
7
Backup
OUTLET RUNS 1.
1*
4
7
Backup
Filter
Net Gain (rag)
. 2. 3
0.50
0.67
2.43
0.55
2. 3
-0.76
0.08
1.07
0.30
Stage Rinse
Net Gain (mg)
2.009
0.005
-0.016
0.012
-0.011
-0.007
-0.020
-0.045
Total Gain
(mg)
2.509
0.675
2.414
0.562
0
0.073
1.050
0.255
All reported values have been blank corrected
* Does not Include nozzle rinse
TABLE 3-6. SUMMARY OF NET CHROMIUM GAINS BY CHEMICAL ANALYSIS
Stage
INLET RUNS 1. 2. 3
1*
4
7
Backup
OUTLET RUNS 1. 2. 3
1*
4
7
Backup
Filter
(mg)
0.557
0.485
2.053
0.233
0.010
0.019
0.905
0.239
Stage Rinse
(mg)
0.030
0.021
NO
NO
NO
NO
NO
NO
Total mg
Of Chromium
0.587
0.506
2.053
0.233
0.010
0.019
0.905
0.239
Does not Include nozzle rinse
All reported values have been blank corrected
NO - Non-detectable
22
-------
The actual flow rate through the Impactor for Run IPS-1 was 0.5168 ACFM,
IPS-2 was 0.5547 ACFM, and IPS-3 was 0.5393 ACFM. The average flow rate was
0.5369 ACFM through the Inlet Impactor. The actual flow rate through the
Impactor for Run OPS-1 was 0.5413 ACFM, OPS-2 was 0.5572 ACFM and 0.5618 ACFM
for OPS-3. The average flowrate was 0.5534 ACFM through the outlet Impactor.
The stage cutpolnt diameter was determined using Figure 3-1.x A
summary of the distribution data for the Inlet 1s presented 1n Table 3-7.
This table presents the data generated from both analytical methods. The
outlet data are summarized similarly 1n Table 3-8. The results were plotted
on logarithmic probability paper with the particle diameter as the ordlnate
and the cumulative percent by weight as the abscissa. Figures 3-2 and 3-3 are
graphical presentations of the chromium distribution for the Inlet and
Figures 3-4 and 3-5 are are a graphical presentations of the particle size
chromium data for the outlet.
3.4 PROCESS SAMPLE ANALYSIS
Table 3-9 summarizes results for Cr+6 and total Cr from the plating
tank solutions collected during each test period. Plating tank solutions from
Tanks 1 and 2 were collected and composited 1n separate bottles for each
tank. The samples were taken at three equal Intervals during each of the
MM 13B and the size distribution tests. Results for both Cr+6 and total
Cr are expressed 1n milligrams per liter (mg/ft). Analytical procedures were
similar to those used for the actual emission samples with the Cr+6
determined by the dlphenylcarbazlde colorimetric method and total Cr by ICAP.
3.5 WASHDOWN HATER ANALYSIS
Table 3-10 summarizes the results for Cr+6 and Cr analysis of the
water used 1n the dally washdown of the mist eliminator. These samples were
collected prior to the beginning of testing every day when the trapped
emissions from the previous day were purged from the system. Results for both
Cr*6 and total Cr are expressed 1n milligrams per liter (mg/1).
Analytical procedures were similar to those used for the actual emission
samples with Cr+6 concentration determined by diphenylcarbazide
colorlmetrlc method and total Cr concentration by the ICAP method.
23
-------
«U ds a* &} oZai 10 ' \.o )A \o Lo io /*
Impactor 50% outpoint, air temp.= 70 F, particle density = 1.0 gm/cc
Figure 3-1. Determination of stage outpoint diameter.
-------
TABLE 3-7. SUMMARY OF INLET DISTRIBUTION DATA
GRAVIMETRIC ANALYSIS
Net Gain
(ma)
X of Total
Particles
Cumulative
1 Less Than
Effective Outpoint
Diameter (micron)
Stage 1*
Stage 4
Stage 7
Backup
INLET
2.509
0.675
2.414
0.562
Net Cr
(ma)
40.73
10.96
39.19
9.12
59.27
48.31
9.12
0
8.0
2.4
0.5
less than 0.5
CHEMICAL ANALYSIS
1 Of
Total Cr
Cumulative
X Less Than
Effective Cutpolnt
Diameter (micron)
Stage 1*
Stage 4
Stage 7
Backup
0.587
0.506
2.053
0.233
17.37
14.97
60.76
6.90
82.63 8.0
67.66 2.4
6.90 0.5
0 less than 0.5
Does not Include nozzle rinse
25
-------
TABLE 3-8. SUMMARY OF OUTLET DISTRIBUTION DATA
GRAVIMETRIC ANALYSIS
OUTLET
Net Gain
(ma)
1 of Total
Particles
Cumulative
X Less Than
Effective Outpoint
Diameter (micron)
Stage 1*
Stage 4
Stage 7
Backup
-0.771
0.073
1.050
0.255
0
5.29
76.21
18.49
100.00
94.71
18.50
0
less
7.90
2.35
0.49
than 0.49
OUTLET
CHEMICAL ANALYSIS
Stage 1*
Stage 4
Stage 7
Backup
Net Cr
(ma)
0.010
0.019
0.905
0.239
X of
Total Cr
0.85
1.62
77.15
20.38
Cumulative
X Less Than
99.15
97.50
20.38
0
Effective Cutpolnt
Diameter (micron)
7.90
2.35
0.49
less than 0.49
Does not Include nozzle rinse
26
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Company: Consolidated Engr.-Mist Elim.Inlet - Chemical Analysis
Application: Andersen Mark III, Modified 4-stage
Pwiidt-Sin Distribution Data:
Pwtid* Diamtttr
(Microns)
a.o
2.4
0.5
Percent In Size Range
17.37
14.97
60.76
Cumulative Pvrcant
•Less Than
82.63
67.66
6.90
»« •* uiii i*' u1
Cumulative Percent Less Than
Figure 3-2. Graphical presentation of inlet chromium distribution,
-------
Company: Consolidated Engr. - Mist Elim. Inlet - Gravimetric Analysis
Application:Andersen Mark III, Modified 4-stage
PtrtidrSite Distribution Data:
Ptrticto Diameter
(Microns)
8.0
2.4
0.5
Percent In Size Range
40.73
10.96
39.19
Cumulative Percent
Less Than
59.27
48.31
9.12
»« **» **i it t!» ' Itf
Cumulative Percent Less Than
Figure 3-3. Graphical presentation of inlet chromium distribution.
-------
Company: Consolidated Engr. - Mist Elim. Outlet - Chemical Analysis
Application: Andersen Mark III, Modified 4-stage
PvtidrSiM Distribution Ottt:
Awtidt Diameter
(Microns)
7.90
2.35
0.49
Percent In Size Range
0.85
1.62
77.15
Cumulative Percent
Less Than
99.15
97.50
20.38
1 1 1 1,11 W Wfi-U
»« MI Ui
Cumulative Percent Less Than
Figure 3-4. Graphical presentation of outlet chromium distribution
-------
Conwnv: Consolidated Engr. - Mist Elim. Outlet - Gravimetric Analysis
Application: Andersen Mark III, Modified 4-stage
Owtribution Data:
Panicto DiaflMttr
(Microns)
7.90
2.35
0.49
Percent In Size Range
0.0
5.29
76.21
Cumulative Percent
Leu Than
100.00
94.71
18.50
H !
-------
TABLE 3-9. SUMMARY OF RESULTS FROM THE LABORATORY ANALYSIS
OF PLATING TANK SOLUTIONS
Sample Cr+1 (ma/ft) Total Cr (ma/ft)
R.yn? J-l and 0-1
Tank 1
Tank 2
Runs 1-2 and 0-2
Tank 1
Tank 2
Runs 1-3 and 0-3
Tank 1
Tank 2
Runs IPS-1 and OPS-1
Tank 1
Tank 2
Runs IPS-2 and OPS-2
Tank 1
Tank 2
Runs IPS-3 and OPS-3
Tank 1
Tank 2
118,000
128.000
128,000
135,000
122,000
124,000
115,000
136,000
123,000
131,000
134,000
128,000
115,000
108,000
111,000
106,000
116,000
105.000
109,000
108,000
115,000
105,000
117.000
101 .000
TABLE 3-10. SUMMARY OF RESULTS FROM LABORATORY ANALYSIS
OF WASHDOWN HATER FROM THE MIST ELIMINATOR
Sample
Wash down 5/12
Nashdown 5/13
Nashdown 5/14
Total Cr (mg/ft)
108,000
58.400
54.800
Cr>6 (mg/fc)
93,300
61.600
62.700
31
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SECTION 4.0
SAMPLE LOCATIONS AND TEST METHODS USED
The test program consisted of simultaneous sampling of the Inlet to and
the outlet from the mist eliminator for plating Tanks 1 and 2. A flow
diagram for the hard chrome plating Tanks 1 and 2 at the Consolidated
Engravers facility 1s shown 1n Figure 4-1. The sampling location for the
chromium and size distribution tests are designated 1n Figure 4-1. Location
A designates the sample location on the Inlet to the mist eliminator and
Location B designates the sample location on the outlet from the mist
eliminator.
4.1 MIST ELIMINATOR INLET
Emission sampling was performed on the 19-5/8-Inch diameter duct using a
fUterless Method 13B Impinger train and a cascade Impactor. As presented
1n Figure 4-2, the location of one of the sample ports on the Inlet required
that a vertical traverse be made during the MM 13B tests. To accomplish
this, a sample box was modified to allow the sample probe to be connected
vertically and suspended above the port with a hoist, allowing the sample
train to be raised and lowered to reach all traverse points. The Inlet duct
had a straight run of 79-1/2 Inches. Two 3-1/2 Inch diameter sampling ports
were Installed on the Inlet duct. One sample port (0) was Installed on the
vertical axis and the second (K) was located 90 degrees from Sample Port J.
These ports were located 58 Inches (approximately 2.9 duct diameters)
downstream from the point where the exhaust ducts from Plating Tanks 1 and 2
join to a common duct. The Inlet sample ports were located 21-1/2 Inches
(1.1 duct diameter) upstream from the nearest disturbance. I.e., 90-degree
horizontal bend Into the mist eliminator.
Table 4-1 presents a summary of traverse point locations. The minimum
number of traverse points for the test was 24, as specified 1n EPA Reference
Method 1. The sample time per point was 7.5 minutes for a total test time
32
-------
ROOF
MOISTURE
EXTRACTOR
B
HIST
ELIMINATOR
U>
LEGEND
Gasflow - I
A - Inlet to mist
eliminator
B - Outlet from mist
eliminator
C - Washdown water
from mist
eliminator
D - Plating tank no.l
E - Plating tank no.2
I- A
D
II
ROOF
'HOODS
Figure 4-1
Flow diagram for the chromium plating Tanks 1 and 2
at the Consolidated Engraver's facility.
-------
Fan Moto
Stack Extension
OJ
*>.
Cross sectional location
of sample ports
Stack diameter
Mist
Eliminator
Port A
Port B
It
79.5"
Sample..^
port K
21.5"
Air Flow
\ Sample
port J
58"
Horizontal location of
sample ports
Figure 4-2. Orthogonal sketch of inlet sampling location.
-------
TABLE 4-1. SUMMARY OF TRAVERSE POINT LOCATIONS
Point No. Inlet Location (1n.) Outlet Location (1n.)
Stack Inner Diameter - 19.625 Inches
1
2 /
3
4
5
6
7
8
9
10
11
12
0.5
1.3
2.3 ,
3.5
4.9
7.0
12.6
14.7
16.1
17.3
18.3
19.2
0.5
1.3
2.3
3.5
4.9
7.0
12.6
14.7
16.1
17.3
18.3
19.2
of 180 minutes for each MM 13B on the Inlet. This sample time was based on
a similar sampling program conducted for the EMB. Traverse Point 1, as
calculated, was located close to the sample ports and Introduced the
possibility of ambient air entering the gas stream and diluting the sample.
To eliminate this problem Traverse Point 2 was sampled for 15 minutes to
complete the 24-po1nt traverse. The relocation of traverse points was
discussed and accepted by the EPA task manager. Particle size sampling was
also performed on the Inlet duct using an Andersen Mark III 8-stage Impactor
with a straight nozzle. The length of the three size distribution runs were
190, 210, and 240 minutes 1n duration following the chromium sampling. The
35
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length of the particle size run was based on previous testing conducted in a
similar test program 1n which the sampling team suspected that their
sampling times may have been Insufficient at 90 minutes.
4.2 MIST ELIMINATOR OUTLET
Figure 4-3 shows an orthogonal sketch of the outlet sampling location.
Emission sampling was performed on the 19.63-Inch diameter duct using a
fllterless Method 13B 1mp1nger train and a cascade Impactor. Prior to
sampling, the outlet duct was modified by removing the existing 30-1nch long
duct and the moisture extractor and replacing them with a 70-1nch long
extension from the transition duct. Since the moisture extractor was not
subject to evaluation, 1t was not connected to the 70-1nch extension.
Two 3.5-Inch diameter sampling ports were Installed on the modified
outlet duct at 50 Inches (2.5 duct diameters) downstream from the Induced-
draft fan and 20 Inches (1 duct diameter) upstream from the atmosphere. The
sample ports were configured on the horizontal axis, 90 degrees apart. A
total of 24 traverse points were required In sampling the outlet duct. The
sampling time per traverse point was 7.5 minutes for a total sampling time
of 180 minutes. The triplicate size distribution sampling runs were
180, 210 and 240 minutes in duration following the MM 13B runs.
Outlet testing was conducted simultaneously with Inlet testing. The
sampling protocol for the outlet was the same as that for the Inlet.
Traverse Point 1, as calculated, was located close to the sampling ports and
Introduced the possibility of ambient air entering the gas stream and
diluting the sample. To eliminate this problem, Traverse Point 2 was
sampled for 15 minutes to complete the 24-point traverse. The relocation of
traverse points was discussed and accepted by the EPA task manager.
36
-------
Cross sectional location
of sample ports
Mist
el uninator
Mist
Eliminator
Air
Flow
Port Port
20'
Vertical location
\— of sample ports
70"
Air
Flow
50'
Stack diameter
Transition
Duct
Fan
Fan
Motor
Roofto
Figure 4-3. Orthogonal sketch of outlet sampling location.
37
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4.3 HEXAVALENT AND TOTAL CHROMIUM SAMPLE EXTRACTION AND ANALYSIS
Prior to sampling, velocity, static pressure, moisture content, and
temperature were measured to define sampling rates and nozzle sizes as
described In the EPA Reference Methods 1, 2 and 4.2 The stack gas
molecular weight was not determined by EPA Method 3. Alternatively, the
molecular weight was assigned the value of 29.0 Ib/lb mole, as stated 1n the
EPA Method 2, paragraph 3.6. A "spot" check to verify the absence of
cyclonic flow at the Inlet and outlet was conducted. This check Indicated
acceptable flow patterns 1n the gas stream. The presence of cyclonic flow
was not suspected because prior tests with similarly configured control
equipment showed no cyclonic flow. Hence, sampling was performed by
conducting triplicate tests at the Inlet and outlet of the mist eliminator.
Samples were collected to determine the uncontrolled Cr+' and Cr
emissions from this source.
4.3.1 Modified Method 13B
An EPA MM 13B3 sample train was used to collect the Cr*6 and
total Cr samples. The sample train consisted of a 316-stainless steel,
button-hook design nozzle, an unheated Pyrex glass-lined probe, and a series
of 1mp1ngers. The first, third and fourth Implngers were of the Greenburg-
Smlth design, modified by replacing the tip with a 1/2-Inch Inside diameter
glass tube extending to 1/2-Inch from the bottom of the flask. The second
1mp1nger was a Greenburg-Smlth 1mp1nger with the standard tip. One hundred
m& of 0.1N NaOH was placed 1n each of the first, second and third
Implngers, and approximately 200 grams of silica gel was placed 1n the
fourth 1mp1nger. The balance of the sampling system consisted of a vacuum
pump, dry gas meter, calibrated orifice, and related temperature and
pressure Indicating apparatus with which to determine dry gas sample volume,
stack gas temperature, volumetric flow rate and 1sok1net1c sampling rates.
During sampling, stack gas temperature and the gas temperature exiting the
fourth 1mp1nger were monitored with thermocouples.
38
-------
The 1mp1ngers were weighed before and after each test to determine the
moisture content of the flue gas stream. These weights were recorded on
"Sample Recovery and Integrity Sheets." The sample recovery data 1s
contained 1n Appendix C. The contents of the 1mp1ngers were placed 1n a
polyethylene container. All connecting glassware, the nozzle and probe were
rinsed with 0.1 N NaOH and combined with the Impinger solution 1n the
polyethylene sample bottle. The liquid level was marked on each sample
bottle and the pH was checked with pH paper to verify that the pH was above
7.0. Appropriate blank solutions were collected in the field for submission
to the laboratory for analysis with the samples. The samples were trans-
ported to the laboratory where total volumes of each sample were measured.
The volume recovered from Run 1-1 was 899 m&, Run 1-2 was 502 mfl. and
844 mfl. was recovered from Run 1-3. The volume recovered from 0-1 was
360 ml. Run 0-2 was 887 mi and 555 ma was recovered from 0-3. Each
sample. Including blanks, was analyzed for Cr*6 and total Cr
concentrations using analytical methodology recently developed by the EPA.
A copy of the draft method entitled "Determination of Hexavalent Chromium
Emissions From Stationary Sources" 1s contained In Appendix B of this
report. This method entails the extraction of the sample with alkaline
solution, followed by the dlphenylcarbazlde colorlmetrlc method.4
At the completion of the Cr+6 analysis, a separate portion of each
sample was digested and analyzed for total Cr by use of ICAP analytical
techniques.5 Appendix B of this report contains the detailed analytical
methodology used for this analysis.
4.3.2 Size Distribution
Three size distribution runs were performed at the Inlet to and the
outlet from the mist eliminator. This data was used to determine the size
distribution of the total Cr emissions. All size distribution tests were
performed 1n accordance with procedures detailed 1n the equipment
manufacturer's operations manual, and through consultation with the
manufacturer.
39
-------
Samples for size distribution measurements were collected using an
Andersen Mark III 8-stage Impactor with glass-fiber filters as the substrate
media. This In-stack Impactor consisted of eight outpoint stages and backup
filter, the Impactor was reconfigured by using Stages 1, 4, 7 and the
backup with glass fiber substrates followed by Stages 2, 3, 5, 6 and 8 for
spacing purposes. The purpose of this technique was to reduce the number of
particle cutpolnts, thereby Increasing the mass of particles collected on
each stage. Validity of this procedure was discussed with and accepted by
the manufacturer of the Impactor as well as by the EPA task manager. The
sampled gas stream enters the system through the precutter. Particles with
sufficient Inertia are Impacted against the sides of the precutter. Smaller
particles flow with the gas stream, exit the precutter, and enter the main
Impactor. Then, particles with sufficient Inertia are Impacted on the front
of the zero stage plate (no filter), smaller particles pass through the
holes 1n the zero stage plate, and the portion of these particles with
sufficient Inertia Impacts on the zero stage filter. The remainder of the
particles pass through the holes 1n the first stage plate and similarly on
to each succeeding stage. Finally, a glass-fiber backup filter removes all
particles remaining 1n the gas stream downstream of the final, seventh stage
plate.
The modified Andersen Impactor was used to collect samples at a point of
average velocity and temperature, at both the Inlet and outlet sample
locations. Sampling times ranged from 190 to 240 minutes for the Inlet and
180 to 240 minutes for the outlet.
Isok1net1c sampling rates were set Initially, based on the average gas
velocity measured during the MM 13B runs. At the completion of each test,
the Impactor samples were recovered according to procedures described 1n
Appendix I.
Each recovered fraction was subjected to a gravimetric analysis using
procedures similar to those 1n the EPA Method 5. At the completion of the
gravimetric analysis, samples were combined by location and stage cutpolnt
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for analysis of total Cr. Analytical procedures followed those previously
described.
All particle size results are based on a particle density of
1 g/cm8. Moisture contents and gas molecular weights were obtained from
MM 13B Cr tests. Size distribution curves were established to represent the
total weight percent of particulate matter smaller than the Indicated
aerodynamic particle diameter 1n micrometers.
4.4 PROCESS SAMPLES
Grab samples were collected from each of the two chromium plating tanks
during the chromium test runs and during the particle size run. Sample
allquots were taken at three equal Intervals during each period of air
sampling, namely at the beginning, midpoint and the end of each three- hour
test. These samples were analyzed for Cr and Cr*6 concentrations.
4.5 WASHDOWN HATER
A grab sample of the mist eliminator washdown water was collected during
the morning following each sampling period. These samples were also
analyzed for total Cr and Cr*6.
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SECTION 5.0
PROJECT QUALITY ASSURANCE
The application of quality assurance procedures to source emission
measurement ensures accurate emission-testing results. Quality assurance
guidelines provide the detailed procedures and actions necessary for
defining and producing acceptable data. In this project, three documents
were used 1n the preparation of a site test plan that would ensure the
collection of acceptable data:
1. "Quality Assurance Handbook for A1r Pollution Measurement Systems,"
Volume III; Stationary Source-Specific Methods," EPA-600/4-77-027B;
2. PEI Laboratory Quality Assurance Plan;
3. Determination of Hexavalent Chromium Emissions From Stationary Sources,
December 13, 1984. (This method has recently been developed by the EPA.)
In this specific test program, which was reviewed by the EPA's Emission
Measurement Branch, the following steps were taken to ensure that the
testing and analytical procedures produced quality data:
On-s1te quality assurance checks, such as leak checks of the
sampling train and velocity measuring apparatus, detailed
Information on these checks 1s presented 1n Appendix C. On-site
quality .assurance checks were performed on all test equipment prior
to Its use.
Triplicate micrometer measurements of the sampling nozzle. These
measurements were recorded on the field data sheets (Appendix C).
Use of sampling equipment as designated 1n EPA Method 13B.
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Standard forms were used for recording the data .and for calculations
of data.
The sample recovery was performed in a warehouse located on site.
Isolated from contamination.
Collected samples were placed 1n polyethylene sample bottles.
Polyethylene bottles are recommended for storing and shipping of
corrosive materials.
Samples were secured upon completion of the sample recovery
activities. The samples and blanks were placed 1n a designated
space 1n the cleanup area. The area was locked when unattended.
For transportation, the samples and blanks were secured 1n boxes.
No special storage was required for these samples.
Samples were 1n the custody of PEER Consultants, P.C., at all times
until transfer to the analytical laboratory. When the samples were
transported to the laboratory the Sample Custodian acknowledged the
laboratory's receipt of the samples (Appendix C).
All glassware and sample bottles were rinsed with 10 percent nitric
add before use 1n the field.
External contaminated surfaces (probe, nozzle and pltot tube) were
rinsed with tap water prior to sample recovery. This was done to
eliminate the risk of sample contamination.
A polyethylene dipper was used to take samples of the chrome plating
solution.
While sampling, the ports were capped and the accessed port was
sealed with a rag to prevent the Introduction of ambient air Into
the duct.
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All field-sampling equipment was calibrated. The pretest and
post-test calibration data for the (equipment used 1n the field 1s
contained 1n Appendix G.
Duplicate and spiked samples were analyzed 1n the laboratory.
Table 5-1 11st the specific sampling equipment used to perform the
MM 13B sampling program. The calibration data for this equipment 1s
presented 1n detail 1n Appendix G.
TABLE 5-1. EQUIPMENT USED IN THE MM 13B SAMPLING PROGRAM
Equipment Identification
Meter Boxes RAC 1065, MB-4
Thermometers
- meter box RAC-1, RAC-2
- sample head SH-1, SH-2
P1tot Tubes S-l, S-3
Thermocouple 3-T-1A, 3T-2A
On-site calculations were made by the EPA Task Manager on the emissions
sampling data to determine the 1sok1net1c variation and moisture content of
the stack gas. All final calculations were done after the post-test
calibrations had been performed on the equipment following the return from
the field test. The final calculations are presented in Appendix D. The
following summarizes the quality assurance activities performed during the
analytical phase of this project.
Emission and process samples were analyzed in the same batches. Reagent
blanks that were set-up in the field were analyzed with the actual sample.
The blank results are presented in Table 5-2.
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TABLE 5-2. SUMMARY OF BLANK ANALYSES
Blank I.D. No.
Bl Run 1-1 & 0-1
B1 Run 1-2 & 0-2
Bl Run 1-2 & 0-2
Cr+« (mg/&)
Less than 0.009
Less than 0.009
Less than 0.009
Total Cr (ma/1)
0.011
0.011
0.013
In addition to the analysis of the submitted samples and blanks,
duplicate and spiked samples were analyzed. Table 5-3 summarizes the result
of these QA/QC checks.
TABLE 5-3. SUMMARY OF ANALYTICAL RESULTS FROM DUPLICATE
AND SPIKED SAMPLES
Sample I.D. No.
Washdown 5/13
Plating solution
Tank No. 1, 5/13/87
MM 138, Run 1-2
Washdown 5/13
Plating solution
Tank No, 1, 5/13/87
MM 13B, Run 1-2
Type of Sample
Cr+«
Duplicate
Duplicate
Duplicate
Total Cr
Duplicate
Duplicate
Duplicate
Results
(ma/a)
69,500
61,600
128,000
128.000
3.1
7.64
(mo/ft)
59,200
54,800
110,000
111,000
4.93
4.16
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REFERENCES
1. Andersen Samplers Inc., Mark III 8-Stage Cascade Impactor Operations
Manual, February 1984.
2. 40 CFR Part 60, Appendix A, EPA Reference Methods 1,2,4,
July 1986.
3 40 CFR part 60, Appendix A, EPA Reference Method 13. July 1987
4 "Test Methods for Evaluating Solid Haste." U.S. EPA SH-846, 2nd
Edition, July 1982. Method 3060
5 "Test Methods for Evaluating Solid Haste," U.S. EPA SH-846, 2nd
Edition, July 1982. Method 3050.
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