peer
FINAL REPORT
DETERMINATION OF TOTAL CHROMIUM
AND HEXAVALENT CHROMIUM EMISSION?
FROM CHROME PLATING TANKS
Candidate Plant
delco Products Division
General Motors Corporation
Livonia, Michigan
' Engineers • Scientists • Planners
consultants p.c.
Pollution, Environment, Energy and Resources
-------
EPA Report No.
September 1987
FINAL REPORT
pCTERMINATION OF TOTAL CHROMIUM
AND HEXAVALENT CHROMIUM EMISSION?
FROM CHROME PLATING TANKS
Candidate Plant
Delco Products Division
General Motors Corporation
Livonia, Michigan
by
Helen J. Owens
Joseph T. Swartzbaugh
PEER Consultants, P.C.
Dayton, Ohic 45432
and
Franklin Meadows
Pacific Environmental Services. Inc.
Cincinnati, Ohio 45246
and
Randy P. Strait
Midwest Research Institute
Raleigh, North Carolina 27612
EPA Contract No. 68-02-4346
Work Assignment 01
Technical Directive 1
Task Manager
Frank R. Clay
Emission Standards and Engineering Division
Office of Air Quality Planning and Standards
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
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TABLE OF CONTENTS
SECTION
Page
Tables v
Figures vi
1.0 INTRODUCTION 1-1
2.0 PROCESS AND OPERATIONS 2-1
2.2 Air Pollution Control 2-2
2.3 Process Conditions During Testing 2-2
3.0 SUMMARY OF RESULTS 3-1
3.1 Introduction 3-1
3.2 Hexavalent and Total Chromium Emissions
Results 3-2
3.3 Process Sample Analysis 3-4
4.0 SAMPLE LOCATIONS AND TEST METHODS USED 4-1
4.1 Location of Measurement Site 4-1
4.2 Hexavalent and Total Chromium Sample Extraction
and Analysis 4-4
4.3 Process Samples 4-8
5.0 PROJECT QUALITY ASSURANCE 5-1
References R-l
iii
-------
TABLE OF CONTENTS
SECTION Page
Appendices
A Field Data Sheets A-l
B Calculations B-l
C Laboratory Analytical Results C-l
D Determination of Cr+6 and Total Cr Emissions .... D-l
E Pretest Calibration Data E-2
F Project Participants and Activity Log F-l
G Analytical Methods for Determining Cr+6 and
Total Cr G-l
iv
-------
LIST OF TABLES
Number Page
2-1 Average Operating Conditions Recorded During Each
Emission Test Run 2-4
2-2 Total Current Consumed During Each Emission
Test Run 2-4
3-1 Test Schedule for Cr+6 and Cr Emissions
Testing at Delco Products, Livonia, Michigan .... 3-16
3-2 Summary of Sample and Flue Gas Conditions
(Delco Products - Livonia, Michigan) 3-3
3-3 Summary of Cr+6 and Total Cr Emission Data
(Delco Products - Livonia, Michigan) 3-3
3-4 Summary of Results from the Laboratory Analysis
of Plating Tank Solutions 3-5
4-1 Inside Dimensions of the Duct at Each Sample Port . . 4-4
4-2 Summary of Traverse Point Locations 4-5
5-1 Equipment Used in the MM 13B Sampling Program .... 5-3
5-2 Summary of Blank Analysis 5-4
5-3 Summary of Analytical Results from Duplicate and
Spiked Samples 5-4
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LIST OF FIGURES
Number Page
1-1 Process Diagram of Chrome Plating Tank on
Line No. 4 1-3
2-1 Schematic of Decorative Chromium Plating Tank
Tested on Line 4 at Delco Products Division,
General Motors Corporation, Livonia, Michigan . . . 2-3
4-1 Simplified Process Flow Diagram 4-2
4-2 Orthogonal Sketch of Inlet Sampling Location . . . 4-3
4-3 Cross-Section of Sample Location Indicating
Traverse Points 4-6
vi
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SECTION 1.0
INTRODUCTION
The U.S. Environmental Protection Agency (EPA) is currently evaluating
whether air emissions of chromium and other potentially toxic metals should
be regulated. Chromium emissions are not included in the New Source
Performance Standards (NSPS) for stationary sources or the National
Emissions Standards for Hazardous Air Pollutants (NESHAP).
As part of this study, the EPA is evaluating uncontrolled emissions from
decorative chromium plating operations. The purpose of these tests is 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. A production facility of the Delco
Products Division of General Motors Corporation located in Livonia,
Michigan, was the selected site at which these tests were performed. The
Delco facility was chosen because it is a large-size, captive shop that
performs decorative chromium electroplating. At this plant, decorative
chromium plate is applied to automobile bumpers. Based on operating
parameters such as current, voltage, plating time and chromic acid
concentration, the plating tank could be considered typical of other large
decorative chromium plating operations. The results from the Delco Products
Test Program will be used to characterize the uncontrolled emissions from
decorative chrome 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
Delco/Livonia plant on March 18 and 19, 1987, under contract to the Emission
Measurement Branch (EMB) of the EPA's Emission Standards and Engineering
Division. Test team members were PEER Consultants, P.C., located in Dayton,
Ohio; Pacific Environmental Services, Inc., (PES), located in Cincinnati,
Ohio; and Midwest Research Institute (MRI) located in Raleigh, North
1-1
-------
Carolina. Triplicate tests using the Modified Method 13B (MM 13B) sampling
train were performed on the exhaust gases from chromium plating Line No. 4.
Line No. 4 chrome plating tank is equipped with single-sided hoods on each
end and two double-sided hoods between each plating cell. The ventilation
hoods on the tank are connected to a common duct that leads to an
evaporator/scrubber. Figure 1-1 presents a process diagram. The results of
these tests were used to determine Cr+6 and total Cr emissions.
Particle size distribution measurements were to be taken at the site, but
these samples were unobtainable due to the length of the nipples on the
sample ports and the inside diameter of each port. Each nipple was
approximately 8 inches in length and the inside diameter of the sample port
was equal to the outside diameter of the impactor. Both of these factors
made it impossible to insert the cascade impactor into the stack. The
particle size data were to be collected using the Andersen Mark III,
eight-stage impactor with a straight nozzle. In addition to the emissions
sampling, samples were taken of the chromium plating solution from each cell
of the plating tank at intervals during each emission sample run and
analyzed for Cr+6 and total Cr.
Some minor modifications to the traverse point locations were required
because the duct walls were concave at the sample port location and because
the sample port nipples extended into the stack cross section. A detailed
discussion of the stack area and traverse point location is presented in
Section 4.0.
The remainder of this report describes the process and its operation in
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 is discussed in Section 5.0. Appendix A presents field data
sheets, Appendix B calculation sheets for each test, Appendix C laboratory
analytical results; Appendix D sampling and analytical procedures,
Appendix E equipment calibration sheets, Appendix F project participants and
activities log, Appendix G methods followed during the analysis of the
samples and Appendix H contains the process monitoring data.
1-2
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LINE 4 CHROMIUM
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Figure 1-1. Process
diagram of chrome plating tank on Line No. 4.
-------
SECTION 2.0
PROCESS OPERATION
2.1 PROCESS DESCRIPTION
The Livonia facility of Delco Products Division, General Motors
Corporation (Delco) is a large captive shop that performs decorative
chromium electroplating of automobile bumpers. The plating facility
consists of five decorative chromium plating lines, but only three lines
(Nos. 2, 4, and 5) are currently operated.
Each plating line consists of about 20 tanks containing various cleaning
and plating solutions. The lines are serviced by automatically controlled
overhead conveyors that transfer racks of up to 14 bumpers to each tank in a
programmed sequence. The chromium plating segment of each line consists of
a plating tank and several rinse tanks.
The chromium plating tank on Line No. 4 was tested to characterize
uncontrolled emissions. Based on size; operating parameters such as
current, voltage, and plating time; and chromic acid concentration, the tank
is typical of other large decorative chromium plating tanks used in the
electroplating industry. The chromium plating tank is 6.1 meters (m)
(20 ft) long, 3.65 m (12.0 ft) wide, and 2.75 m (9.0 ft) deep and is divided
into three cells that are each 2.0 m (6.7 ft) long. The tank holds
approximately 61,170 liters (16,160 gal) of plating solution, which contains
chromic acid in a concentration ranging from 250 to 375 grams/liter U)
(33 to 50 ounces/gal) of water. Sulfuric acid is used as a catalyst in a
chromic acid to sulfuric acid ratio of 180:1.
Line No. 4 is operated 16 hr/day, 5 days/wk. Typically, two or three
cells are operated at a time. One rack of bumpers is plated per cell for
about 2.25 minutes (min). Each bumper receives a chromium plate that is
2-1
-------
0.305 micrometer (0.012 mil) thick. Two separate transformer/rectifiers
charge the electrodes in each cell. For the first 15 seconds of plating,
the surface area of the bumpers is activated. During activation, each
rectifier is set at 5 to 6 volts (V) and 2,500 to 3,000 amperes (A). After
activation, the actual plating phase of the cycle begins. During plating,
each rectifier is set at 16 to 17 V and 8,500 to 10,000 A. The electrical
settings are determined by the required current density for a particular
rack of bumpers. Typical current densities range from 1,600 to
2,150 amperes per square meter (150 to 200 amperes per square foot) of
surface area.
2.2 AIR POLLUTION CONTROL
The chromium plating tank on Line No. 4 is equipped with single-sided
draft hoods on each end and double-sided draft hoods between each cell
(Figure 2-1). The hoods on the tank are connected to a common duct that
leads to an extensive evaporator/scrubber system. The total ventilation
rate is about 990 cubic meters per minute (35,000 cubic feet per minute).
2.3 PROCESS CONDITIONS DURING TESTING
Three test runs were conducted at the inlet of the evaporator/scrubber
to characterize the uncontrolled emissions from the decorative chromium
plating tank. The process was operated within normal limits during each
test run.
Process operating parameters such as voltage, current, and plating
solution temperature were monitored and recorded during each test run. The
number of plating cycles and the number of bumpers plated also were recorded
for each test run. Data sheets documenting process operating conditions and
the workload during each test run are presented in Appendix H. Average
values for the operating conditions recorded during each emission test run
are presented in Table 2-1.
2-2
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ro
i
CO
AIRFLOW LEGEND
LEGEND:
A = TEST PORT
B = GRAB SAMPLE LOCATION
PLATING TANK
2nd FLOOR
TO FAN
iC
n
- - - —
B
-»f
I
1
J
-
B
-»r
1
i
I
F
—
B
1 .
V
J
1
1
* V
y
1st FLOOR
EVAPORATOR/SCRUBBER
Figure 2-1. Schematic of decorative chromium plating tank tested on Line 4 at
Delco Products Division, General Motors Corporation, Livonia, Michigan.
-------
In addition, grab samples of the plating solution were taken from each
cell in the tank during the course of each test run to determine the chromic
acid concentration of the plating solution. The analytical results for each
sample are presented in Section 3.0 of this report.
Test Run No. 1 was interrupted for 13 minutes for electrical repairs on
the plating line. Test Run No. 2 was interrupted three times for 51, 3, and
11 min. The 3-minute interruption was caused by delays at the racking
station where bumpers were being mounted on the racks. The other two
interruptions occurred when the process was stopped for repairs. Test Run
No. 3 was interrupted three times for 3, 5, and 165 minutes. The
interruptions were a result of malfunctions with the overhead conveyor.
The total amount of current supplied to the tank during each test run is
calculated in terms of ampere-hours and is included in Appendix H. A
tabular summary of the total current values is presented in Table 2-2.
TABLE 2-1. AVERAGE OPERATING CONDITIONS RECORDED DURING
EACH EMISSION TEST RUN
Test
run No.
1
2
3
Bath
temperature,
°C (°F)
54 (130)
54 (130)
55 (131)
No. Of
cycles
138
139
120
Voltage,
volts
22.3
22.0
22.8
Current,
amperes
20,507
21,697
21,747
No. of
bumpers
1,043
1,143
984
TABLE 2-2. TOTAL CURRENT CONSUMED DURING
EACH EMISSION TEST RUN
Test Run No. Total current, ampere-hr
1 97,392
2 103,519
3 89,609
2-4
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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 emissions
tests performed at the inlet and the plating solution sampling from
Line No. 4 were analyzed for total Cr and Cr"1"6. Cr+6 analysis was
performed using the procedures outlined in "Determination of Hexavalent
Chromium Emissions From Stationary Sources." This method is presented in
Appendix G. Total Cr concentration was determined by the Inductively
Coupled Argon Plasmography (ICAP) Analytical Procedure. This procedure is
outlined in EPA Method 3050 of EPA document SW-846, and is also presented in
Appendix G. The results of these analytical procedures are presented in the
remainder of this section.
TABLE 3-1. TEST SCHEDULE FOR Cr+6 and Cr EMISSIONS TESTING
AT DELCO PRODUCTS, LIVONIA, MICHIGAN
Run
No.
1-1
1-2
1-3
Date
(1987)
3/18
3/19
3/19
Sample
Time MM
0934 to
1259
1437 to
1851
0945 to
1549
Parameters Analytical
13B
X
X
X
Cr+6
Diphenylcarbazide
Col ori metric Method
X
X
X
Parameters
Total Cr
ICAP
X
X
X
3-1
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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 in dry standard cubic feet (dscf) and dry
normal cubic meters (dNm3). Volumetric flow rates are corrected to
standard conditions (68°F and 29.92 inches Hg [20°C and 760 mm Hg]
and zero percent moisture) and are expressed as dry standard cubic feet per
minute (dscfm) and dry normal cubic meters per minute (dNm3/min).
Concentrations of Cr+6 and total Cr are expressed in grains per dry
standard cubic feet (gr/dscf) and milligrams per dry normal cubic meter
(mg/dNm3). Mass emissions rates are expressed in pounds per hour (Ib/h)
and kilograms per hour (kg/h). Each recovered sample consisted of the
rinseate from the nozzle and probe combined with the impinger solutions and
the rinseate from all connecting glassware. The sample was collected in a
polyethylene sample bottle.
As reported in Table 3-2 sample volumes were consistent and ranged from
151.110 to 155.638 dscf for the sample trains. The isokinetic variation
ranged from 98.0 to 98.5 percent which is within the acceptable range of
90 to 110 percent.
At the scrubber inlet, the average volumetric flow at standard
conditions was 23,000 dscfm (650 dNm3/min). Flue gas temperatures
ranged from 74 to 76°F and averaged 75°F (23 to 24°C and averaged
24°C). The moisture content of the gas stream averaged 0.92 percent
(based on the average of Runs 1-2 and 1-3). During the sample recovery of
Run 1-1, the final impinger weight was incorrectly recorded which resulted in
erroneous moisture data. Thus, the average moisture content (0.92 percent)
was used in the calculations for Run 1-1. The static pressure was checked
during the collection of preliminary data and recorded using a 0- to
10-inch H20 manometer during each test. The static pressure was measured
from the negative side of the pitot tube and measured 3.0 inches H20.
3-2
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TABLE 3-2. SUMMARY OF SAMPLE AND FLUE GAS CONDITIONS (DELCO PRODUCTS - LIVONIA, MICHIGAN)
U)
I
U)
Sample Parameter
Sampl e__ygT_ume _
Run No.
in. H20
1-1
1-2
1-3
Date
(1987)
3/18
3/18
3/19
Sample
Location
Inlet
Inlet
Inlet
TABLE 3-3.
Volumetric
Percent Flow Rate
dNM3
4.28
4.41
4.39
SUMMARY
dscf
151.110
155.638
155.156
OF Cr+6 AND
Isokinetic dNm3/min
98.0 641
98.5 656
98.3 656
dscf /mi n
22,633
23,183
23.161
Flue Gas Condition
Temper-
ature
oF oc
76 24
74 23
75 24
Moisture
Content %
0.92
1.03
0.82
Static
Pressure
-3.0
-3.0
-3.0
TOTAL CR EMISSION DATA (DELCO PRODUCTS - LIVONIA, MICHIGAN)
Concentration
Run No.
1-1
1-2
1-3
Date
(1987)
3/18
3/18
3/19
Sampl e
Location
Inlet
Inlet
Inlet
Cr+6
mg/dNm3 gr/dscf
1.95
1.30
1.54
0.00085
0.00056
0.00067
Total Cr
mg/dNm33 gr/dscf
1.66 0.00072
1.21 0.00053
1.45 0.00063
Mass
Cr+6
kg/h
0.08 0
0.05 0
0.06 0
Emission Rate
Ib/h
.17 0
.11 0
.13 0
Total Cr
kg/h Ib/h
\
.06 0.14
.05 0.10
.06 0.13
-------
Analysis of the gas stream composition was not performed because the process
was emitting essentially air. The molecular weight was assigned a value of
29.0 Ib/lb-mole.
The Cr+6 content of the gas stream at the inlet to the
evaporator/scrubber ranged from 5.6 x 10~4 to 8.5 x 10~4 gr/dscf
(1.30 to 1.95 mg/dNm3) and averaged 6.8 x 10~4 gr/dscf (1.60 mg/ dNm3)
for the three tests. The total Cr concentration ranged from 5.3 x 10~4 to
7.2 x 10~4 gr/dscf (1.21 to 1.66 mg/dNm3). '
rate for total Cr was 0.12 Ib/h (0.06 kg/h).
7.2 x 10~4 gr/dscf (1.21 to 1.66 mg/dNm3). The average mass emission
The total amount of Cr+6 that was captured in the sample trains during
each test was 8.37 mg for Run 1-1, 5.71 mg for Run 1-2 and 6.78 mg for Run
1-3. Total Cr contained in the sample train for these runs was
7.11 mg, 5.37 mg and 6.38 mg, respectively. Note that the Cr+s
concentration in the samples is reported to be higher than the total Cr
concentration. In Section 5.0 of this report it is demonstrated that the
percent recovery of Cr+fi in the colorimetric method exceeds that of the
ICAP method for total Cr. This difference in recovery rates can account for
such apparent discrepancies and the Cr+6 would appear to be the more
accurate result. In any case, the results indicate that the majority of
chromium in these samples is in the form of Cr+6. The calculation sheets
for the Cr+6 and total Cr concentrations and emission rates are presented
in Appendix B.
3.3 PROCESS SAMPLE ANALYSIS
Table 3-4 summarizes results for Cr+6 and total Cr from the plating
tank solutions collected during each test period. Plating tank solutions from
Line No. 4 chrome plating tank, cells 1, 2, and 3 were collected and
composited in different bottles for each cell. The samples were taken at
three equal intervals during each of the MM 13B tests. Results for both
Cr+6 and total Cr are expressed in milligrams per liter (mg/a).
Analytical procedures were similar to those used for the actual emission
3-4
-------
samples with the Cr+6 determined by the diphenylcarbazide colorimetric
method and total Cr by ICAP.
TABLE 3-4. SUMMARY OF RESULTS FROM THE LABORATORY ANALYSIS
PLATING TANK SOLUTIONS
Sample Total Cr (ma/fi.) Cr+6 (ma/fi.)
Run 1-1
Cell 1 153,000 150,000
Cell 2 147,000 160,000
Cell 3 157,000 153,000
Run 1-2
Cell 1 152,000 152,000
Cell 2 151,000 154,000
Cell 3 146,000 160,000
Run 1-3
Cell 1 151,000 158,000
Cell 2 151,000 158,000
Cell 3 138,000 160,000
3-5
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SECTION 4.0
SAMPLE LOCATIONS AND TEST METHODS USED
4.1 LOCATION OF MEASUREMENT SITE
Samples were extracted from the inlet to the evaporator/scrubber.
Figure 4-1 depicts a simplified process flow diagram and Figure 4-2 is an
orthogonal sketch of the inlet sample location. At the inlet to the
evaporator/scrubber, six sampling ports were identified (from left to right)
as ports A,B,C,D,E, and F.
The scrubber inlet measurement site (identified in Figure 4-1) was
located in a vertical rectangular duct having nominal dimensions of
24 x 96 inches. The six 3-inch I.D. sample ports were located at equal
distances along the 96-inch side. Upon measurement of the stack's inside
dimension, it was discovered that all six sample ports extended into the
stack cross-sectional area for 3.5 inches past the inside wall. A visual
inspection of the ductwork also revealed that the duct was partially
collapsed along the front and back sides. Measurement of the duct inside
dimensions through each of the six ports resulted in six different values.
These are summarized in Table 4-1. The inside width was 95.8 inches. Using
stack dimensions of 20.7 x 95.8 inches the gross area of the duct cross-
section at the measurement site was 1983 square inches. In order to compute
the net cross-sectional area it was necessary to correct for the area of the
nipples which extended into the duct. All nipples were 3.5 inches outside
diameter and extended 3.5 inches into the duct cross-sectional area. The
total blockage was 73.5 square inches (3.5 x 3.5 x 6). Thus, the net area
of the duct was 1910 square inches. The equivalent stack dimensions were
19.9 x 95.8 inches for an equivalent inside diameter of 33.0 inches.
4-1
-------
LINE 4 CHROMIUM
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2nd FLOOR
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LOCATION OF SAMPLING PORTS
i
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1st FLOOR
EVAPORATOR/SCRUBBER
Figure 4-1. Simplified process flow diagram.
-------
96"
24'
D
location ** outline
Transition duct
72.5"
8" , 16"
—/ A
>ctio
)
n of Flow
y
3.0" (ID)
D MEM (E J
4 3/8 "
T£
44.5' ,
^
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Side view showing the distance i
port configuration
Direction of
Flow
3.5'
ran tne nearest downstream disturbance and the
HTs^
Figure 4-2. Orthocfonal sketches of inlet sampling location.
4-3
-------
TABLE 4-1. INSIDE DIMENSIONS OF THE DUCT
AT EACH SAMPLE PORT
Port
A
B
C
D
E
F
Average
Inside Depth
(Inches)*
22.4
19.9
19.4
19.5
20.0
22.8
20.7
* Does not include 3.5-inch nipple protrusion
into the duct.
The measurement side was located 72.5 inches (2.2 duct diameters)
downstream of a duct transition and 44.5 inches (1.3 duct diameters)
upstream of an elbow. According to EPA Method 1 criteria, this location
required 30 sample traverse points using a 6 x 5 matrix. Three sets of
sample traverse dimensions were used. Measurements of the distance across
the duct from each sample port indicated that the measurements through ports
A and F were nearly identical, B and E were nearly identical, and C and
D were nearly identical. Thus, three sets of sample traverse points were
used. Due to the protrusion of the sample port nipples into the duct, the
first traverse point was relocated to 1.0 inch past the end of each nipple.
The resultant sample traverse point locations are summarized in Table 4-2,
and a cross section of the inlet showing the traverse points is presented in
Figure 4-3. The figure is exaggerated but demonstrates the methodology
applied in locating the traverse points. This alternative method of
locating the traverse points was discussed and approved by the EPA Task
Manager. Each point was isokinetically sampled for 6.0 minutes to acquire a
total test time of 180 minutes.
4.2 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. The stack gas
4-4
-------
TABLE 4-2. SUMMARY OF SAMPLE TRAVERSE POINT LOCATIONS
Traverse Inside of Nipple Depth Traverse Point
Point Near Wall to Inside Location From
No. Traverse Point of Near Wall Outside of Nicole
Ports A & F (averaae diameter =
1
2
3
4
5
Ports B & E
1
2
3
4
5
Ports C & D
1
2
3
4
5
2.26 (4.5)
6.78
11.30
15.82
20.34
(average diameter
2.00 (4.5)
6.00
10.00
14.00
18.00
(average diameter
1.95 (4.5)
5.85
9.75
13.65
17.55
22.6 inches)
4.375
4.375
4.375
4.375
4.375
= 20.0 inches)
4.375
4.375
4.375
4.375
4.375
= 19.5 inches)
4.375
4.375
4.375
4.375
4.375
6.6 (9.0)
11.2
15.7
20.2
24.7
6.4 (9.0)
10.4
14.4
18.4
22.4
6.3 (9.0)
10.2
14.1
18.0
21.9
4-5
-------
22.4"
22.8"
Figure 4-3. Cross-section of sample location indicating traverse points.
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molecular weight was not determined by procedures outlined in EPA Method 3.
Alternatively, the molecular weight was assigned the value of 29.0 Ib/lb
mole, as stated in the EPA Method 2, paragraph 3.6. In addition,
verification of the absence of cyclonic flow at each sample traverse point
was assessed based on procedures described in the EPA Reference Method 1.
In this method, the face openings of the Type-S pi tot tube are aligned
perpendicular to the duct cross-sectional plane, designated "0-degree
reference." Null (zero) pi tot readings obtained at 0-degree reference
indicate an acceptable flow condition at a given point.
If the pitot reading was not zero at 0-degree reference, the pi tot was
rotated until a null reading was obtained. The value of the rotation angle
(yaw) was recorded for each point and averaged across the duct. Method 1
criteria stipulate that average angular rotations greater than 20 degrees
indicate cyclonic (nonaxial) flow conditions in the duct. The average of
the angular rotations was 7.8 degrees, which indicated acceptable flow
patterns and enabled the extraction of representative samples from this
source. The cyclonic flow data is contained in Appendix A. Following this,
sampling was performed by conducting triplicate tests at the inlet to the
evaporator/scrubber. Samples were collected to determine the uncontrolled
Cr+s and total Cr emissions from this source.
An EPA MM 13B2 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 impingers. The first, third and fourth impingers were Greenburg-Smith
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
impinger was a Greenburg-Smith impinger with the standard tip. In the
first, second and third impinger 100 mfi, of 0.1N NaOH was placed, and
approximately 200 grams of silica gel was placed in the fourth impinger.
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
4-7
-------
temperature, volumetric flow rate and isokinetic sampling rates. During
sampling, stack gas temperature and the gas temperature exiting the fourth
impinger were monitored with thermocouples.
The impingers were weighed before and after each test to determine the
moisture content of the flue gas stream. The contents of the impingers were
placed in a polyethylene container. All connecting glassware, the nozzle
and probe were rinsed with 0.1 N NaOH and combined with the impinger
solution in 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 transported to the laboratory where total volumes of each sample were
measured. The volume recovered from Run 1-1 was 698 mfi., Run 1-2 was
770 mfl- and 672 mft was recovered from Run 1-3. Each sample, including
blanks, was analyzed for Cr+6 concentrations using analytical
methodology recently developed by the EPA. A copy of the draft method
entitled "Determination of Hexavalent Chromium Emissions From Stationary
Sources" is contained in Appendix G of this report. This method entails the
extraction of the sample with alkaline solution, followed by the
3
diphenylcarbazide colorimetric method.
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
4
techniques. Appendix G of this report contains the detailed analytical
methodology used for this analysis.
4.3 PROCESS SAMPLES
Process samples (plating tank solutions) were collected by PEER
personnel during each test period. A sample from each cell of the chromium
plating tank was collected and composited at three equal intervals during
the 3-hour test period and placed in corresponding polyethylene containers.
These samples were analyzed for Cr+6 and total Cr following procedures
similar to those used for the emission samples.
4-8
-------
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 in the preparation of a source-specific test plan that would
ensure the collection of acceptable data:
1. Quality Assurance Handbook for Air 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-site quality assurance checks, such as leak checks of the sampling
train and pi tot tube, detailed information on these checks is presented
in Appendix A. 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 A).
Use of sampling equipment as designated in EPA Method 13B.
5-1
-------
Standard forms were used for recording data and in calculating air flow
results.
The sample recovery was performed in the plant in an area isolated from
contamination, and in the van.
Samples were collected in 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 in a designated area in the clean-up
van. The van was locked when unattended. For transportation, the
samples and blanks were secured in a cooler. No special storage was
required for these samples.
Samples were in the custody of PEER Consultants, P.C., at all times.
When the samples were transported to the laboratory, the Sample
Custodian acknowledged the laboratory's receipt of the samples (Appendix A).
All glassware and sample bottles were rinsed with 10 percent nitric acid
before use in the field.
Prior to sampling, the ports were cleaned to minimize the possibility of
contamination of the sample train when inserting or removing the probe.
External contaminated surfaces (probe, nozzle and pitot tube) were rinsed
prior to sample recovery. This would 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 room air into the duct.
5-2
-------
All field-sampling equipment was calibrated. The pretest and post-test
calibration data for the equipment used In the field Is contained in
Appendix E.
Duplicate and spiked samples were analyzed in the laboratory, the
results of which are presented below.
Table 5-1 list the specific sampling equipment used to perform the MM
13B sampling program. The calibration data for this equipment is presented
in detail in Appendix E.
TABLE 5-1. EQUIPMENT USED IN THE MM 13B
SAMPLING PROGRAM
Equipment Identification
Meter Box RAC 1065
Thermometers
- meter box RAC-1
- sample head SH-1
Pi tot Tubes S-l, S-2
Thermocouple 3-T-1A
On-site calculations were made by the EPA Task Manager on the emissions
sampling data to determine the isokinetic 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 B. The
following summarizes the quality assurance activities performed during the
analytical phase of this project.
5-3
-------
Emission and process samples were analyzed In the same batches. The
linear regression data of the spectrophotometer calibration for these
samples is presented in Appendix C. Standards containing 0, 5, 10, 15,
20 and 25 >ig of Cr+6 per 50 mfl. were analyzed with the samples. The
ICAP was calibrated prior to the total Cr analysis. This calibration data
is presented in Appendix C. Reagent blanks that were set-up in the field
were analyzed with the actual sample. The blank results are presented in
Table 5-2.
In addition to the analysis of the submitted samples and blanks,
duplicate and spiked samples were analyzed. Table 5-3 summarizes the
results of these QA/QC checks.
TABLE 5-2. SUMMARY OF BLANK ANALYSIS
Blank I.D. No.
Bl.Run 1-1
Bl.Run 1-2
Bl.Run 1-3
Cr+6 (mg/H)
less than 0.02
less than 0.02
less than 0.02
Total Cr (ma/2,)
0.011
0.011
0.013
TABLE 5-3. SUMMARY OF ANALYTICAL RESULTS FROM DUPLICATE
AND SPIKED SAMPLES
Sample I.D. No.
Run 1-2, tank 2
Run 1-1, emission
Run 1-3, tank 1
Run 1-2, emission
Type of Sample
duplicate
spiked
Total Cr
duplicate
spiked
Results
154,000 mg/ft.
155,000 mg/ft,
98.5% recovery
153,000 mg/fi.
149,000 mg/fi,
89.3% recovery
5-4
-------
REFERENCES
R-l
-------
REFERENCES
1. 40 CFR Part 60, Appendix A, EPA Reference Methods 1,2,4, July 1986.
2 40 CFR part 60, Appendix A, EPA Reference Method 13, July 1987.
3 "Test Methods for Evaluating Solid Waste," U.S. EPA SW-846, 2nd Edition,
July 1982, Method 3060.
4 "Test Methods for Evaluating Solid Waste," U.S. EPA SW-846, 2nd Edition,
July 1982, Method 3050.
R-2
-------
APPENDIX A
Field Data Sheets
A-l
-------
TRAVERSE POINT LOCATIONS FOR RECTANGULAR DUCTS
T24—
« •/ •« _ ,
— fZ. - f=^
PLANT
DATE .
L>tLL<-O
3.0.
U<
/N
SAMPLING LOCATION
INSIDE STACK DIMENSIONS
INSIDE OF NEAR WALL TO
OUTSIDE OF NIPPLE. (Distinct 8}
EQUIVALENT STACK 1.0
NEAREST UPSTREAM DISTURBANCE
NEAREST DOWNSTREAM DISTURBANCE _
NUMBER OF TRAVERSE POINTS ARRAY
CALCULATOR
<~
ILLUSTRATE
PORT LOCATIONS
AND
STACK DIMENSIONS
J_
INCREMENT
DIMENSIONS
h
TRAVERSE
POINT
NUMBER
INSIDE OF NEAR
WALL TO TRAVERSE
POINT
(Distance A)
DISTANCE B
TRAVERSE POINT LOCATION
FROM OUTSIDE OF NIPPLE
(SUM OF DISTANCES A+B)
PORT
LOCATION
DISTANCE
FROM
EDGE OF STACK
A
A-2
PACIFIC FNV1Rnv»'cvTfl- fffM'f^f 'V-
-------
PRELIMINAR}
Plant: P£i_£0 P/ZoPo£7"_s
Date: 3-/fc-f
Location:
"'Stack 1.0
£>c (in e>,2,(3l jTUi_£T
•'• Otiifr X £]£. X
Barometric Pressure, in. Hg:
Stack Gauge Pressure, in. H2
Operators : fft\ £7t D/JJXJ>- H flu
0*1^ (4(3
0: — 3,O
jexis
Pilot Tube I.D. Number: S-3-
Temperature Readout I.D.: 0me&A C^S*?
Pi tot Tube Leak Check: c»L.
u/u*s.r ^ c^
Traverse
Point
Number
yf-/
^
3
V
JT
6 - '
JL
3
V
r
£ - '
a
3
^
^
Average
Velocity
Head (Aps)
in. H-jO
o.&
0, 3^
0. *£(*
0,23-
0-W
6- n
O. £6
o.aa.
^. /^
(?. ^>
a.oe
o< /a
i7, ;«Y
o, n
0,23
^J«0£j
Stack
Temp.
73
73
-7*
73
7-5
7f
7/
7/
7^
7P-
4^9
C'l
^^
-,/
-7/
Cyclonic
Flow Check
• from Null
13°
12"
r>
k* fifVlli)
5e-
Clock t?u
•
t Q Q
1 F)
IS
. e
iS-docku.
N'fttefa.
/7£
4'
S-^orJoLi',
(D MtffAltiiift
// (JcCJtlLi*?
VELOCITY TRAVERSE
O
Schematic of Trav<
Traverse
Point
Number
P- /
}
3
v
G
0. 3$ '
0.3/
0,£0
0.^^
0,77
O.(,3-
O.SZ
\
Sampling,^ O 4-
Location T
t
srse Point Layout
Stack
Temp.
7o
70
If
7(
7^
~7d
7f
12>
-73-
73
-79-
73
-73
13
73
Cyclonic
Flow Check «
• fron Null
7"
In'tiirtu*
3*
3<
Cjo
lO'CLK****
lo'eLoirjAyA
3°
Q°
ly
l^'tLotkL&i
Z'cLcc&o-*
0°
5°
o
"7,£ °
PAL SERVICES INC
<*_
p
c
-------
NOMOGRAPH DATA
Plant: Dd.Cc
Date: 3-/J-
Sampling Location: 2»c
\
Calibrated Pressure Differential Acros^
Orifice, in. H2O
Average Meter Temperature (ambient + 20°F),
•f
Percent Moisture in Gas Stream by Volume
Ear one trie Pressure at Meter, in. Hg.
Static Pressure in Stack, in. Hg.
(Pm _+ 0.073 x stack gauge pressure in in. H2O)
Ratio of Static Pressure to Meter Pressure
Average Stack Temperature, °F
c
Average Velocity Head, in. H2O
Maximum Velocity Head, in. R2O
C Factor
Calculated Nozzle Diameter, in.
Actual Nozzle Diameter, in.
Reference Ap, in. H2O
^
avg
BWO
Pm
PS
*%.-
8 avg
*Pavg
apmax
/J *
O.J6^
' o,r
,H
/oo
/. -r
^,s^
*i.*
o.w
74,
0,*
M3
^r •
A-4
PAafTC ENVIRONMENTAL SERVICES. INC. •
-------
I
c
s
£
F
C
A
E
S
E
i
F
. i
F
g
2
n
T
Tl
E
1
1 >
Tl 1
z i-n
2
-
CA
n
5
n
/>
E
1
>lant |>£t_Co P/t<5t>u.c7"S -Mi/0*^i/t-
)ate J -j£ -/ 7
ampllng L
ample Typ
un Number
Operator j
location 5c£Mtf/}cv7 tx/cCT"
e ^yt d o , i^ft
P"- KHET/VOO**.> - rt, fl^oJ^
jnbient Temperature If0^
a rone trie Pressure A^, S"O "/<*
tatlc Pressure (P.) - 3, o " ^i °
'liter Number (•) A^/A
•re test Leak Rate « ,00 » cfm I y&> in. Hg
re test Pi tot Leak Check Qit
're test Orsat Leak Check *-*/A
lead and Record all Data Every ^ Minutes
P/\^f~ 1 OF 3-
Traverae
Point
Number
A- 1
a.
}
V
5-
6- /
A
J .
i/
f
C- 1
%
J
«/
^~
/Clock
Sampling / Tlma
Time, /(24-hour
(min) / clock)
o / o^y^
(f / 0*1*^0
/*• / Q^Hfa
If" / O^S?-
jy / 0 qs'fr
J <.•> / / b O t-t
/too?
3(r / iO 1 LJ
HZ / IDiLO
Wfr tlb*(f
5^4 / 10 32.
la 0 /ItoZK
UQt-10
(0(4 //OL{(O
7 3L- //Q£"d*
19 IIOSl
4
A i/ ^ ^ C"T
?(C"^J ^7 1 H '
T' * A ^' '
ffl^&
«wk
£-7) fioV
£15X10
%Q>0;uo(t
ZZ'+tSX
%(f<\ ttj()i
FIELD DATA
Probe 1
UllULt C At,l&t nfteiJ Pi tot 1
(£) , }aJ Nozzle
g? > *o f Assumed
(f) • *gj. Temp. P
/V<- • 2o3 Meter B
Meter A
C Facto
Meter G
Heater
Referen
Post Te
U//*
1 c-
st Leak Rate -,O6>
Schematic of Post Test PI tot Leak Chec
Traverse Point Layout Post Test Orsat Leak Chec
TC
3-T-lrt
Ve loci ty
Head (APfl)
in. H30
Oi y^f
d i So
0> 2 3
CJi / ^
O i At-
6r4ltftfax
a. J3-
^7. 59
a /f
0. /
7
O.-2.0
A 4137' '
c>, /o
^, /?-
<7. /.T
^?i <
1
*,a^
/>•. ^s3^
Orifice Pres,
Differential
(AH), in. H70
Desired
75 o?
lot
101+
lot
1 0(f
1 0?
/^96
/ 07
7/2*?
i//
///
/ot,£
Temp.
Outlet
"out
7V
"7 6>
7F
fro
g-j
7fii3
%s
f
(pi
-------
l ;
, Plant Name i PCLCO P&OPacrJ - Ll
I
L/OO//V
Run Numbert
Test Datei
Operator!
Page
ot
Traverse
Point
Number
D- 1
c-
I=-L
/Clock
Sampling / Time
Tim^, /(24-hour
(min) / clock)
/ no-
/ (
/OA / //
/ M 3o
/ U
^v
120
Gaa Meter
Reading.
(v) ft3
W3>
OSO
VOC/
Velocity
Head (APS)
In. II .O
o.n
o.u*
0.V7
0,
0,2
AP
Orifice Pres.
Differential
(AH) in. H20
Desired Actual
/.so
£,*>
i.ts
2,02-
SO
v
J.7-70
Stack
Temp.
(Tg)
«F
n
17
77'
19
7^7
-79
Dry Gas Meter Temp.
Inlet
/M
Avt,,
Outlet
(Tm ) »
"out
93
3±L
99
/OO
Pump
Vacuum
in. llg
-
.2-
Sample
Box Temp.
Filtejr
Temp. *F
-# Te»r
nsf f2£>rKtz.-nst>
i?-i>
Im-
pinger
Temp.
•F
53
££-
A*.
Ate
y
$*
OM
on
-------
SAMPLE RECOVERY AND INTEGRITY DATA FORM
Plant J 'U.c.~ ''e.-ii-Vi.; o (LI./.T*/.''>,
Sample date 3>J 'Q/&.'•
* ...*/.--*< 3i ci.agr,
Net volume (wt)
Total moisture
Color of silica gel
ml
Silica gel
Final wt
Initial wt ?3l. (n g
Net wt /g
_g
_g
Description of impinger water
RECOVERED SAMPLE
Blank filter container number
Filter container number
Sealed
Sealed
Description of particulate on filter
Acetone rinse
container number
Acetone blank
container number
Liquid level
marked?
Liquid level
marked?
Samples stored and locked
Remarks
Date of laboratory custody
Laboratory personnel taking custody
Remarks
(c 0 //
A.O
to,?
XI
-e
S1
A- 7
PACIFIC ENVIRONMFNTAt <;cpv'rcc
-------
m
<
f
m
m
a
O
FIELD DATA
Plant
Date
Sampling Location
Sample Type
Run Number
Operator
/3 (3
F
21.
-^
Ambient Temperature
Barometric Pressure
Static Pressure (Pa) —.'
Filter Number (s) py*
Pretest Leak Rate • cfm t _
Pretest Pi tot Leak Check 0 /£
Pretest Orsat Leak Check
In. Hg
0
0,
w fr
Probe Length and TYpe J ' AgC*
Pi tot Tube I.D. No. £- /
Nozzle I.D.
D.30?
Assumed Moisture, %
Temp. Readout S/N
Meter Box Number
Meter AH* _ /, <
C Factor
- /O
Schematic of ,
Traverse Point Layout
3-T-|A
Post Test Leak Rate ',001 cfm
Post Test Pi tot Leak Check
Post Test Orsat Leak Check
^5" in. Hg
Velocity
Head (AP8)
In. H.O
o.i'r
0,33
6,10
I
IE
ASfjf
Orifice Pres.
Differential
(AH) In. H70
Desired Actual
3.6-0
3,10
S.IO
3./a
/•70
n.7?_
3,10
3. /O
a./a-
1,70
AM
^•?7
/.a.C
Tgo
Stack
Temp.
(Tfl)
F
3
J23_
ifc
-2it
7Jffc
TV.
Sff-l
Dry Caa Meter Temp.
Inlet
/03
7J.9
/OS"
XU-
/oy
ML
Outlet
(T
out
»F
-75-
j-£.
33-
Pump
Vacuusi
in. H
5,7
2^L
3,1.
&
j. V
±t
3. Off!
Sample
Box Temp.
filter '
1//T
^/»-
Ira-
pinger
Temp.
•F
57
O'l
ON
-------
PO
Page
of
Plant Namet j>EXCO PfZOQCiCTS -V-WOlJl/V.
Run Numberi 31- SL
Teat Datei
3 -itr-t 7
Operator: f~?
- H.
m
<
§
m
f
m
5
Traverse
Point
Number
F- 1
/Clock
Sampling / Time
Time, /(24-hour
(win) / clock)
/ no (a
9U //7
5,
M.3-
I3tei
tin
Sample
Box Temp.
Filter
Temp. *F
iJ/A-
A//*
vi/
A/A-
Im-
pinger
Temp.
°F
o3
53
5-5:^,
S'<
on
P/vrtlA<»
4" '"I '0
1731
-------
1
3
— — .— ^— — — — — — — - - — — — — — — — u ui i i
•.:••* /
SAMPLE RECOVERY AND INTEGRITY DATA FORM
Plant OTL^O f COOWCLTJ ^'Voix/M} Sample date 3/'&/~r)'7
Sample location ChRomE c.^? M s««ffi«v't.
Sample recovery person AiWf|S">A'vJ
Filter (s) number N//A
MOISTURE
Impingers
Final volume (wt) Si^ ml (g)
Initial volume (wt) S-""^ ml (g)
Net volume (wt) ml (g)
Total moisture g
Color of silica gel
Description of impinger water () .1 tJ V(.L
i-v^-7 Run number .J- ^>
Recovery date 3/1 $ /&•
Silica gel
Final wt 737.3-g
Initial wt 7 ok,
-------
P/J
-g.
I
m
z
M
m
31
>
FIELD DATA
Plant
Date
Sampling Location
Sample Type rnp>
Run Number
Operator ?* rvie7*t>ou)S -
T-3
-3t0
Ambient Temperature _
Baronetrie Pressure _
Static Pressure (P8)
Filter Number(s)
Pretest Leak Rate • ,oo( cfm
Pretest Pi tot Leak Check
Pretest Great Leak Check
in. Hg
0(C
Utl-lUZ
/VJ6-
/J/A
Probe Length and Type
Pi tot Tube I.D. No. _
Nozzle I.D. 0.303
S-l
Assumed Moisture,
Temp. Readout S/N
Meter Box Number
Meter AHj ), fry
C Factor 1,
-------
Page
of
Plant Namet
Run Numberi
Pft
g-3
yucTS
~Mv/ B
01
tit
10 3
Outlet
t
LO_L
o?-
lOO,1-
Pump
Vacuum
in. Hg
J.P-
3,3
6. -5"
76. oj
Sample
Box Temp.
Fitter
Temp. °F
Im-
pinge r
Temp.
•F
SO
SI
s/
X
on
-------
SAMPLE RECOVERY AND INTEGRITY DATA FORM
Plant
3 - H-
Sample location hi rCTTU. U
rL'>bhr~r
Sample date
T^iT Run number
X-3
Sample recovery person
Filter(s) number
Recovery date 3-/*>-/ 7
MOISTURE
Impingers
Final volume (wt)
Initial volume (wt)
Net volume (wt)
Total moisture
Color of silica gel
Description of impinger water
ml (g)
5>OO ml (g)
ml (g)
Silica gel
Final wt g
Initial wt "737.3 g
Net wt g
_g
_g
_g
RECOVERED SAMPLE
Blank filter container number
Filter container number
Sealed
Sealed
Description of particulate on filter
Acetone rinse
container number
Acetone blank
container number
Liquid level
marked?
Liquid level
marked?
Samples stored and locked
Remarks
Date of laboratory custody
Laboratory personnel taking custody
Remarks
fcnfiL
652.6.
O
737.3
23.V
A-13
PACIFIC
-------
SAMPLE CHAIN OF CUSTODY
Plant: tAfO "><1 mCJS- V^-Wo-W^JL Test Number:
Date Sampled: 3| \q\fc~l _ Run Number: X
SAKPLE RECOVERY
Container Code Description
Person Engaged in Sample Recovery
/Vn
Location at whiclr Recovery was Done^g) £lf^L*O"
Date and Time of Recovery: 5|l^ ^"1 4.600
Sample(s) Recipient Upon Recovery if Not Recovery Person
Signature:
Title:
Date and Time of Receipt:
Saaple Storage:
Laboratory Person Receiving Sample--, ,.y
Signature: s- •.•
Title: \";:_.v>/v -
.., .=
Date and Time of Receipt: <'/?•< X"-/' -'-*3<:2
~ .-
Sample Storage:
ANALYSIS
Date and Time
Container Code Method of Analy«i« of Analysis Signature of Analyst
A-14
-------
SAMPLE CHAIN OF CUSTODY
Plant: J\J \ f ^ ProfitirK-Li /AYUA Test Number:
Date Sampled: 3/ f<3//Q"7
Run Number:
SAMPLE RECOVERY
Container Code
Description
Person Engaged in S
Signature
Title:
le Recovery
Location at which
Date and Time of Recovery:
covery was Done:^L
^i
Sample(s) Recipient Upon Recovery if Not Recovery Person
Signature:
Title:
Date and Time of Receipt:
Sample Storage:
Laboratory Person Receiving Sample
Signature:
Title:
/"
Date and Ti»e of Receipt:
Sample Storage:
ANALYSIS
Container Code
Method of An*ly«i«
Date and Time
of Analysis
Signature of Analyst
A-15
-------
SAMPLE CHAIN OF CUSTODY
Plant: PP-^ p<2opuC7"£ - /•> it/o*J i A~ Test Number:
Date Sampled: 3~/f-f ? _ Run Number:
SAMPLE RECOVERY
Container Code
Description
-f
n i/
^n^
Person Engaged in Sample Recovery
Title
: fy
Location at which Recovery was Done: AT p
Date and Time of Recovery: 3llt Ik "7 I'iOO
Sample(s) Recipient Upon Recovery if Not Recovery Person
Signature: '
Title:
Date and Time of Receipt:
Sample Storage:
Laboratory Person Receiving Staple
Signature: r\
Title: CA,
Date and Time of Receipt:
Sample Storage:
..v/
<''
ANALYSIS
Container Code
Method of Analy«i«
Date and Tine
of Analysis
Signature of Analyst
A-16
-------
SAMPLE CHAIN OF CUSTODY
Plant: J>O_^j ?gQ(>uCT5- l-M/fl/P'/l" Test Number:
Date Sampled: 3/> f /^Kl _ Run Number:
SAMPLE RECOVERY
Container Code
B-f _ Q.I A/ tJa-OH
Description
Person Engaged in Sample Recovery
Signature .
-JT- • ' / /'•;•
Signature:
/ , .,
Title:
Date and Time of Receipt:
Sample Storage:
^
9 y ? / ,>' 7
ANALYSIS
Date and Time
Container Code Method of Analysis of Analysis
Signature of Analyst
A-17
-------
SAMPLE CHAIN OF CUSTODY
Plant: pgt_CQ
Date Sampled:
Test Number: —
Run Number: j- /
SAMPLE RECOVERY
Container Code
Description
0,1
ft-
+n
---
Person Engaged in Sample Recovery
Signature:
Title:
/ J~\ \t~JJ\jU\
7i
Location at which Recovery was Done:
Date and Time of Recovery: 3/
pLWT
O.OOO
Sample(s) Recipient Upon Recovery if Not Recovery Person
Signature:
Title:
Date and Time of Receipt:
Sample Storage:
Laboratory Person Receiving Sample
Signature: , '^ IL
Title: CL,
Date and Time of Receipt:
Sample Storage:
.9 An I in
ANALYSIS
Container Code
Method of Analy«i«
Date and Time
of Analysia
Signature of Analyst
A-18
-------
SAMPLE CHAIN OF CUSTODY
Plant: £>£j.£O /.iVo/vynQj m»C>u Test Number:
Date Sampled: 3lt*j I-K~] Run Number:
SAMPLE RECOVERY
Container Code Description
TA.
Person Engaged in Sample Recovery
Signature:
Title:
Location at which Recovery was Done: & /?T &J.Ai\n~
Date and Time of Recovery:
Sample(s) Recipient Upon Recovery if Not Recovery Person
Signature:
Title:
Date and Time of Receipt:
Sample Storage:
Laboratory Person Receiving Sample
^•' -"> -• x
Signature:
Title:
Data and Time of Receipt: .'5/3'* / ^'^ S* 3G
Sample Storage:
ANALYSIS
Date and Time
Container Code Method of Analysis of Analysis Signature of Analyst
A-19
-------
SAMPLE CHAIN OF CUSTODY
•Plants S^>Et6o J-.Vor^v m.r,^. Test Number:
Date Sampled: 3.l/&(*7 ^ 3Ji
-------
SAMPLE CHAIN OF CUSTODY
Plant:
m*:h.
-
Date Sampled:
Test Number:
Run Number:
^"-JL
SAMPLE RECOVERY
Container Code
'L
Description
3/g/ft 7 *? ! «ro Xl/rt. / /: /o
TA/JX. .3
^
ft^TI/Vrv ^^Lv
^^•^h^***fc*^™^'^"'*^l^*^
^/t-K/n'7
Person Engaged in Sample Recovery
Signature: /^k^x^- kJ.JAJ
Title: •"TV
/v
Location at which Recovery was Done: A~f
Date and Time of Recovery:
l-g/157 A3.I.-5V3
Sample(s) Recipient Upon Recovery if Not Recovery Person
Signature:
Title:
Date and Time of Receipt:
Sample Storage:
Laboratory Person Receiving Sample
// - -i
Signature:
title:
^ .!>•» — -
Co*.., lo
Date and Ti»e of Receipt:
Sample Storage:
J/3.~ 7 . :/-?
ANALYSIS
Container Code Method of Analysis
Date and Time
of Analysis
Signature of Analyst
A-21
-------
Plant:
Date Sampled:
SAMPLE CHAIN OF CUSTODY
- Test Number:
Run Number:
SAMPLE RECOVERY
Container Code
Description
o.
Ov Sol
Person Engaged in Sample Recovery
Signature: H^fL^j.-t>^~ M/. (X JJ
Title: TECJ-, A/ic. i A (\J
Location at which Recovery was Done:
Date and Time of Recovery:
(Pi A NT
Sample(s) Recipient Upon Recovery if Not Recovery Person
Signature:
Title:
Date and Time of Receipt:
Sample Storage:
Laboratory Person Receiving Sample
»/..
Signature: _
Title:
a /
V, \
^f"
(./.<../ -^-y* /*.-( < Q^.—
Date and Tine of Receipt:
Sample Storage:
:•] It •-', I >,* --j
ANALYSIS
Container Code
Method of Analysis
Date and Time
of Analysis
Signature of Analyst
A-22
-------
APPENDIX B
Calculations
B-l
-------
EMISSION TEST CALCULATIONS
PLANT PG-CQ pgODgcTS - )-H/Q*-l/A- SOURCE/RUN J~- / DATE 3-//-) = ^f.^O lb/lb-mole
B-2
-------
J"' I
6. Stack Gas Velocity, Average
VSavg = 85.49Cp (V/AP )avg
= 85.49 ( .^ )
3avg
f t/s
Volunctric Flow Itotc, Ac tun 1 Conditions (Stack Tonjjoraturc and Pressure)
X Vg (
-------
EMISSION TEST CALCULATIONS
PLANT Pfcuco pflooac-rs- igoo.O(A- SOURCE/RUN
1. Leakage Correction for Volume Metered
VIT = Vm - (Lp-La)8 = Vm- (Lp-0.02)0=
3
X-2.
DATE *>-
-0.02)
ft
2. Volume Metered, Standard Conditions (68°F, 29.92 in.Hg)
17.64
- 17.64
= 155". ^5^ dscf
3. Volume Water Vapor Collected, Standard Conditions
Impingers = V^ = 0.04707 (Vf - V±) = 0.04707 (H.
Silica Gel = Vws= 0.047(5 (Wf - Wi) = 0.047IS CiO
Vw
std
4. Percent Moisture, By Volume
Vw
Vwstd Vmstd
scf'
rt/
/,03/o
5. Molecular Weight, Stack Gas
Dry Molecular Weight, Md = 0.440 (%CO2) + 0.320(%02) + 0.280 (%N2 + %CO)
= 0.440 ( ) + 0.320( ) + 0.280 ( )
Ib/lb - nole
Percent Excess Air,%EA =
- 0.5 %CO
L0.264(%N2H%02-0.5 %CO
%EA =
+ 18.0
X100
_0.264(
H
-0.5(
X 100
= (JL9.0 ) (1- .010* ) + 18.0 (.0/03 ) =
Ib/Ib-role
B-4
-------
00
o
-T-
6. Stack Gas Velocity, Average
V*avg " 85'
vs = 30.
PsMs
= 85.49
( 5^ >
avg
f t/s
7. Shirk Volunetrlc Flow Jin to, Actunl Conditions (Stack Tcmjjoraturc and Pressure)
Qa (circular) =
X v
(5>454 x 1Q-3} (d2)
144
= 60 X
(5.454 X 10~3) (
JLw) =
L44 J
"or" Qa( rectangular) = 60 X V ) = 60 X V (L X W) 6.944"'X 10
s 144 s
-3
= 60 X
) 6.944 X 10
-3
Qa =
ac£m
8. Stack Volumetric Flow Rate, Standard Conditions (68°F, 29.92 in. Hg)
=17-64
Q
std
dscfm
9. Isokinetic Variation
%I = K
Ps Vs An
= 0.0944
1-.OIQ3)
B-5
-------
EMISSION TEST CALCULATIONS
PLANT VQ_CQ
-Lli/Q/J/'ft- SOURCE/RUN
DATE
1. Leakage Correction for Volume Metered
Vnic = vm ~ (Lp-La)8 = Vm - (Lp-0.02)6 =
ft3
-0.02) (
2. Volume Metered, Standard Conditions (68°F, 29.92 in.Hg)
' 13.6
V,
= 17.64
Vmstd= /5S.
dscf
3. Volume Water Vapor Collected, Standard Conditions
Inpingers = V = 0.04707 (Vf - Vj^) = 0.04707 ( 5'.^ ) = 0,llf<-f
rK.f
Silica Gel = Vws=0.047fS (Wf - Wi) = 0.047IS ( ^3.^. ) = / . (03
std = Vwc + Vws =
scf
scf
Vw
4. Percent Moisture, By Volume
*std
vw.
= O.OO&'Z.
S Vwstd + Vmstd ( I
5. Molecular Weight, Stack Gas
Dry Molecular Weight, M& = 0.440 (%CO2) + 0.320(%O2> + 0.
= 0.440 ( ) + 0.320( ) + 0.
i. 0 Ib/lb - mole
280 (%N2
280 (
+ %CO)
)
Percent Excess Air,%EA =
%0? - 0.5 %CO
^.264(%N2H%02-0.5 %CO
%EA =
+ 18.0
X100
0.264(
H
-0.5(
X 100
18.0
Ib/lb-role
B-6
-------
o
6. Stack Gas Velocity, Average
Vs = 85.49C (X/P )avg
f t/s
= 85.49
savg
7. Shirk Volunctr.ic Flew Rite, Actual Conditions (Stack Tcmi^.-raturc and Pressure)
Qa (circular) «/6° X Vg (* dV/1 V 60 X Vs (5.454 X 1(T3) (d2,
= 60 X
(5.454 X 10~3) (
or" Qa (rectangular) = 60 X
= 60 X 30.
= 60 * v
-------
w-*! £
/s / . no
=• V- ? 7 ^
So
/ U
")
L-
O.tO.U
. 363
I
B-8
-------
-Ko
^ (O< 000^<4
»
-------
B-10
-------
-------
._ CO /v/; C .:. _ -
« S ^ ^TTJ )
u
xmf_ „ Q.02_™ A /l-O ^
^^ V XT* 4 _."Ml^4t^
cftJsn? I
-------
•t-
(Q.(2(o &
< A^
-+H
Ii
J!
B-13
-------
APPENDIX C
Laboratory Analytical Results
C-l
-------
PEI Associates. Inc.
11499 Chester Rd.
Cincinnati, OH 45246
(513) 782-4700
APK i 4 1987
Clienti Peer Consultants
4134 Linden Avenue
Suite 202
Dayton, Ohio 45432
Attn: Ms. Helen Owens
Project No.t
Requisition No.t
Date Received:
Sampled by:
Date Reported:
4761
T7-03-136
3/23/87
Client
4/14/87
Sample ID
Run 1-
Run 1-
Run 1-1
Run 1
Run 1
Run 1
Run 1
Run 1
Run 1
Run 1-
Run 1-
PEI No.
Run
Blank
Blank
1-
1 Tank 1
1 Tank 2
Tank 3
2 Tank 1
2 Tank 2
2 Tank 3
3 Tank 1
3 Tank 2
3 Tank 3
1 Emission Sample
2 Emission Sample
3 Emi ssi on Samp1e
•for Run 1&2
for Run 3
01A
O2A
03A
O4A
05A
O6A
07A
08A
09A
1OA
11A
12A
13A
14A
Total
Chromium,
mg/1
153,000
147,000
157,000
152,000
151,000
146,000
151,000
151,000
138,000
10.2
6.93
9.52
<0.02
<0.02
Hexavalent
Chromium,
mg/1
150,OOO
160,000
153,OOO
152,OOO
154,OOO
160,000
158,OOO
158,000
160,000
12.0
7.42
1O. 1
O.O11
O.O13
C-2
Submitted by:
-------
PEI Associates. Inc.
11499 Chester Rd.
Cincinnati, OH 45246
(513) 782-470O
APR ] 4 1037
Client: Peer Consultants
4134 Linden Avenue
Suite 202
Dayton, Ohio 45432
Attn: Ms. Helen Owens
Project No.:
Requisition No.:
Date Received:
Sampled by:
Date Reported:
4761
T7-03-137
3/23/87
Client
4/14/87
Sample ID
Filter
Filter
Filter
Filter
Filter
Filter
Filter
Filter
Filter
Filter
Filter
Filter
Blank
Blank
Blank
#AC-2
#AC-2A
#AC-4
#AC-4A
#BC-6
#BC-6A
#DC-5
#DC-5A
#EC-1
#EC-1A
#EC-3
#EC-3A
Filter #1
Filter
Filter
#2
#3
PEI No.
01A
O2A
O3A
04A
05A
O6A
O7A
O8A
O9A
10A
MA
12A
13A
14A
ISA
Hexvalent
Chromium, ug
<0.8
-------
APR
PEI Associates. Inc.
11499 Chester Rd.
Cincinnati, OH 45246
(513) 782-4700
Client: Peer Consultants
4134 Linden Avenue
Suite 202
Dayton, Ohio 45432
Attn: Ms. Helen Owens
Project No.:
Requisition No.t
Date Received:
Sampled by:
Date Reported:
4761
T7-03-137
3/23/87
Client
4/14/87
Sample ID
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
Sample
Sample
Sample
Samp1e
Sample
Sample
Sample
Sample
Sample
Samp1e
Samp1e
Sample
Sample
Sample
Sample
Sample
Sample
Samp1e
Sample
Sample
Sample
Sample
Sample
Sample
Blank
#AC-2
#AC-2A
#AC-4
#AC-4A
#BC-6
#BC-6A
#DC-5
#DC-5A
#EC-1
#EC-1A
#EC-3
#EC-3A
#AP-6
#AT-6
#BP-2
#BP-4
#BT-2
#BT-4
#CP-5
#CT-5
#FP-1
#FP-3
#FT-1
#FT-3
PEI No.
16A
17A
18A
19A
20A
21A
22A
23A
24A
25A
26A
27A
28A
29A
30A
31A
32A
33A
34A
35A
36A
37A
38A
39A
4OA
Hexvalent
Chromium, ug
1.8
8.0
-------
Analyst
__
\ "T^O.. S?*<^
PN grJfl? *7 *> / .- , . /
LAbUKAlUK* UAIA
Analysis _
Method Number
Checker *-*"'
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-------
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LABORATORY DATA
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C-10
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C-ll
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rupnt P^ ^ r /^.^ ^ ix J4,* ^-f s xi^X Analysis .^/Ac«-/-><-
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C-12
-------
LMOUKAIUKI UMIM
rupnt.^ J^L , .* C^^.^ ^^ZGL^ A x^^y Analysis
Analyst
Date
/
Method Number
Checker
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VALUC
MUI...TIPL If'P
1 5.366014 H
15.519ftc>45
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-------
2 IM D 1_T C TT I V E L V C. O XJ IT' J.- E D r» 1_ J\ £T. r*T A
A IM A 1_ V TT I C A I_ n T : IP O R. -£•
Client: Peer Consultants Date of Analysis: 4-9-87
PN<1761 W.O.«T7-03-136
Rgt Dlk O_Cr
mean - 0.
uni ts n»g/
PEI *3 prp O_Cr_
mean 0.9834
un its mg/I
3-136-1*1:100 O_Cr_
mean 15.3100
uni t s mg/1 s
136-2a 1:100 O_Cr_
mean 14.7250
units mq / I * '
136-3a 1:100 O_Cr_
mean 15 . 7250
units mg/1 _- /?f7i5O*'*
136-4a 1:100 O_C r_
mean 15.2200
units mg/1 =/S'ZZCC^'
136-5a 1:100 O_Cr_
mean 15.0850
units mg / 1 ; /^
l36-6a 1:100 O_C r_
mean 14.6350
uni t s mg/1
136-7a 1:100 O_Cr_
mean 15.3200
units mg / 1 /:>"
»36-7aR 1:100 O_Cr_
mean 14.9100
units mg/
\
'
3 (- -8 a 1:100 O_Cr_
mean 15.1200
units mg/1 ,$i3.0C '*»J5/X
(7
36-9a 1:100 O_Cr_ C-15
mean 13.7500
units mg/l ,--5 lS'«-*C 'J
-------
136-10* O_Cr_
me*n 10.2000
uni t s mg / 1
136-11* O_Cr_
mean 6 .9260
units mg/1
136-11* +1 O_Cr_
*r sit/^cV mean 7.6655
units mg/1 -
136-12* O_Cr_
mean 9.5220
units mg/1
136-13* O_Cr_
me * n - 0 . 0 (/I S
units mg //i
st«tus window edge
136-14* O_Cr
mean -0 .
un i t s mg
C-16
-------
PN
Analyst
i-MOOKMIUKI UMIM
Hate
Analysis
Method Number
Checker
&.m
GO
"
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±L
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-------
D \j c:
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Client: Crown Cntrl.Peer Consultants
PN: 6310.1761
Date of Analysis: 4-9-87
Cal Blk
Chk Std
PEI #3
:al Blk
I
I
hk Std #1
Cal Oik
hk Std tl
'El #3
mean
units
status
mean
un its
mean
units
mean
units
status
mean
uni t s
mean
un its
mean
un its
0_C
-0
mg
r_
. oXl 8
i/C
window edge
<.
O_C
2
mg
O_C
0
mg
O_C
-0
mg
-C
-------
APPENDIX D
Determination of Cr+6 and Total Cr Emissions
D-l
-------
APPENDIX D
DETERMINATION OF Cr6 AND TOTAL Cr EMISSIONS
The following sample and analytical procedures were used during this
test program. Sampling procedures generally followed those described in the
EPA Test Method 13B (MM 13B). The sample train used at the evaporator/
scrubber inlet test location was assembled by test crew personnel and
consisted of the following items:
Nozzle - Stainless steel (316) with sharp, tapered leading edge and
accurately measured round opening.
Probe - Borosilicate glass without a heating system.
Pi tot Tube - Type-S pi tot tube that meets all geometric standards. The
tube was attached to the probe to monitor the stack gas velocity.
Thermocouple - Type-K thermocouple capable of measuring stack gas
temperatures within 2 percent. This thermocouple was attached to the
probe.
Draft Gauge - An incline manometer made by Dwyer with a range of 0 to
10 inches of H20.
Impingers - Four Greenburg-Smith impingers connected in series with
glass ball joints. The second impinger was of the standard
Greenburg-Smith design. The first, third, and fourth impingers were of
the Greenburg-Smith design, but modified by replacing the tip with a
1 40 CFR 60, Appendix A, Reference Method 13B, July 1985,
D-2
-------
1/2-inch i.d. glass tube extending to 1/2-inch from the bottom of the
flask.
Metering System - Vacuum gauge, dry gas meter, leak-free pump,
thermometers and related equipment to maintain an isokinetic sampling
rate and to determine the sample volume.
Barometer - Aneroid type to measure atmospheric pressures to within
(approximately) 2.5 mm Hg (approximately 0.1 in. Hg).
Sampling Procedures
Prior to departure, all glassware used in this study was washed with
10 percent nitric acid to minimize the potential for contamination. On
hundred mfi, of 0.1 N NaOH was placed in each of the first three impingers;
approximately 300 g of silica gel was added to the fourth impinger. The
train was set up with the probe as shown in Figure D-l. The sampling train
was leak checked at the sampling site prior to each test run by plugging the
inlet to the nozzle and pulling a 15- to 16-inch Hg vacuum, and at the
conclusion of the test by plugging the inlet to the nozzle and pulling a
vacuum equal to the highest vacuum reached during the test run.
The pi tot tube and lines were leak checked at the test site prior to and
at the conclusion of each test run. The check was made by blowing into the
impact opening of the pi tot tube until three or more inches of water was
recorded on the manometer and then capping the impact opening and holding it
for 15 seconds to assure that it was leak free. The static pressure side of
the pitot tube was leak checked using the same procedure, except suction was
used to obtain the 3-inch H 0 manometer reading. Crushed ice was placed
around the impingers to keep the temperature of the gases leaving the
impinger at 68°F (20°°C) or less.
During sampling, stack gas and sampling train data were recorded at each
sampling point to monitor when significant changes in stack flow conditions
D-3
-------
1.9-2.5 cm
(0.7S-1 in
1.8 cm (0.75-1 in.) •
STACK WALL
H
^
%fc* I ~"~ '
THERMOCOUPLE
PROBE
PITOT TUBE
HEATED GLASS PROBE
THERMOMETER
\
S-TYPE
PITOT TUBE
PITOT
MANOMETER
IMPINGERS
VACUUM
LINE
THERMOMETERS
BYPASS
VALVE
O VACUUM
V ) GAUGE
ORIFICE
MANOMETER "
AIR TIGHT
PUMP
IMPINGER CONTENTS
1. 100 ml 0.1 N NaOH
2. 100 ml 0.1 N NaOH
3. 100 ml 0.1 N NaOH
4. 200 g SILICA GEL
Figure D-l. Cr /Total Cr sampling train.
D-4
-------
occurred so proper adjustments could be made. Isokinetic sampling rates
were set throughout the sampling period with the aid of a nomograph.
Sample Recovery Procedures
The MM 13B trains were moved carefully from the test site to the
designated cleanup/recovery area. The cleanup area was located in the plant
in an area isolated from possible contamination and when possible, sample
recovery was done in the cleanup van.
Each impinger was weighed after each test to determine the amount of
moisture present. Sample fractions were recovered as follows:
Container No. 1 - The nozzle and probe were rinsed with 0.1N NaOH and
brushed with a nylon brush. This rinseate was collected in a
polyethylene bottle. The inter-connecting glassware was rinsed with
0.1 NaOH and combined with the probe and nozzle rinses. After the
impingers were weighed, their contents were combined with the rinseates
from the nozzle, probe and glassware in the sample bottle. The
impingers were also rinsed with 0.1N NaOH and this rinseate was combined
with the rinses from the other sample train constituents in the
polyethylene sample bottle.
Container No. 2 - Approximately 400 ma of 0.1 N NaOH was taken during
each sample recovery activity for blank analysis.
The silica gel from the fourth impinger was weighed, and this value was
recorded with other pertinent data on the Sample Recovery and Integrity Data
Sheet.
Sample Analysis - Hexavalent Chromium
Each sample including blanks was analyzed for Cr+6 using analytical
methodology recent developed by the EPA. A copy of the draft method
D-5
-------
entitled "Determination of Hexavalent Chromium Emissions From Stationary
Sources" is contained in Appendix G of this report. Procedures generally
follow those described in EPA Method 3050.2
Prior to analysis, an aliquot from Container 1 was filtered through
Teflon to remove any solids present in the sample. The Teflon filter was
cut into small pieces and placed in a 250-mfc beaker. Twenty-five mfi. of
NaOH/N CO digestion solution was added to the beaker. The beaker
2 3
was covered with a watch glass and heated to near boiling on a hot plate.
The solution was stirred constantly for 30 minutes, and care was taken to
avoid evaporating the solution to dryness.
The solution was cooled and filtered through a 47-mm Teflon filter, the
beaker was rinsed with deionized, distilled (DI) water, which was then
filtered. The filtrate was transferred quantitatively from the filter flask
to a 100-mfi, volumetric flask, and then brought to volume with DI water.
Blank filter samples were digested and prepared in a similar manner.
A 50-mfi, or small aliquot of the prepared sample was transferred to a
volumetric flask. A two percent volume-to-volume ratio of diphenylcarba-
zide solution was added. The solution was allowed to stand for
approximately 10 minutes for color development. A portion of the sample was
A 50-mfi. or small aliquot of the prepared sample was transferred to a
volumetric flask. A two percent volume-to-volume ratio of diphenylcarba-
zide solution was added. The solution was allowed to stand for
approximately 10 minutes for color development. A portion of the sample was
transferred to a 1-cm absorption cell, which was placed in the spectrophoto-
meter. The absorbance was then measured at the optimum wavelength using the
blank solution as zero reference.
2 Test Method for Evaluating Solid Waste, U.S. EPA SW-846,
2nd Edition, July 1982, Method 3050.
D-6
-------
Sample Analysis - Total Chromium
The filtrates from the impinger contents (Container 1) were analyzed
2
for total Cr using preparation described in EPA Method 3050. Inductively
Coupled Argon Plasma (ICAP) spectroscopy techniques were used for sample
analysis.
2 Test Method for Evaluating Solid Waste, U.S. EPA SW-846,
2nd Edition, July 1982, Method 3050.
"D-7
-------
APPENDIX E
Equipment Calibration
E-l
-------
PRETEST CALIBRATION DATA
E-2
-------
DRY GAS METER AND ORIFICE CALIBRATION
Date:
Box No.:
C.
Barometric
Orifice
Manometer
Setting,
AH,
in. H-jO
0.5
1.0
2.0
4.0
8.0
Pressure
Gas Vol.
Wet Test
Meter
ft •
3 •?£ S~
7-'72-H
//-j-os
/s~-ix7
•if in. He
Wet Test
Meter
Op
_^s-
?3 _>-
£r
?S'-O
?S"-<3
j Dri
Tempei
Dri
Inlet
op
Z?
^7 _J • ^"~
r Gas M<
rature
' Gas M«
Outlet
°F
^.j-
3-9-- S~
%o->~
VL-C
...
2f6. &
Jter No.:
•ter
Average
Op
fr.X
Avei
Time
Q,
min.
/C'-C,
/ ^ o
/«• - 0
/ <•• -o •
/CJ- 0
rage
Y
tiT*o
^.•JT?
^i?"J?
0,9")S
0,1ft
\M*I
A Hi
l.tl
/,->W
•i^O
/, *0
/•*J7
**•/
Calculations:
AH
0.5
Irt
• U
2.0
4.0
6.0
8.0
AH
13.6
0.0368
Ort"7^ "7
* U / J /
0.147
0.294
0.431
0.588
Y
Vw Pb
-------
TEMPERATURE SENSOR CALIBRATION DATA FORM
Date 3-X3-/7
Ambient temperature
Thermocouple number /2/f-r: /
°C Barometric pressure in. Hg
Reference: mercury-in-glass
other
Reference
point
number3
Source
(specify)
Reference
thermometer
temperature,
Thermocouple
potentiometer
temperature,
Temperature
difference,
7 (» "Ppy-v
V. /
0.37
o
Every 30°C (50°F) for each reference point.
Type of calibration system used.
C|(ref temp. °c -t- 273) - (test thermom temp, °C + 273)1
L^ ref temp, °C + 273 ^J
100<1.5%
-------
PITOT TUBE CALIBRATION DATA SHEET
Calibrated By: /[,~
Date: J-/£"-,
Pi tot I.D. No.:
Effective Length: 3
Pi tot Tube Assembly Level? Yes
-------
PITOT TUBE CALIBRATION DATA SHEET
Calibrated By:
Date: ,?//£"
Pi tot I.D. No.: S-P>
Effective Length: PlToT TIP
Pi tot Tube Assembly Level? Yes *^ No
Pitot Tube Openings Damaged? Yes (explain below) No
° -
O • (<10°) ai™ O * (<10°) /
1 • c/ KIU-J. 1*2
62
«
Y - • e - • A - •
f—"""-
z - A sin - 0,050 cm (in.;) 0.32 ca (<1/8 in.)
-^^x
w - A sin - d cm (Tn~)) 0.08 cm (<1/32 in.)
cm
0
-------
TEMPERATURE SENSOR CALIBRATION DATA FORM
Date
Thermocouple number
- f
Ambient temperature °C Barometric pressure
Calibrator 'y//fJt#-*Lr*i Reference: mercury-in-glass
if * * 7
other
in. Hg
Reference
point
number3
Source
(specify)
Reference
thermometer
temperature,
Thermocouple
potentiometer
temperature,
Temperature
difference,
aEvery 30°C (50°F) for each reference point.
Type of calibration system used.
(ref temp, °c + 273) - (test thermom temp, °C + 273)
^
F
V
ref temp, °C + 273
E-7
-------
POST-TEST CALIBRATION DATA
E-8
-------
POSTTEST DRY GAS METER CALIBRATION DATA FORM
3 /£>*"/&:? Meter box number
Plant
Barometric pressure, P, = £ft <3,7? in- Hg Dry gas meter number
Pretest Y r p
Orifice
manometer
setting,
(AH),
in. H.,0
•OJO
0.70
0.70
p —
Gas volume
ftrf
meter
(V-
ft3
G»3.*H|
^.775"
Dry gas
meter
(vd).
ftJ
3H7.7«5"
3S1.SSO
7? 7?-r u«;x --
-------
TEMPERATURE SENSOR CALIBRATION DATA FORM
Date */- i^-
Thermocouple number £A-C
Ambient temperature "W '(= °C Barometric pressure
Calibrator F ftf Reference: mercury-in-glass
other
in. Hg
IS -((,7 C
Reference
point
number
Source
(specify)
Reference
thermometer
temperature,
°C
Thermocouple
potentiometer
temperature,
Temperature
difference,
v
/o
,3 7
Every 30°C (50°F) for each reference point.
DType of calibration system used.
:f(ref temp, °C + 273) - (test thermom temp, °C + 273)
ref temp, °C
273
E-10
-------
m m •K^anv
-gsaa
TEMPERATURE SENSOR CALIBRATION DATA FORM
DateJ-//^///'%7 Thermocouple number 3-7-//-V
Ambient te
Calibrator
Reference
point
number
d.
Li
mperature ?2>"'/f °£ Barometric pressure
fh\,-\jj
Source
(specify)
(.*«&
Reference: mercury-in-glass
other
Reference
thermometer
temperature,
<>* *-^cf
3"^' / ^ *-"
o \&
Thermocouple
potentiometer
temperature,
J
j
;/'!.<{ in. Hg
'••> '<_-,'!£-
Temperature
difference,
O
O
O
aEvery 30°C (50°F) for each reference point.
Type of calibration system used.
cf(ref temp, °C + 273) - (test thermom temp, °C * 273)1
L ref temp, °C + 273 J 10(X1.5%.
E-ll
-------
TEMPERATURE SENSOR CALIBRATION DATA FORM
Date '!/"•//<> '/
Thermocouple number .5//v~/
Ambient temperature 70
Calibrator /V/O//1/
°JC Barometric pressure £>~'
in. Hg
Reference: mercury-in-glass
other
Reference
point
number3
Source
(specify)
Reference
thermometer
temperature,
Thermocouple
potentiometer
temperature,
°C
Temperature
difference,
3
O
0
Every 30°C (50°F) for each reference point.
Type of calibration system used.
'F(ref temp, °C + 273) - (test thermom temp, °C + 273)1
Lref temp, °C * 273^J
E-12
100^1.5%.
•31 —iT',- f\
-------
APPENDIX F
Project Participants and Activity Log
F-l
-------
TABLE F-l. PROJECT PARTICIPANTS
Name
Title
Responsibility
F. Clay
J. Swartzbaugh
H. Owens
A. Weisman
F. Meadows
R. Barker
Task Manager
U.S. EPA - EMB
PEER Consultants, P.C.
Program Manager
PEER Consultants, P.C.
Project Leader
PEER Consultants, P.C.
Technician
PES
Project Leader
MRI
NSPS contractor
Coordinated test
activity, on-site data
reduction and calcu-
lations.
Coordinated test activi-
ty with subcontractors
and EPA, report
preparation.
Coordinated test activi-
ty with EPA, MRI, PES
and Delco personnel,
report preparation.
Collected process
samples, sample recovery.
Site leader for inlet
testing, data reduction
Monitored process
operation and
coordinated test
activity.
TABLE F-2. ON-SITE ACTIVITY LOG
Date
03-16-87
03-17-87
03-18-87
03-19-87
Activity
Test crew and equipment travel to Livonia,
Michigan, set up equipment, prepared site,
conducted preliminary measurements.
No testing - process not operating.
Conducted two MM 13B and collected all relative
process samples, monitored the process conditions.
Conducted one MM 13B, collected process samples,
monitored process conditions, packed van,
returned to home offices.
F-2
-------
APPENDIX G
Analytical Methods For Determining
Cr+6 and Cr
G-l
-------
Metnoo - Detprnn nati on of hexavalent Cnromiutn
Emissions from Stationary Sources
1. Applicability and Principle.
1.1 Applicability. This metnod applies to the determination of
hexavalent chromium (Cr*&) emissions from specified stationary sources
only.
1.2 Principle. Particulate emissions are collected from the source
by use of Method 5 (Appendix A, 40 CFR Part 60). The collected samples are
digested in an alkaline solution and analyzed by the diphenylcarbazide
coloritnetric method.
2. Range. Sensitivity. Precision, and Interferences.
2.1 Range. A straight line response curve was obtained in the range
5 yg Cr*6/100 ml to 250 vg Cr+6/100 ml. For a minimum analytical accuracy
of *10 percent, the lower limit of the range is 50 ^g/100 ml. The upper
limit can be extended by appropriate dilution.
2.2 Sensitivity. A minimum detection limit of l_wg Cr^o/lOO ml
has been observed.
2.3 Precision. The overall precision for sample collection and
analysis for Cr"*^ was tested at a ferrochrome smelter, a chemical plant,
and a refractory brick plant. Replicate Method 5 filters with both high
and low particulate loadings were analyzed. The relative standard
deviation was 4.4. 8.3, and 13.3 percent, respectively.
2.4 Interference. Very large quantities of iron, molybdenum,
vanadium, and mercury can interfere with the analysis. Ho interference
was observed at the sources listed in Section 2.3.
G-2
-------
3. Apparams.
2.1 Sampling Train. Same as Method 5. Section 2.1.
3.2 Sample Recovery. Same as Method 5. Section 2.2.
3.3 Analysis. The following equipment is needed.
3.3.1 Beakers. Borosilicate. 250 ml, with watchglass covers.
3.3.2 Filtration Apparatus. Vacuum unit with 47 mm diameter,
3.0 u pore size Teflon filters.
3.3.3 Volumetric Flasks. 100 ml and other appropriate volumes.
3.3.4 Hot Plate.
3.3.5 Pipettes. Assorted sizes, as needed.
3.3.6 Spectrophotometer. To measure absorbance at 540 nm.
4. Reagents.
4.1 Sampling. Same as Method 5, Section 3.1.
4.2 Sample Recovery. Same as Method 5, Section 3.2.
4.3 Analysis. The following reagents are required. _
4.3.1 Sodium Carbonate. Na2C03. anhydrous, analytical reagent
grade.
4.3.2 Sodium Hydroxide. NaOH, analytical reagent grade.
4.3.3 Potassium Dichromate. ^Cr^O;, analytical reagent grade.
4.3.4 Water. Deionized distilled, meeting American Society for
Testing and Materials (ASTM) specifications for type 3 reagent - ASTM
Test Method 0 1193-77 (incorporated by reference - see S 61.18). If high
concentrations of organic matter are not expected to be present, the
analyst may eliminate the KMn04 test for oxidizable organic natter.
G-3
-------
<.3.S Digestion Solution. Dissolve 2u.O 9 NaOH and 3f.O g
in deionized distilled water in a 1-liter volumetric flask and dilute to
the mart. Store the solution in a tightly capped polyethylene bottle and
prepare fresh monthly.
4.3.6 Potassium Oichromate Stock Solution. Dissolve 141.4 mg of
dried I^CrzO; in deionized distilled water and dilute to 1 liter
(1 ml = 50 ug Cr*6).
4.3.7 Potassium Dichromate Standard Solution. Dilute 10.00 ml
K2Cr20? stock solution to 100 ml (1 ml = 5 vg Cr*6) with deionized
distilled water.
4.3.8 Sulfuric Acid. 10 Percent (v/v). Dilute 10 ml of reagent grade
^SO^ to 100 ml in deionized distilled water.
4.3.9 Diphenylcarbazide Solution. Dissolve 250 mg of
1. 5-diphenylcarbizide in 50 ml acetone. Store in a brown bottle. Discard
when the solution becomes discolored.
4.3.10 Acetone. Same as Method 5. Section 3.2.
5. Procedure.
5.1 Sampling. Same as Method 5. Section 4.1.
5.2 Sample Recovery. Same as Method 5. Section 4.2.
5.3 Preservation. Tests with the source samples described in
Section 2.3 demonstrated that Cr+6 is stable in particulate form.
Nevertheless, all samples should be protected from extreme heat, and
should be analyzed within 1 month of collection.
G-4
-------
S.< Sample Digestion ana Preparation. Place the contents of
Container Number l (tne filter) ana Container Number 2 (tne acetone probe
rinse) in a 250 ml beaker. Evaporate to dryness. Add 40 ml of digestion
solution (Section 4.2.5). Cover the beaker with the watchglass and heat to
near boiling on a hot plate with constant stirring for 30 minutes. Oo not
allow the solution to evaporate to dryness.
Cool the solution and transfer it quantitatively to the filtration
apparatus with deionized distilled water. Filter the solution through
the 47 mm Teflon filter. Transfer the filtrate from the filter flask
quantitatively to a 100 ml volumetric flask. Fill to the mark with
deionized, distillea water.
5.5 Reagent Blank Preparation. Place a 47 mm diameter filter in a
100 ml beaker. Proceed as in Section 5.4.
5.6 Silica Gel Weighing. Weigh the spent silica gel (Container
Number 3) or silica gel plus impinger to the nearest 0.5 g using a balance.
This step may be conducted in The field.
5.7 Analysis.
5.7.1 Color Development and Measurement. Transfer 50 ml aliquot of
the prepared sample to a 100 ml volutnetric flask. Add 2.0 ml of
diphenylcarbazide solution. Adjust the pH to 2 * 0.5 with 10 percent ^50$
and dilute to volume with deionized distilled water. Allow the solution to
stand about 10 minutes for color development. Transfer a portion of the
sample to a 1-cm absorption cell and measure the absorbance at the optimum
wavelength (Section 6.2.1), using the blank solution as a zero reference.
G-5
-------
Dilute tne sample anc the blanl with equal volumes of oeiomzeo cistillec
water if tnt absorbance exceeds A4 . tne absorbance of the 250 vg Cr*6
standard as determined in Section 6.2.2. Use oeionized. distilled water to
iero the instrument.
5.7.2 Check for Matrix Effects on the Cr*6 Results. Since the
analysis for Cr*6 by colorimetry is sensitive to the chemical composition
of the sample (matrix effects), the analyst shall check at least one sample
from each source using the method of additions as follows:
Add or spike an equal volume of standard solution to an aliquot of the
sample solution, then measure the absorbance of the resulting solution and
the atsorbance of an aliquot of unspiked sample.
Next, calculate the Cr"1"6 concentration Cs. in ug/ml of the sample
solution by using the following equation:
Where:
ca = Cr* concentration of the standard solution g/nl.
As = Absorbance of the sample solution.
At « Absorbance of the spiked sample solution.
Volume corrections will not be required if the solutions as analyzed have
been made to the same final volume. Therefore. Cs and Ca represent Cr*6
G-6
-------
concentrations oefore dilutions. If the results of the method of Additions
procedure used on the single source sample oo not agree to within S percent
of the value obtained by the routine spectrophotome trie analysis, then
reanalyze all samples from the source using this method of additions
procedure.
6. Calibration.
6.1 Sampling Train. Perform all of the calibrations described in
Method 5, Section 5.
6.2 Spectrophotometer Calibration.
6.2.1 Optimum Wavelength Determination. Calibrate the wavelength
scale of the Spectrophotometer every 6 months. The calibration may be
accomplished by using an energy source with an intense line emission such
as i mercury lamp, or by using a series of glass filters spanning the
measuring range of the Spectrophotometer. Calibration materials are
available commercially and from the National Bureau of Standards. Specific
details on the use of such materials should be supplied by ^he vendor;
general information about calibration techniques can be obtained from
general reference books on analytical chemistry. The wavelength scale
of the Spectrophotometer must read correctly within ^5 nm at all
calibration points; otherwise, the Spectrophotometer shall be repaired
and recalibrated. Once the wavelength scale of the Spectrophotometer is
in proper calibration, use 540 nra as the optimum wavelength for the
«easurement of the absorbance of the standards and samples.
G-7
-------
Alternatively, a scanning procedure may be employee to determine tne
proper measuring wavelengtr.. If the Instrument is a double-beam
spectrophotometer, scan the spectrum between 530 and 550 nm using a
250 ug Cr"*6 standard solution in the sample cell and a blank solution in
The reference cell. If a peak does not occur, the spectrophoTometer is
malfunctioning and should be repaired. When a peak is obtained
within the 530 to 550 nm range, the wavelength at which this peak occurs
shall be the optimum wavelength for the measurement of absorbance of both
the standards and the samples. For a single-beam spectrophotometer. folio*.
the scanning procedure described above, except that the blank and standard
solutions shall be scanned separately. The optimum wavelength shall be
the wavelength at which the maximum difference in absorbance between the
standard and the blank occurs.
6.2.2 Determination of Spectrophotometer Calibration Factor Kc. Add
0.0 ml. 10 ml. 20 ml, 30 ml. and 50 ml of the working standard solution
(1 ml « 5 ug Cr*^) TO a series of five 100-ml volumetric "flasks. Analyze
these calibration standards as in Section 5.7.1. This calibration
procedure must be repeated on each day that samples are analyzed.
Calculate the specrrophotometer calibration factor as follows:
K -inn V 2A2*3A3 *A4 ^ ^
c — 21
G-8
-------
Where:
Kc = Calioration factor.
Aj * Absorbance of the 50 Cr*° standard.
A2 * Absorbance of tne 100 Cr*6 standard.
A3 «= Absorbance of the 150 Cr*6 standard.
A4 « Absorbance of the 250 Cr*6 standard.
7. Emission Calculations.
Carry out the calculations, retaining at least one extra decimal
figure beyond that of the acquired data.,. Round off figures after final
calculations.
7.1 Total Cr"*"6 in Sample. Calculate m. the total -»g Cr+6 in each
sample, as follows:
m = Kc 2AF Eq. G -3
Where:
2 « Factor to correct 50 ml aliquot analyzed to 100 ml "total sample.
A = Absorbance of sample.
F « Dilution factor (required only if sample dilution was needed to
reduce the absorbance into the range of calibration).
7.2 Average Dry Gas Meter Temperature and Average Orifice
Pressure Drop. Same as Method 5. Section 6.2.
7.3 Dry Gas Volume. Volume of Water Vapor, Moisture Content. Same
as Method 5, Sections 6.3, 6.4, and 6.5, respectively.
G-9
-------
7.< Cr* Emission Concentration. Calculate cs (g/dscm). the Cr*6
concentration in the stack gas. cry basis, corrected to standard
conditions, as follows:
Cs - (0.001 g/mg)(m/Vm(sld)) Eq. G-4
7.5 Isokinetic Variation. Acceptable Results. Same as Method 5.
Sections 6.11 and 6.12. respectively.
8. Bibliography.
1. Test Methods for Evaluating Solid Waste. U.S. Environmental
Protection Agency. SW-846. 2nd Edition. July 1982.
2. Cox. X.B., R.W. Linton. F.E. Butler. Determination of Chromium
Speciation in Environmental Particles - A Multitechnique Study of
Ferrochrome Smelter Dust. Accepted for publication in Environmental
Science and Technology.
2. Same ^s Method 5. Citations 2 to 5 and 7 of Section 7.
G-10
-------
METHOD 3050
ACID DIGESTION OF SLUDGES
i-0 Scope and Application
1.1 Method 3050 1s an add digestion procedure used to prepare sludge-
type and soil samples for analysis by flame or furnace atomic absorption
spectroscopy (AAS) or by Inductively coupled argon plasma spectroscopy (ICP).
Samples prepared by Method 3050 may be analyzed by AAS or ICP for the
following metals:
Antimony Lead
Arsenic Nickel
Barium Selenium
Beryllium Silver
Cadmium Thallium
Chromium Z1nc
Copper
1.2 Method 3050 may also be applicable to the analysis of other metals
in sludge-type samples. However, prior to using this method for other
metals, it must be evaluated using the specific metal and matrix.
2-° Summary of Method
2.1 A dried and pulverized sample is digested 1n nitric add
and hydrogen peroxide. The digestate 1s then refluxed with either nitric
acid or hydrochloric acid. Hydrochloric add is used as the final reflux
acid for the furnace analysis of Sb or the flame analysis of Sb. Be, Cd. Cr.
Cu. Pb, Hi. and Zn. Nitric acid is employed as the final reflux add for
the furnace analysis of As. Be. Cd. Cr. Cu. Pb. N1. Se. Ag, Tl. and Zn or the
flame analysis of Ag and Tl.
3.0 Interferences
3.1 Sludge samples can contain diverse matrix types, "each of which may
present Us own analytical challenge. Spiked samples and any relevant
i!!ud!r^ref€rence mater1*1 should be processed to aid In determining whether
Method 3050 1s applicable to a given waste. Nondestructive techniques such as
neutron activation analysis may also be helpful 1n evaluating the applicabil-
ity of this digestion method.
4-0 Apparatus and Materials
4.1 125-wl conical Phillips' beakers.
4.2 Watch glasses. ., ,..
\j~ j. j.
-------
2 / WORKUP TECHNIQUES - Inorganic
4.3 Drying ovens that can be maintained at 30* C.
4.4 Thermometer that covers range of 0" to 200* C.
4.5 Whatman No. 42 filter paper or equivalent.
for imri Waef 93: Watef Sh°uld be
level 5of imouHt^fedrJ1tr1C *?d: *1d Sh°uld be anal*2ed to mn
blank correct ""Purities are detected, all analyses should be
mine evelmnriM h*dr^h!orl"c."^ Acid should be analyzed to deter-
blank correctedT impurities are detected, all analyses should be
mDurP<:f Sh°uld be anal^zed to Determine
blank corrected ^"ties are detected, all analyses should be
6*° ^'"P'e Collection. Preservation, and Handling
mUSt ha*
and df
-------
3050 / 3
7.3 After the second reflux step has been completed and the sample
has cooled, add 2 ml of Type II water and 3 ml of 30% hydrogen peroxide (H^
Return the beaker to the hot plate for wanning to start the peroxide reaction
Care must be taken to ensure that losses do not occur due to excessively
vigorous effervescence. Heat until effervescence subsides, and cool the
beaker.
7.4 Continue to add 30% ^2 in 1-ml aliquots with warming until the
effervescence is minimal or until the general sample appearance is unchanged.
(NOTE: Oo not add more than a total of 10 ml 30% H202-)
7.5 If the sample is being prepared for the furnace analysis of Ag and
Sb or direct aspiration analysis of Ag, Sb, Be, Cd, Cr, Cu, Pb, Ni , Tl , and
Zn, add 5 ml of 1:1 HC1 and 10 ml of Type II water, return the covered beaker
to the hot plate, and heat for an additional 10 min. After cooling, filter
through Whatman No. 42 filter paper (or equivalent) and dilute to 100 ml with
Type II water (or centrifuge the sample). The diluted sample has an approximate
acid concentration of 2.5% (v/v) HC1 and 5% (v/v) HN03 and is now ready for
analysis.
7.6 If the sample is being prepared for the furnace analysis of As, Be,
Cd, Cr, Cu, Pb, Ni , Se, Tl , and Zn, continue heating the acid-peroxide
digestate until the volume has been reduced to approximately 2 ml, add 10 ml
of Type II water, and warm the mixture. After cooling, filter through
Whatman No. 42 filter paper (or equivalent) and dilute to 100 ml with Type II
water (or centrifuge the sample). The diluted digestate solution contains
approximately 2% (v/v) HN03. For analysis, withdraw aliquots of appropriate
volume, add any required reagent or matrix modifier, and analyze by method of
standard additions.
8.0 Quality Control
8.1 For each group of samples processed, procedural blanks (Type II
water and reagents) should be carried throughout the entire sample-preparation
and analytical process. These blanks will be useful in determining if
samples are being contaminated.
8.2 Duplicate samples should be processed on a routine basis. Duplicate
samples will be used to determine precision. The sample load will dictate
the frequency, but 10% is recommended .
8.3 Spiked samples or standard reference materials should be employed
to determine accuracy. A spiked sample should be Included with each group of
samples processed and whenever a new sample matrix Is being analyzed.
8.4 The concentration of all calibration standards should be verified
against a quality control check sample obtained from an outside source.
8.5 The method of standard addition shall be used for the analysis
of all EP extracts and whenever a new sample matrix is being analyzed.
G-13
-------
APPENDIX H
Process Data Monitored During Tests
H-l
-------
CALCULATION OF TOTAL CURRENT IN AMPERE-HOURS FOR RUN NO. 1
No. of plating cycles during test: 207-69 = 138
No. of bumpers plated during test: 1,162-119 = 1,043
A. Plating Cycle
Average current, 20,507 A per cycle
Average plating time, 2.00 min
1. Average Ampere-Hours for One Plating Cycle
Ah/cycle = (average current)*(plating time)
684 Ah/cycle = (20,507 amperes/cycle)*(2.00 min)*(l h/60 min)
2. Average Ampere-Hours for all Plating Cycles
Ah = (Ah/cycle)*(No. of cycles)
94,392 Ah = (684 Ah/cycle)*(138 cycles)
B. Activation Cycle
Average current, 5,217 A per cycle
Average activation time, 15 s
1. Average Ampere-hours for One Activation Cycle
Ah/cycle = (average current)*(activation time)
21.74 Ah/cycle = (5,217 amperes/cycle)*(15 s)*(l h/3,600 s)
2. Average Ampere-Hours for all Activation Cycles
Ah = (Ah/cycle)*(No. of cycles)
3,000 Ah = (21.74 Ah/cycle)*(138 cycles)
C. Total Ampere-Hours for Run No. 1
Ah = (Ah for plating cycles)+(Ah for activation cycles)
97,392 Ah = (94,392 Ah)-i-(3,000 Ah)
H-2
-------
CALCULATION OF TOTAL CURRENT IN AMPERE-HOURS FOR RUN NO. 2
No. of plating cycles during test: 144-5 = 139 •
No. of bumpers plated during test: 2,890-1,747 = 1,143
A. Plating Cycle
Average current, 21,697 A per cycle
Average plating time, 2.00 min
1. Average Ampere-Hours for One Plating Cycle
Ah/cycle = (average current/cycle)*(plating time)
723 Ah/cycle = (21,697 amperes/cycle)*(2.00 min)*(l h/60 min)
2. Average Ampere-Hours all for Plating Cycles
Ah = (Ah/cycle)*(No. of cycles)
100,497 Ah = (723 Ah/cycle)*(139 cycles)
B. Activation Cycle
Average current, 5,217 A per cycle
Average activation time, 15 s
1. Average Ampere-Hours for One Activation Cycle
Ah/cycle = (average current)*(activation time)
21.74 Ah/cycle = (5,217 amperes/cycle)*(15 s)*(l h/3,600 s)
2. Average Ampere-Hours for all Activation Cycles
Ah = (Ah/cycle)*(No. of cycles)
3,022 Ah = (21.74 Ah/cycle)*(139 cycles)
C. Total Ampere-Hours for Run No. 2
Ah = (Ah for plating cycles)-»-(Ah for activation cycles)
103,519 Ah = (100,497 Ah)+(3,022 Ah)
H-3
-------
CALCULATION OF TOTAL CURRENT IN AMPERE-HOURS FOR RUN NO. 3
No. of plating cycles during test: (97-55)-(110-97)+(210-119) = 120
No. of bumpers plated during test: (315-0)-(382-315)-(1191-455) = 984
A. Plating Cycle
Average current, 21,747 A per cycle
Average plating time, 2.00 min
1. Average Ampere-Hours for One Plating Cycle
Ah/cycle = (average current)*(plating time)
725 Ah/cycle = (21,747 amperes/cycle)*(2.00 min)*(l h/60 min)
2. Average Ampere-Hours for all Plating Cycles During Run No. 3
Ah = (Ah/cycle)*(No. of cycles)
87,000 Ah = (725 Ah/cycle)*(120 cycles)
B. Activation Cycle
Average current, 5,217 A per cycle
Average activation time, 15 s
1. Average Ampere-Hours for One Activation Cycle
Ah/cycle = (average current)*(activation time)
21.74 Ah/cycle = (5,217 amperes/cycle)*(15 s)*(l h/3,600 s)
2. Average Ampere-Hours for all Activation Cycles
Ah = (Ah/cycle)*(No. of cycles)
2,609 Ah = (21.74 Ah/cycle)*(120 cycles)
C. Total Ampere-Hours for Run No. 3
Ah = (Ah for plating cycles)+(Ah for activation cycles)
89,609 Ah = (87,000 Ah)+(2,609 Ah)
H-.4
-------
SOURCE SAMPLING PROCESS DATA SHEET
Place: Delco Products Division
General Motors Corporation
Livonia, Michigan
Date: March 18, 1987
Test run No.: 1
Counter Readings
Test start
Test stop
Time,
24-h clock
09:35
09:40
09:45
09:50
09:55
10:00
10:05
10:10
10:15
10:20
10:25
10:30
10:35
10:40
10:45
10:50
time:
time:
Tank
eel 1
No.
1
2
3
1
2
3
2
3
1
2
1
2
2
3
3
1
3
1
2
1
2
2
3
1
3
1
2
2
3
1
2
09:34
12:59
Temp., *F
128
128
128
128
128
128
128
128
128
128
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
No. of bumpers (start): 119
No. of bumpers (end): 1,162
No. of plating cycles (start): 69
No. of plating cycles (end): 207
Operating
voltage,
volts
26.0
24.0
26.0
17.5
20.0
24.0
19.0
22.5
21.0
19.5
20.5
21.0
22.0
22.5
24.0
21.5
24.5
22.0
19.5
22.5
21.5
21.0
22.0
22.0
22.5
22.5
20.0
20.0
23.0
23.5
20.0
Operating
current,
amperes Notes
19,000
20,000
20,000
19,500
19,400
21,000
20,750 Grab samples of plating
20,250 solution taken at 09:50
21,750
22,000
21,000
20,500
19,600
19.250
19,000
22,000
19,000
21,750 Plating cycle: 2.0 min
20,500 Activation cycle: 15 s
20,500
19,400
18,800
20,750
21 ,250
18,750
21 ,250
19,800
19,800
19,000
20,750 Plating cycle: 2.08 min
19,050 Activation cycle: 15 s
(continued)
H-.5
-------
SOURCE SAMPLING PROCESS DATA SHEET (continued)
Time,
24-h clock
10:55
11:00
11:05
11:10
11:15
11:20
11:25
11:30
11:35
11:40
11:45
11:50
11:55
12:15
12:20
12:25
12:30
12:35
12:40
12:45
Tank
eel 1
No.
1
2
1
2
2
3
1
2
1
2
2
3
2
3
3
2
3
1
1
3
1
2
1
2
1
2
2
3
1
3
2
3
1
1
3
1
3
Temp., *F
130
130
130
130
130
130
130
130
130
130
130
130
132
132
132
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
Operating
voltage,
volts
24.5
20.5
23.5
20.5
20.0
22.0
24.0
20.5
23.5
19.5
21.0
25.0
22.5
23.5
24.0
21.0
25.0
22.5
23.5
23.5
23.5
22.0
22.5
20.0
22.0
20.0
20.5
23.5
23.5
25.5
21.0
23.5
24.0
22.0
24.5
22.0
24.5
Operating
current,
amperes
20,300
19,200
20,100
21 ,250
20,250
18,750
20,800
19,400
20,500
20,000
20,000
19,750
20,250
20,250
21,500
21 ,250
19,800
21,000
20,500
20,000
21 ,250
21,500
21,500
20,050
22,750
21 ,250
21,250
20,250
22,000
21,750
20,250
24,000
21 ,250
20,750
22,000
20,500
21,500
Notes
Grab samples of plating
solution taken at 1 1 :
10
Plating cycle: 2.08 min
Activation cycle: 15 s
Stopped testing: 11:59
(electrical repair)
Started testing: 12:12
Plating cycle: 2.00 min
Activation cycle: 15 s
Grab samples of plating
solution taken at 12:
40
(continueoT
H-6
-------
SOURCE SAMPLING PROCESS DATA SHEET (continued)
Time,
24-h clock
12:50
12:55
13:00
Tank
. cell
No.
1
2
2
3
1
3
Temp . , " F
130
130
130
130
130
130
Operating
voltage,
volts
23.0
21.0
21.0
24.5
23.5
22.5
Operating
current,
amperes
19,600
19,200
22,000
19,500
20,000
23,250
Notes
Plating cycle:
Activation cycle
Testing stopped
2.00 min
: 15 s
at 12:59
Average
130-
22.3
20,507
H-7
-------
SOURCE SAMPLING PROCESS DATA SHEET
Place: Delco Products Division
General Motors Corporation
Livonia, Michigan
Date: March 18, 1987
Test
Test
Test
run No.:
start time:
stop time:
Tank
T i me , ce 1 1
24-h clock No.
14:35
14:40
15:35
15:40
15:45
15:50
15:55
16:00
16:05
16:10
16:15
16:20
16:25
16:35
i
2
2
1
2
1
2
1
3
1
2
2
3
1
2
1
2
2
3
1
1
2
2
3
1
2
2
14:37
18:51
Temp . , * F
134
134
134
128
128
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
Counter
No. of
No. of
No. of
No. of
Operating
voltage,
volts
22.5
20.8
20.0
22.0
20.0
22.5
19.5
22.0
23.0
20.5
21.0
19.0
23.5
22.5
20.5
22.5
20.5
20.5
23.5
23.5
24.0
21.0
21.0
24.0
23.0
20.0
Readings
bumpers (start): 1,747
bumpers (end): 2,890
plating cycles (start): 5
plating cycles (end): 144
Operating
current,
amperes Notes
21,250 Started testing: 14:37
20,500
22,500 Stopped testing: 14:45
(Blown fuse)
Started testing: 15:36
21,250
21,750
24,250
22,750
23,000 Grab samples of plating
22,750 solution taken at 15:
22,000
21,250
-
45
22,500 Plating cycle: 2.00 min
20,250 Activation cycle: 15 s at
5,000 amps, 10 volts
24,500
21,000
21,000
21,250
22,000
21,250
22,250 Activation cycle: 15 s
5,000 amps, 10 volts
21,000
20,250
21,250 Stopped testing: 16:31
(Racking 1 ine down)
19,600 Started testing: 16:34
20,500 Activation cycle: 15 s
21,500 5,000 amps, 10 volts
at
at
(continued)
H-8
-------
SOURCE SAMPLING PROCESS DATA SHEET (continued)
Time.
24-h clock
16:40
16:45
16:50
16:55
17:00
17:05
Tank
eel 1
No.
2
3
2
3
1
3
1
3
2
3
1
Temp . , * F
130
130
130
130
130
130
130
130
130
130
130
Operating
voltage,
volts
21.5
23.5
21.0
25.5
23.5
25.5
23.5
25.0
20.0
24.0
23.5
Operating
current,
amperes
20,250
20,300
19,000
20,350
19,600
20,500
20,750
21,500
21,000
20,250
19,600
Notes
Plating cycle:
Activation cycle
Stopped testing:
2.00 min
: 15 s
17:10
(Electrical repair)
17:20
17:25
17:30
17:35
17:40
17:45
17:50
17:55
18:00
18:05
18:10
18:15
18:20
18:25
3
1
3
2
3
3
1
3
1
2
1
2
2
3
1
3
1
2
2
3
1
3
1
2
2
3
3
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
22.0
21.0
24.5
19.5
23.5
23.5
22.5
24.5
24.5
20.5
20.5
20.0
20.5
22.5
24.0
21.5
22.0
19.0
20.0
23.0
21.5
24.0
22.5
19.0
21.5
23.5
23.5
21,000
19,000
19,600
20,500
22,500
24,000
19,000
21,750
19,800
18,800
18,200
23,750
20,750
23,250
22,250
23,500
23,750
23,500
21 ,250
23,500
23,250
22,750
24,500
23,000
20,500
23,750
24,750
Started testing:
-.
Grab samples of
solution taken
17:21
plating
at 17:35
Plating cycle: 2.00 min
Activation cycle
: 15 s
(continued)
H-9
-------
SOURCE SAMPLING PROCESS DATA SHEET (continued)
Time,
24-h clock
18:30
18:35
18:40
18:45
18:50
Tank
cell
No.
1
2
2
3
2
3
1
2
2
3
Temp., *F
130
130
130
130
130
130
130
130
130
130
Operating
voltage,
volts
22.5
19.0
21.0
22.5
21.5
25.0
22.0
20.5
20.0
24.0
Operating
current,
amperes
22,250
23,500
22,000
23,500
23,250
21,750
24,250
20,200
24,000
22,250
Notes
Grab samples of
solution taken
Plating cycle:
Activation cycle
Testing stopped
plat! ng
at 18:30
2.00 min
: 15 s
at 18:51
Average
130
22.0
21,697
H-10
-------
SOURCE SAMPLING PROCESS DATA SHEET
Place: Delco Products Division
General Motors Corporation
Livonia, Michigan
Date: March 19, 1987
Test run No.: 3
Counter Readings
Test start
Test stop
Time,
24-h clock
09:45
09:50
09:55
10:00
10:05
10:10
10:15
10:20
10:25
10:35
10:45
13:35
13:40
time:
time:
Tank
cell
No.
1
3
1
2
2
3
2
3
1
2
3
1
3
1
2
2
3
1
3
1
3
1
3
1
2
I
2
09:45
15:49
Temp., 'P
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
130
No. of bumpers (start): 0
No. of bumpers (end): 1,191
No. of plating cycles (start): 59
No. of plating cycles (end): 210
Operating
voltage,
volts
23.5
24.5
21.0
17.5
21.0
23.5
20.0
23.0
22.0
20.0
23.5
23.5
21.5
24.0
20.0
21.0
24.0
23.0
24.0
24.0
23.5
23.5
23.5
23.0
20.0
25.0
22.0
Operating
current,
amperes
19,600
22,000
22,500
19,800
22,000
22,500
24,500
21,750
23,500
23,000
23,500
23,500
22,000
23,000
21,500
22,500
20,550
21,750
21,000
20,250
21,000
21,750
21,750
22,500
21,500
21 ,750
19,850
Notes
Started testing: 09:45
Activation cycle: 15 s at
5,500 amps, 9.5 volts
Grab samples of plating
solution taken at 10:00
Plating cycle: 2.00 min
Activation cycle: 15 s at
5,800 amps, 10.0 volts
Plating cycle: 2.00 min
Activation cycle: 15 s at
5,000 amps
Stopped testing: 10:31
(Conveyor down)
Started testing: 10:35
Stopped testing: 10:41
(Conveyor down)
Started testing: 10:46
Stopped testing: 10:51
(Conveyor down)
Started testing: 13:34
Mo. of bumpers (stop): 315
No. of cycles (stop): 97
No. of bumpers (stop): 455
No of cycles (start): 119
(continued)
H-ll
-------
SOURCE SAMPLING PROCESS DATA SHEET (continued)
Time,
24-h clock
13:45
13:50
13:55
14:00
14:05
14:10
14:15
14:20
14:25
14:30
14:35
14:40
14:45
14:50
14:55
15:05
15:10
15:15
15:20
Tank
cell
No.
2
3
2
3
1
3
1
2
1
2
1
2
2
3
3
2
1
2
1
2
2
3
1
3
1
2
1
3
1
3
1
3
2
3
1
3
Temp . , ' F
130
130
130
130
130
130
130
130
130
130
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
131
132
132
132
132
Operating
voltage,
volts
22.0
23.0
21.5
25.0
22.5
24.0
23.0
21.0
23.5
21.5
24.0
21.0
20.5
23.5
26.5
23.0
25.0
21.0
23.5
20.5
21.0
24.0
24.0
24.0
24.0
21.0
21.5
24.0
23.5
23.5
23.0
24.0
21.5
23.5
23.0
24.5
Operating
current,
amperes Notes
22,000
21,000
23,500
21,750
21 ,050
20,750
21,750
20,750
23,500
20,300
20,750
20,500
22,500
20,250
21,500 Stopped testing: 14:20
(electrical repair)
Started testing: 14:21
21,750 Grab samples of plating
solution taken at 14:20
23,250
21,750
21,500
22,250
22,750
19,800
19,950
20,500
21,500
20,750
22,250
21,000
20,050
20,750
20,550
19,400
21 ,750
20,750
21 ,250
22,500
(continued)
H-12
-------
SOURCE SAMPLING PROCESS DATA SHEET (continued)
Time,
24-h clock
15:25
15:30
15:35
15:40
15:45
Tank
eel 1
No.
2
3
2
3
1
3
1
3
2
3
Temp., *F
132
132
132
132
132
132
133
133
133
133
Operating
voltage,
volts
21.5
24.0
22.5
26.0
24.0
25.0
25.0
25.0
20.5
23.5
Operating
current,
amperes Notes
23,500
21,750
22,750 Grab samples of plating
21,500 solution taken at 15:30
20,050
21,750
23,000
22,750
24,250 Stopped testing: 15:49
20,250
Average
131
22.8
21,747
H-13
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