OFFICE OF ENFORCEMENT
E PA-330/2-7 8-01 8
SO 2 Emission Testing
o
at the
Bunker Hill Company
Kellogg, Idaho
(MAY 1 2-26,1 978)
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
DENVER, COLORADO
AND
REGION X .
OCTOBER 1978
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Environmental Protection Agency
Office of Enforcement
EPA-330/2-78-018
S02 EMISSION TESTING
AT THE
BUNKER HILL COMPANY
KELLOGG, IDAHO
[May 12-26, 1978]
Timothy Osag
October 1978
National Enforcement Investigations Center - Denver
and
Region X - Seattle
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ACKNOWLEDGMENTS
The author wishes to thank EPA Region X and the members of
NEIC's Field Operations Branch, Chemistry Branch, and the Word
Processing Section of the Technical Services Branch for their
assistance with the Bunker Hill study report.
Special thanks to Ed Struzeski, Paul dePercin, Utah Hardy,
and Dick Ross for their contributions.
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CONTENTS
I. INTRODUCTION 1
II. SUMMARY AND CONCLUSIONS 3
III. PROCESS AND S02 EMISSION SOURCE DESCRIPTION 8
LEAD SMELTER 8
ZINC PLANT 11
IV. TESTING AND PROCESS OBSERVATION PROCEDURES 15
NEIC SAMPLING METHODOLOGY 15
NEIC SAMPLING LOCATIONS 21
COMPANY SAMPLING METHODOLOGY AND LOCATIONS 28
PROCESS OBSERVATION PROCEDURES 30
V. TEST RESULTS 33
SURVEY DATA 33
COMPARISON OF NEIC AND COMPANY DATA 46
VI. PROCESS EVALUATION 49
REFERENCES 50
APPENDICES
A Request for Sampling Site Modifications
B Project Plan and Field Modifications to Plan
C Sampling Train Description
D Chain-of-Custody
E TECO Analyzer Description
F Calibration Data
G Raw Data Sheets and Calculations - separately bound,
EPA-330/2-78-018-B
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TABLES
1 Summary of Method 8, S02 Data, Acid Plant 1 34
2 Summary of Method 8, S02 Data, Acid Plant 2 34
3 Summary of Method 8, S02 Data> Ac1d p,ant 3 35
4 Summary of Method 8, S02 Data, Sinter Machine Weak Stream ... 35
5 Summary of TECO, S02 Data 37
6 Comparison of Method 8 and TECO, S02 Data, Acid Plant 1 .... 38
7 Comparison of Method 8 and TECO, S02 Data, Acid Plant 2 .... 38
8 Comparison of Method 8 and TECO, S02 Data, Acid Plant 3 .... 39
9 Comparison of Method 8 and TECO, S02 Dat3) $inter Machine
Weak Stream 39
10 Evaluation of TECO Performance 40
11 Summary of Adjusted TECO, S02 Data 42
12 Six-Hour Average S02 Concentrations, Acid Plants 1 thru 3 ... 43
13 Summary of Gas Stream Parameters 45
14 Comparison of NEIC and Company Flow Data 47
15 Comparison of Adjusted TECO and Reich Test, S02 Data
Acid Plants 1 thru 3 48
FIGURES
1 Simplified Process Flow Sheet of Lead Smelter 9
2 Simplified Process Flow Sheet of Zinc Plant 12
3 Sampling and Dilution System for Continuous Monitor 18
4 Sampling Locations at Acid Plant 1 22
5 Sampling Locations at Acid Plant 2 24
6 Sampling Location at Acid Plant 3 26
7 Sampling Location at Sinter Machine Weak S02 Stream 27
8 Sampling Location at Blast Furnace 1 29
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I. INTRODUCTION
The Bunker Hill Company, a subsidiary of Gulf Resources, Incor-
porated, operates a lead smelter and zinc plant with annual production
capacities of 127,000 and 100,000 m. tons (140,000 and 110,000 tons),
respectively, at Kellogg, Idaho. On November 19, 1975, Region X of
the Environmental Protection Agency (EPA) disapproved Regulation "S"
of Idaho's State Implementation Plan (SIP), which limited sulfur diox-
ide (S02) emissions from the Bunker Hill complex and substituted a
replacement regulation1. The replacement regulation established S02
concentration limits (6-hour averages) on the acid plants and the
lead smelter main stack of 2,600 and 2,000 ppm, respectively. In
addition, the regulation established a 7-day emission limitation of
617 m. tons (680 tons) of S02 from the entire complex. Compliance
with the concentration limits was to be determined either by continu-
ous measurement systems or Method 82. The continuous monitoring
systems were required to meet performance specifications delineated
in Appendix D of 40 CFR 523.
The Bunker Hill Company challenged the disapproval of Regulation
"S" and substitution of the above limitations with the result that
the U.S. Court of Appeals for the Ninth Circuit remanded the replace-
ment regulation to EPA for further consideration of its technological
feasibility. Region X subsequently requested that the National En-
forcement Investigations Center (NEIC) aid in the remand by conducting
tests to determine S02 concentrations and flow rates at the following
locations [Figures 1 and 2], which are considered the major sources
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2
of S02 emissions from the Bunker Hill complex:
1. Tailgas from Acid Plant 1 (Stations 48901 and 48907)
2. Tailgas from Acid Plant 2 (Stations 48902 and 48903)
3. Tailgas from Acid Plant 3 (Station 48904)
4. Sinter Machine weak stream (Station 48905)
5. Blast Furnace exhaust stream (Station 48906)*
Reconnaissance inspections of the Bunker Hill complex were con-
ducted by NEIC during December 12 and 13, 1977, and March 27 to 30,
1978, to evaluate sampling sites and to identify process data that
would be collected in conjunction with testing. Region X subsequently
informed the Company of necessary sampling site modifications and
process data requirements [Appendix A]. An additional visit to the
plant was made by NEIC on May 3, 1978 to verify completion of the
requested site modifications.
Sampling at Bunker Hill commenced May 12 and ended May 26, 1978.
With few exceptions, all measurements were conducted according to the
procedures detailed in the Project Plan [Appendix B]. Sulfur dioxide
concentrations were measured using both Method 8 and a Thermo Electron
Corporation (TEC0) pulsed-fluorescence analyzer. Only TEC0 data were
collected at the blast furnace because of the adverse working environ-
ment at that location. Flow rates were measured using Method 22 with
traversing according to Method l2.
* Bunker Hill has two blast furnaces, but operate only 1 at a time.
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II. SUMMARY AND CONCLUSIONS
From May 12 to May 26, the National Enforcement Investigations
Center (NEIC) measured gas stream flow rates and sulfur dioxide (S02)
concentrations at selected sites within the Bunker Hill lead smelter
and zinc plant at Kellogg, Idaho. During this time, the lead smelter
was operating near capacity, while the zinc plant was operating at
about 70% of capacity. Operating conditions at both the smelter and
zinc plant were reported to be normal; no unusual conditions (upsets
or malfunctions) occurred which would have greatly affected S02 emis-
sions.
Gas stream velocities were measured intermittently using Method 2
and traversing according to Method 1. Based on these velocities
and the measured moisture content of the gas streams, the following
gas flows were calculated for the outlets of the three acid plants
and the Sinter Machine weak stream:
Flow rate (dry @ standard conditions)*
m3 (ft3)/min
Location
Average
Range
Acid Plant 1
Acid Plant 2
Acid Plant 3
444 (15,700) 393-475 (13,900-16,800)
408 (14,400) 297-450 (10,500-15,900)
659 (23,300) 552-736 (19,500-26,000)
Sinter Machine
weak stream
475 (16,800) 371-594 (13,100-21,000)
* Standard conditions are 20°C (68°F) and 760 mm (29.92 in) Hg.
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4
Sulfur dioxide concentration data were collected at the above
locations by 1-hour Method 8 tests. Results of these tests, which
characterized the average S02 concentrations in the acid plant tailgas
streams and the sinter machine weak stream during the testing program,
are summarized below:
1-hour Average S02
Location Hours Concentration (ppm)
Acid Plant 1 11 3,580
Acid Plant 2 10 2,270
Acid Plant 3 9 1,920
Sinter Machine
weak stream 9 8,700
No method 8 or velocity data were collected at Blast Furnace 1 be-
cause of the adverse working environment caused by fugitive emissions
from the furnace tapping and charging areas.
Sulfur dioxide concentrations were also measured at all loca-
tions using a TEC0 pulsed-fluorescence analyzer. The TEC0 measured
S02 concentrations on a continuous basis for 2 to 9 hours/day and
provided information regarding S02 fluctuations. The performance of
the TEC0 analyzers at the acid plants and sinter machine were eval-
uated against the following performance specifications of 40 CFR 52,
Appendix D:
Accuracy <20% of reference mean value
Calibration Error <5% of calibration gases
Zero Drift (2-hours)* <2% of emission standard
Calibration Drift (2-hours)* <2% of emission standard
Response Time 15 min
* The 2-hour zero and calibration drift specifications were eval-
uated using the proposed emission standard (2,600 ppm) at the
acid plants and the average concentration measured by Method 8
(8,700 ppm) at the Sinter Machine.
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5
These performance specifications were used as the criteria for assess-
ing the quality of the TECO data and its relationship to Method 8.
Because of time restrictions, the purpose of the testing was limited
to characterization of the gas stream S02 concentrations and not cer-
tification of the TECO analyzer. Only those specifications pertaining
to data quality — accuracy, calibration error, zero and calibration
drift, and response time -- were, therefore, addressed. A condition-
ing period for the instrument was not provided and the 168-hour opera-
tional period specification was not addressed because these require-
ments measured instrument durability and not data quality. Because
the monitors were only operated for periods of 8 to 10 hours at a
time, the 24-hour drift specifications were also not addressed.
The TECO did satisfy the zero drift and response time specifi-
cations at all locations. The TECO was also able to meet the accu-
t racy specifications of ±20% at Acid Plant 3, but not at the other lo-
cations. The analyzer was unable to consistently meet the calibration
error and calibration drift specifications; i.e., the calibration
error specification was satisfied at two of the four locations.
The failure of the TECO analyzer to consistently meet the accu-
racy specification prevents the unqualified use of these data. How-
ever, for the purpose of additional data analysis, the Method 8/TECO
comparisons can be used to bring the TECO data into closer agreement
with the Method 8 results. For example, the average S02 concentra-
tions measured by Method 8 at Acid Plant 1 (3,220 ppm) was 15% greater
than the average concentration measured by the TECO (2,800 ppm) during
nine hours of concurrent sampling. The TECO data was, therefore, multi-
plied by 1.15 which, on the average, brings it into closer agreement
with the Method 8 results. Similar adjustments were also made on the
data for Acid Plants 2 and 3 and the Sinter Machine weak stream using
the r'esults of the concurrent Method 8/TECO sampling conducted at
these locations.
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6
TECO data, both unadjusted and adjusted, are summarized below:
Hours of Average S09 Concentration (ppm)
Location Data Unadjusted Adjusted
Acid Plant 1
27
2,720
3,130
Acid Plant 2
29
2,800
2,100
Acid Plant 3
35
1,690
1,770
Sinter Machine
weak stream
29.5
6,970
8,080
Blast Furnace 1
6
1,840
a Since no Method 8 tests were conducted at the Blast Furnace 1
the TECO results could not be adjusted.
Adjusted TECO data were interpreted in terms of running 6-hour
averages for those days during which at least 6 hours of concentration
data were obtained. Six-hour average S02 concentrations in excess of
the proposed 2,600 ppm limit were measured at Acid Plants 1 and 2 with
maximum 6-hour concentrations of 4,400 and 3,500 ppm, respectively.
The maximum 6-hour average S02 concentration at Acid Plant 3 was 2,080
ppm.
Average S02 emission rates based on NEIC measured flow rates and
adjusted TECO S02 concentration data are listed below:
Average S09 Emission Rate
Location m. tons (tons)/day
Acid Plant 1
5.4
(5.9)
Acid Plant 2
3.3
(3.6)
Acid Plant 3
4.4
(4.9)
Sinter Machine
weak stream
14.8
(16.2)
No emission rate was calculated for the blast furnace because no
gas flow rates were measured for this service.
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7
Company flow data was extracted from the operating logs for Acid
Plants 1 through 3 for the period of May 12 through 25 and the average
for each sampling period was compared (after adjustment for S02 content)
to NEIC-measured flow data for the same period. The comparison in-
dicated that Company flow measurements at Acid Plant 2 averaged approxi-
mately 7.0% low compared to the NEIC data, while Company measurements
at Acid Plants 1 and 3 were higher by 24% and 30%, respectively.
The NEIC flow data were based on average gas velocities measured
using Method 2 and traversing by Method 1 and have an expected accu-
racy of approximately ±10%. The accuracy of Company flow data is
unknown, but the use of single point velocity measurements makes this
data questionable.
Both adjusted TECO data and concurrent Reich test results were
used to calculate a daily average S02 concentration for each acid
plant tailgas stream which reflected a 2 to 11 hour sampling period.
The overall average S02 concentrations, based on TECO and Reich test
results, agreed to within 17% for all three acid plants. Less agree-
ment was noted when the average concentrations for a single day were
considered. No direct comparison was made between Method 8 and Reich
test results because of the difficulty associated with identifying con-
current pairs of data.
Company measured S02 concentrations for the Sinter Machine weak
stream were in wide disagreement with NEIC measurements. During test-
ing at this location from May 13 to 17, the maximum Company measured
S02 concentrations was 3,500 ppm, while the NEIC S02 concentrations
data (adjusted TECO) averaged 8,080 ppm.
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III. PROCESS AND S02 EMISSION SOURCE DESCRIPTION
The Bunker Hill facilities in Kellogg, Idaho, consist of a lead
smelter, a zinc plant, and a phosphoric acid-ammonium phosphate fer-
tilizer plant jointly owned with Stauffer Chemical Company. The phos-
phate fertilizer complex uses some of the sulfuric acid produced by
the three acid plants operated as S02 controls at the lead smelter
and zinc plant. Byproducts recovered from the metallurgical facili-
ties include silver, gold, copper, cadmium, antimony, zinc oxide and
sulfuric acid.
LEAD SMELTER
The Bunker Hill smelter [Figure 1] is a custom smelter; it han-
dles concentrate from several outside sources, as well as those pro-
duced by Company-owned mines. As many as 30 different concentrates
are handled during a year. Production capacity is reported to be
127,000 m. tons (140,000 tons)/year of metallic lead.
Lead concentrates are received primarily by rail and unloaded to
receiving bins. Individual concentrates are then blended and sent to
the bedding plant for preparation of a charge consisting of lead con-
centrates, lime and silica fluxes and recycled materials from the
smelter and zinc plant. After a bed of material has been brought
within specifications, it is removed from the bedding plant, mixed
with recycled sinter, pellitized and sent to a sintering machine.
-The sintering process removes sulfur by oxidation and allows
agglomeration of the charge. In the first stage of sintering, a high
strength (>5%) S02 gas stream is produced which is sent to a sulfuric
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Fluxes and Recycled
Materia 1s
Monarch
rtn nace
Skim
Refined
S11 ver
Fischer Lindberq
Furnace
Dore
Lead Concentrates
Beddinq
Pi les
Sinter
Macln ne
Stronn
SO., Stream
Silver Refinery S.VJkir.
7n
Si lver and
Gold Kettles
Dezincing
Kettle
Me ta111 c
Lead
.Raw material and Product Flow
Air Emissions Flow
Softening
Furnace
= E
O r-
E -*
^ W>
w
c
¦ I.
Electric
Furnace
llaid
Lead
Coke
Dross Kettles
pul1 ion
Blast Turnace
Banhouse
Weak S0? Stream
Station 40905
llo 3
Ac ld Plant
By Pass
..V.tJ t.
Soda Ash
Station 48706
Dust
Slaq
Reverb
Furnare
Coal
7inc Fuminq
T urnare
Electric Furnace
and Cd Plant
topper
Matte
Zinc Oxide
Dust
Cadmium
Sponge to
Zinc Plant
Baqhouse
Oaqhouse
Zinc Fuming
Furnace Stack
T
o
Raqhouse
Figure 1 Simplifled'Process flow Sheet of Lead Smelter
Cunker Hill Company
Kellogg, Idaho
3~
Acid Plant
7ai1 Gas
Station
48904
Baghouse
n
1 Smelter
ti st;vr~C
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10
acid plant (No. 3). The conventional Lurgi updraft sinter machine
used by Bunker Hill also produces a weak (M%) S02 stream which is
blended with the exhaust gases from the blast furnaces and lead re-
fining area, treated for particulate removal (baghouse) and sent to
the smelter stack.
Material leaving the Sinter Machine is separated into coarse and
fine fractions with the oversized material sent to a blast furnace
and the undersized material recycled to the Sinter Machine. Bunker
Hill has two oxygen-enriched blast furnaces (Nos. 1 and 3) but oper-
ates only one at a time. Lead sinter and coke are fed to the blast
furnace in approximately a 9:1 ratio. The lead oxide (PbO) in the
sinter is reduced to an impure metallic form called bullion which is
tapped from the furnace and sent through a series of purification
steps -- drossing, softening, degolding, desilvering and dezincing.
The end product of these refining steps is pure lead. Byproducts
recovered during the purification steps include copper, antimonial
lead (hard lead), silver, and dore metal (silver-gold alloy). The
blast furnace slag is sent to the zinc fuming furnace where it is
treated to recover zinc and lead oxides.
Major process sources of S02 emissions from the lead smelter are
the weak and strong gas streams from the Sinter Machine and the blast,
furnace exhaust. The weak S02 stream from the Sinter Machine, the
blast furnace gas stream and assorted exhaust streams from the lead
refinery are treated for particulate removal in the main baghouse and
then emitted to the atmosphere from the 217 m (715 ft) smelter stack.
The strong S02 stream from the Sinter Machine is treated in a separate
baghouse and is then sent to a 270 m. tons (300 tons)/day single-contact
acid plant (No. 3).
Acid Plant 3 was designed and built by Monsanto and began opera-
tion in 1972. It was designed to handle gas flows up to 910 m3
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11
(32,000 scf)/min with an inlet S02 concentration of 5%. Designed
conversion efficiency for the acid plant was 97.5%. Tailgas from the
acid plant is combined with the gas stream from the main baghouse and
vented to the smelter stack.
Other possible sources of S02 emissions from the lead smelter
include the exhaust from the zinc fuming furnace, the silver refinery,
the lead softening furnace, the tapping floor ventilation and the
dross reverb furnace. The zinc fuming furnace emissions are treated
by a baghouse and then emitted to the atmosphere from the zinc fuming
furnace stack. Exhaust gases from the silver refinery, the lead softening
furnace and the tapping floor are combined with the blast furnace
gases prior to the main baghouse [Figure 1] while the dross reverb
gases are treated in a separate baghouse, and then combined with the
above streams after the main baghouse. All of these streams vent to
the smelter stack.
ZINC PLANT
The zinc plant [Figure 2] treats concentrates purchased from
outside sources as well as concentrates from Company-owned mines.
Production capacity has been reported as 100,000 m. tons (110,000
tons)/year. Zinc concentrates are received primarily by rail and are
unloaded to one of 14 receiving bins at the zinc plant. Each bin
normally holds a separate concentrate. Processing begins with a sul-
furic acid leach of those zinc concentrates (~33% of total) containing
sufficient dolomitic material (magnesium-calcium carbonate) to require
magnesium or calcium removal before zinc recovery. The concentrates
(both treated and untreated) are then dried, blended and sent to the
roasters to remove sulfur prior to the electrolytic reduction process.
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Zn Plant
Stack
Gas Cleaning
System
Acid
Plant
Roaster 5
Baghouse
Station 40901
Station 4B907
Concentrator
Q Scrubber
Boiler Cyclone
Cooler
Leach
Tanks
Screens
Calcine
Station 18003
Residue to
Smelter
Storage
Dryer
Station 40902
ESP
0--D---.P
Roasters Boilers Cyclones
Acid
Plant 2
Gas Cleaning System
Acid Plant Bynass
2nd Stane
Clean Up
3rd Stane
1st Stane
Pun f ication
Solution to
Zn Leach
Cd Residue
Cu Residue
Spent Electrolyte
Cd Residue
Leach Tank
Leach
Tank
Cell
Air Emissions Flow
Raw Materials and
Product Flow
Cd Solution
Spent
Filter
Filter
Cd Stripping
Electrolyte
Cu Resldue
Cd Mel ting
Arsenic Oxide, Copper
Sulfate, Zinc Dust
Zn Alloying and Casting
Zinc Dust, Copper Sulfate
Ski ins and Oross
Recycled
Zinc Dust
Zn Blocks
Zn Anodes
Zn A1loys
Zn Slabs
Figure 2 Simplified Process Flow Sheet of Zinc Plant
Bunker Mill Company ~—»
Kellong , Idaho ^
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13
Bunker Hill has five flash roasters (Nos. 1-5) but reportedly
operates a maximum of four at any one time. Roaster 5 is the largest
with a rated capacity of 320 m. tons (350 tons)/day. Each of Roasters
1-4 has a rated capacity of 110 m. tons (120 tons)/day. Exhaust gases
from the roasters, containing approximately 6% S02, are normally sent
to two sulfuric acid plants (Nos. 1 and 2).
Calcine from the roasters is cooled and then leached with spent
electrolyte from the zinc electrolytic cells. Residue from the leach
tanks is sent to the lead smelter for recovery of the lead, gold and
silver content while the solution, which contains the soluble zinc,
is sent through a series of purification steps.
Purification consists of the sequential addition of arsenic oxide,
copper sulfate and/or zinc dust to the zinc sulfate solution to precipi-
tate cadmium, cobalt, nickel, copper and arsenic impurities. Following
each purification step, the solution is filtered and the filtrates
are either sent to the cadmium plant for recovery of cadmium and copper
or recycled to the first stage of the purification sequence.
The purified solution is pumped to the cell room where zinc metal
is recovered by electrolysis on aluminum cathodes. The cathodes are
removed from the cells, and the zinc is stripped and sent to melting
furnaces for casting.
The most significant process sources of S02 emissions at the
zinc plant are the offgases from the five flash roasters. The gas
stream from Roasters 1-4 are passed through waste heat boilers for
heat recovery, combined and sent to an electrostatic precipitator
(ESP) for particulate removal. The gas stream which exits the ESP is
sent to a wet cleaning system (Peabody scrubber and two mist precipi-
tators), combined with the cleaned gases from Roaster 5 and sent to
Acid Plants 1 and 2, operated in parallel.
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14
The exhaust gases from Roaster 5 undergo treatment similar to
that described for Roasters 1-4; they pass through a waste heat boiler,
a baghouse and a wet gas cleaning system (Peabody scrubber and mist
precipitator) prior to mixing with the gases from the other roasters.
Any of the roaster gas streams can bypass the acid plants on the way
to the main stack.
Acid Plant 1 was installed in 1954 by Monsanto. It is a single-
contact acid plant designed for a flow rate of 620 m3 (24,000 scf)/min
and an inlet S02 concentration of 7.0%. Designed conversion efficiency
at the above operating conditions is 95%. Acid Plant 2, also single-
contact, was designed and built by Chemico and started operation in
1964. The design flow rate and inlet S02 concentration are 710 m3
(25,000 scf)/min and 7.5%, respectively. Designed conversion effi-
ciency is 97.5%. Tailgases from the two acid plants are combined and
sent to the 185 m (610 ft) zinc plant stack. The tailgases can also
be vented to the atmosphere directly from the absorption towers.
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IV. TESTING AND PROCESS OBSERVATION PROCEDURES
A copy of the Project Plan [Appendix B] was provided to the
Bunker Hill Company prior to the time NEIC entered the plant. During
the testing program, Bunker Hill was provided all pilot tube, dry gas
meter and orifice calibration data; span gas concentrations; and
copies of all data collected by NEIC. Aliquots of all Method 8 sam-
ples and blanks were provided to Alsid, Snowden and Associates, a
consulting firm retained by Bunker Hill. Alsid, Snowden and Asso-
ciates was also provided access to all sampling locations an field
laboratories.
NEIC SAMPLING METHODOLOGY
Sulfur dioxide concentrations were measured by both Method 8 and
TECO pulsed-fluorescent analyzers. Method 8 was used to measure S02
concentrations at all locations except Blast Furnace 1. No Method 8
tests were conducted at the blast furnace because of the adverse work
ing environment at this site caused by fugitive emissions from the
tapping and charging areas.
The purposes of the Method 8 testing were to characterize the
S02 concentrations of the gas streams by the reference method and to
provide a measurement of the relative accuracy of the TECO data.
Nine Method 8 tests were required at each site to allow an evaluation
of the relative accuracy of the TECO; that is, the results of the
Method 8 test were compared to the average S02 concentrations meas-
ured by the TECO over the same 1-hour periods.
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16
Since only S02 concentrations were to be measured by the Method
8 tests, it was not necessary to perform isokinetic sampling. Samp-
ling was conducted at a constant rate of approximately 0.014 m3 (0.50
ft3)/min at the center point of the duct.
The Scientific Glass, Inc. Model AP 5000 sampling train [Appen-
dix C] was used for all Method 8 sampling and was arranged as follows:
Stainless steel (316) nozzle
Glass-lined probe
First impinger - Greenburg-Smith with 100 ml of 80%
isopropanol solution
Glass fiber filter (5.1 cm diameter)
Second Impinger - modified Greenburg-Smith with 100 ml of 5%*
hydrogen peroxide solution
Third Impinger - Greenburg-Smith with 100 ml of 5%* hydrogen
peroxide solution
Fourth Impinger - modified Greenburg-Smith with approximately
200 grams of silica gel.
Sample recovery and cleanup was according to the procedure listed
below:
1. All impingers were weighed to determine the amount of moisture
collected, and the contents of Impingers 1 and 4 were then
discarded; as was the 5.1 cm filter.
2. Contents of Impingers 2 and 3 were transferred to a 1,000
ml graduated cylinder. The impingers and all connecting
glassware between the filter holder and the silica gel
(fourth) impinger were washed with deionized distilled
* 15% hydrogen peroxide solution was used at the Sinter Machine
weak stream.
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17
water and this washwater was added to the graduated cylinder.
Deionized distilled water was then added to bring the volume
to 1,000 ml. This sample was transferred to a 1,000 ml
polypropylene container* and the container was sealed.
Following completion of a day's testing, the container was
opened and an aliquot provided to representatives of the
Bunker Hill Company. The container was then resealed, the
liquid level in the container was marked, and the sample
was stored for shipment to Denver.
3. The nozzle, probe, first impinger and all connecting glass-
ware between the probe and the filter were washed with 80%
isopropanol and the washings discharged.
All Method 8 samples were returned to the NEIC laboratories for
analyses according to the procedures described in Method 8. Sample
Chain-of-Custody was maintained at all times and sample blanks were
obtained for the hydrogen peroxide and distilled water used during
the testing [Appendix D]. All peroxide-distilled water samples saved
as blanks were first used as a second wash for Impingers 2 and 3 of
the Method 8 train. As noted previously, NEIC furnished an aliquot of
all samples and blanks to Alsid, Snowden and Associates, a consulting
firm retained by Bunker Hill.
TEC0 analyzers [Appendix E] were also used to measure S02 concen-
trations at all locations. A gas sample was continuously removed
from the duct of interest, the sample was mixed with clean dry air at
a predetermined ratio, and the diluted sample was sent to the analyzer
[Figure 3]. The purpose of diluting the sample prior to analysis was
threefold:
* Two 500 ml containers were used for some samples at acid plants
1 and 2 (Stations 48901 and 48902).
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SS Probe
Teflon
Hanifold
Regulator
Span
Gas
Fi1ter
Rotometer
Rotometer
Fi1ter
Drierite and
Molysieve
Puregas Meatless
Air Dryer used in
place of carbon
and Drierite columns
in second system
Atmos
All Sample Gas Stream Components
are Made of Either Glass or Teflon
Mi xer
Mamfold
To Analyzer
Figure 3 Sampling and Dilution System for Continuous Monitor
Bunker Hi 11 Company
Kellogg, Ida ho
i—•
CO
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19
1. Reduce the moisture content of the gas sent to the analyzer,
thereby lowering the dewpoint and avoiding condensation.
2. Provide a sample which is essentially S02 in the air (i.e.,
^0% C02 and 21% 02) so that the quenching effect* of C02 is
eliminated and that of 02 can be compensated for during
calibration.
3. Bring the S02 concentration of the sample within the upper
limit of the analyzer (5,000 ppm maximum).
O
The TECO analyzer measures the fluorescence excited at the 2100A
(ultraviolet) region of the S02 spectrum. In the absence of interferring
gases (C02 and 02), the fluorescence is linearly proportional to the con-
4
centration of S02. Both carbon dioxide and oxygen reduce the fluorescent
signal by quenching the excited S02 molecule, but this was compensated for
by diluting the sample and using a S02 in air calibration gas.
At the acid plant and Sinter Machine sites, the TECO analyzers were
evaluated against the following performance specification of 40 CFR 52,
Appendix D:
Parameter
Speci fi cation
Accuracy
Calibration Error
Zero Drift (2-hours)a
Calibration Drift (2-hours)'
Response Time
< 20% of reference mean value
< 5% of each (50% and 90% span)
calibration gas mixture
< 2% of emission standard
< 2% of emission standard
15 minutes maximum
a Expressed as sum of absolute mean value plus 95% confidence
interval of a series of tests.
These performance specifications were used as the criteria for assessing
the quality of the TECO data and its relationship to Method 8. Because
of time restrictions, the purpose of the testing was limited to
* Excited S02 molecules can transfer energy to C02 and 02
molecules by collision (quenching), thereby reducing the
intensity of the f1uorescence.
-------
20
characterization of the gas stream S02 concentration and not certi-
fication of the TECO analyzer. Only those specifications pertaining
to data quality -- accuracy, calibration error, zero and calibration
drift, and response time -- were addressed. A conditioning period
for the instrument was not provided, and the 168-hour operational
period specification was not addressed because these requirements
measured instrument durability and not data quality.
The promulgated acid plant emission standard of 2,600 ppm was
used to evaluate 2-hour zero and calibration drift specifications at
the three acid plant sites; 8700 ppm, the average S02 concentration
measured by Method 8, was used for the Sinter Machine weak stream.
Because the monitors were only operated for periods of 8 to 10 hours
at a time, the 24-hour drift specifications were not addressed in the
sampling program.
In conjunction with the Method 8 and continuous S02 monitoring,
gas flow rates were determined throughout the day, initially at ap-
proximately 1-hour and later at 2-hour intervals. Method 2 (using an
isolated S-type pitot tube) with traversing according to Method 1 was
used to measure gas velocities. Temperature measurements were col-
lected with a thermocouple-potentiometer arrangement at the same time
as the velocity measurements.
A gas sample was collected (Method 32, grab) concurrent with the
velocity measurements and analyzed with Fyrite analyzers (approximately
every third sample was analyzed using an Orsat analyzer) for calcula-
tion of gas molecular weight. Moisture contents of the gas streams
were determined from the Method 8 sampling train (weight gain of Im-
pingers 1-4).
All pitot tubes, dry gas meters and orifices used during the
survey were calibrated both prior to the start of the survey and at
its completion [Appendix F]. Thermocouples used to measure stack gas
-------
21
temperatures were checked against ASTM* thermometers prior to the
start of the survey and at its completion. The TECO analyzers were
operated in accordance with the calibration and quality control pro-
cedures of 40 CFR 52, Appendix D. All span gases were analyzed by
Method 62 procedures for S02 concentrations both when the survey began
and at its completion [Appendix F]. The average measured concentration,
which differed from the reported value by as much as 10%, was used
for all calculations. In addition, a span check was performed at
each site using a gas of unknown concentration.
NEIC SAMPLING LOCATIONS
Acid Plant 1 (Stations 48901 and 48907)
Sulfur dioxide concentrations in the tailgas from Acid Plant 1
were measured at a sampling location (48901) in the 91 cm (36 in)
diameter stainless steel duct which connects the absorption tower
with the downcomer to the fiberglass-reinforced plastic (FRP) duct-
work which leads to the stack [Figure 4]. Two 10 cm (4.0 in) diam-
eter ports are located on one side of the duct, with a 0.46 m (1.5
ft) separation between the two ports. The distances between this
sampling location and the nearest upstream and downstream flow dis-
turbances are approximately 11 and 3.3 m (35 and 11 ft), respectively.
The Method 8 train was operated at the upstream port, because of space
limitations, while the TECO sample was collected from the downstream
port. Sulfur dioxide concentrations were measured at the midpoint of
the duct. Station 48901 was not used for velocity measurements be-
cause only one part was available at the Method 8 sampling location.
Velocity measurements were conducted at a sampling site (48907)
in the downcomer section of ducting using two 10 cm (4.0 in) ports,
with a 90° separation, located approximately 1.8 m (6.0 ft) downstream
* American Society for Testing and Materials
-------
Station 48901
Port C
Expansion Joint
From
Absorption
Tower
JX
Port A~^0 o*-Port B"
0 9m
(3 ft)
0 46m
(1.5 ft)
9.1m
(30 ft)
(5 ft)
(11 ft)
Gas
Flow
Side View
Note All ports are 10 cm (4 in) ID with 25 cm (10 in)
flanges Ports B and c at Station 48901 are
90° apart as are Ports A and B at Station 48907.
1,8m
(6 ft)
Station
48907
Port A
3 Port B
2 4m
(8 ft)
Gas
Bypass
Figure 4. Sampling Locations at Acid Plant 1
(Stations 48901 and 48907)
Bunker Mill Company
Kellogg, Idaho
ro
ro
-------
23
and 2.4 m (8 ft) upstream of the nearest flow disturbances. Twenty-
four sample points were used to measure average gas velocity. Although
this site does not satisfy the minimum downstream separation required
by Method 1, results of simultaneous velocity measurements conducted
at Stations 48901* and 48907 showed that, on the average, the velocity
measured at Station 48907 was only 2.9% greater than that measured at
Station 48901. Station 48907 was, therefore, deemed acceptable and
used for all future measurements.
Acid Plant 2 (Stations 48902 and 48903)
A sampling site (48902) is located in the 107 cm (42 in) diam-
eter horizontal stainless steel duct which connects the absorption
tower with the downcomer to the FRP duct [Figure 5]. This site is
similar to the one at Acid Plant 1; two 10 cm (4.0 in) sampling ports
are installed on one side of the duct, with approximately a 0.61 m
(2.0 ft) separation between them. This sampling location is less
than 1.2 m (4.0 ft) downstream of a constriction in the ducting;
therefore, no velocity measurements were collected at this site.
Both ports were used to measure S02 concentrations; a TEC0 was used
to sample the downstream port while a Method 8 train was used at the
upstream port. The Method 8 sampling was done at the upstream part
because of space limitations at the downstream location. Sulfur dioxide
concentrations were measured at the midpoint of the duct.
Two 10 cm (4.0 in) ports with a 90° separation are located in
the downcomer to the FRP duct approximately 7.6 m (25 ft) downstream
of Station 48902. This location (48903) is approximately 6.1 m (20
ft) downstream and 2.4 m (8.5 ft) upstream of the nearest flow dis-
turbances. Twenty-four sample points were used to measure velocity.
* Station 48901 satisfied the requirements of Method 1
-------
24
1.8m
(6 ft)
ITTt
(6 ft)
0.3m
ITT
Station 48902
Absorption
Tower
Spray
Chamber
Ports
Side View
Gas
Flow
(20 ft)
Ports A and B at Station
48903 are 90° apart.
Station 48903
Port A- t CK-Port
Gas 1
Bypass
(8 5 ft)
Figure 5 Sampling Locations at Acid Plant 2
(Stations 48902 and 48903)
Bunker Hill Company
Kellogg, Idaho
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25
Acid Plant 3 (Station 48904)
A sampling site is located in the 140 cm (54 in) diameter FRP
downcomer which connects the outlet from the acid plant to the down-
stream fan [Figure 6]. Two 10 cm (4.0 in) diameter ports (Ports B
and D) are installed on the front side (with respect to the platform)
of the duct, one port 0.61 m (2.0 ft) below the other. Two additional
downstream ports (A and C) are installed at the same level as Port B,
each at 45° to that port.
The sampling location is approximately 3.7 m (12 ft) and 7.6 m
(25 ft), respectively, from the nearest downstream and upstream flow
disturbances. The upstream port (Port D) was used for the TEC0 while
Port B was used for the Method 8 sampling. The two remaining down-
stream ports (Ports A and C) were used for velocity measurements using
24 sample points.
Sinter Machine Weak Stream (Station 48905)
The Sinter Machine weak stream was sampled about 3.0 m (10 ft)
upstream of the point where it connects with the high-velocity flue
leading to the main baghouse [Figure 7]. Two 10 cm (4.0 in) diameter
ports (Ports A and B) are installed on the side and top of the 110 cm
(42 in) diameter duct, about 3.0 m (10 ft) upstream of the connection
with the high-velocity flue. This site is approximately 2.1 m (7.0
ft) and 3.0 m (10 ft), respectively, from the nearest upstream and
downstream disturbances. Port A was used for Method 8 sampling, while
both ports were used for velocity measurements using 28 points. A
third 10 cm port (Port C) is located 0.70 m (2.4 ft) upstream of
Port A. The TEC0 was installed in Port C.
-------
26
From Absorption
Tower
Note All Ports are 10 cm (4 in
with 25 cm (10 in)
Flanges Ports A and B,j
and B and C are 45° /
apart /
Gas
Flow
(25 ft)
Port D
Front View
C\J CO
(2 0 ft)
Ports
Oft)
Gas Bypass
Platform
(12 ft)
(4 5 ft)
To Fan
Duct Support
Ground
Figure 6 Sampling Location at Acid Plant 3 (Station 4C904)
Bunker 111 11 Company
Kellogg, Idaho
-------
Side View
Mote All Ports are 10 cm (4 in) ID with 25 cm (10 in) Flanges.
Ports A and B are 90° Apart
Port B
Port A
Gas Flow
High
Velocity
Port C
From
Sinter
Machine
Figure 7 Sampling Location at Sinter Machine Weak S02 Stream (Station 48905)
Bunker Hill Company
Kellogg, Idaho
no
-------
28
Blast Furnace 1 (Station 48906)
Blast Furnace 1 was sampled in the gooseneck duct which connects
the furnace with the brick flue which leads to the high-velocity flue
[Figure 8]. Five 10 cm (4.0 in) ports are installed on the top of
the duct in a line perpendicular to the duct's axis, with an equal
separation between ports. Sulfur dioxide concentrations were meas-
ured at approximately the middle of the duct using a TECO monitor
installed in the center port. No velocity data was collected at this
site because of the poor working environment.
COMPANY SAMPLING METHODOLOGY AND LOCATIONS
Bunker Hill presently monitors both S02 concentration and gas
flow rate at the following locations:
Smelter main stack
Zinc plant main stack
Inlets to Acid Plants 1 through 3
Roaster 5 exhaust
The instrumentation at the smelter and zinc plant main stacks is
the same; a DuPont Model 460 (UV spectrophotometer) S02 monitor and
an Annubar velocity sensor. Sulfur dioxide concentration and gas
flow are measured at the 53 m (175 ft) level of the 217 m (715 ft)
smelter stack and at the 71 m (200 ft) level of the 185 m (610 ft)
zinc plant stack.
Inlet S02 concentrations to the acid plants are measured between
the drying tower and the blower of each plant by both the Reich test*
(grab sample taken once/2 hrs) and a thermal conductivity monitor
(continuous sample). Flow rates to the acid plants are measured at a
location between the drying tower and the blower using either a pi tot
* The Reich test, using a starch indicator, measures the volume of
gas required to completely react with a known amount of iodide
reagent.
-------
r ront
V1 ew
Side View
Ilote All Ports are 10 cm (4 in) with
25 cm (10 in) Flanges
Ports
From Blast Furnace Hood
Ports
(10 ft)
TTTt)
(25 ft)
Brick Flue
Figure 8 Sampling Location at Blast furnace 1 (Station "8906)
Bunker Hill Company
Kellogg, Idaho
-------
30
tube or pi tot-tube-type device. More specific information regarding
the thermal conductivity monitors and the velocity sensors was re-
quested of the Company, but was not provided. No information was
obtained regarding the flow and SO2 instrumentation at Roaster 5.
Sulfur dioxide concentrations are also measured at the weak and
strong streams off the Sinter Machine and the outlets of the acid
plants. A DuPont Model 400 (UV spectrophotometer) measures the S02
concentration of the Sinter Machine strong stream at two locations;
upstream of the spray chamber preceding the baghouse, and at the out-
let of the No. 6 fan. The weak stream is also measured approximately
3.0 m (12 ft) off the Sinter Machine hood. The DuPont 400 monitors
the three sites on a time-sharing basis, allocating a third to each
site. Concentrations at the outlets of each acid plant are deter-
mined once-per-hour by the Reich test.
PROCESS OBSERVATION PROCEDURES
The NEIC collected the following logs, control sheets, etc., to
characterize the operation of the Sinter Machine, blast furnace, zinc
roasters and acid plants during the testing program:
Lead Smelter
1. Daily Operating Log Sheet (Acid Plant)
2. Sinter Plant Operation Process Control Sheet
3. Sinter Plant Process Control Sheet
4. Main Baghouse Operation Log
5. Lead Refinery Daily Report
6. Blast Furnace Process Control Sheet
7. Blast Furnace Schedule Control Sheet
8. Smelter Bedding Plant Work Sheet
9. Casting and Loading Schedule Control Sheet
-------
31
10. Ore Preparation Schedule Control
11. Strip chart showing inlet S02 concentration at acid plant
12. Circular chart showing inlet gas flow at acid plant
13. Feederman Process Control Sheet
14. Circular chart showing S02 concentrations in gas streams from
Sinter Machine
15. Shift Report, Smelter Division, Hi-Line Department
*
16. Strip chart showing S02 concentration and flow at smelter main stack
Zinc Plant
1. Daily Operating Report, No. 5 Roaster
2. Flash Roaster Daily Report (Roasters 1-4)
3. Daily Operating Log Sheets (Acid Plants No. 1 and 2)
4. Strip charts showing inlet S02 concentrations at acid plants
5. Materials Handling Sheet
6. Electrolytic Zinc Plant Pretreatment Sheet
7. Strip chart showing gas flow from No. 5 Roaster
8. Strip chart showing S02 concentration of exhaust from No. 5 Roaster
9. Strip chart showing S02 concentration and flow at zinc main stack
The Company provided copies of the preceding data only for those
days during which NEIC was actually at a facility; lead smelter data
were provided for the periods May 10 to 18 and May 26, while zinc
plant data were provided for the period of May 20 to 25. All data
were collected and retained by the Company until it was provided to
NEIC in exchange for copies of NEIC test data, normally at the end of
a test period.
During the testing program, an NEIC observer was allowed access
(when accompanied by a designated Company representative) to the
* Strip chart shows S02 concentration and flow for both the smelter
and zinc plant stack.
-------
32
meteorological station and the following process control rooms:
Lead Smelter
1. Sinter Machine
2. Blast Furnace
3. Acid Plant 3
Zinc Plant
1. Acid Plants 1 and 2
2. Roaster 5
'3. Roasters 1-4
Normally, 2 to 3 visits per day were made to the control rooms asso-
ciated with the facility being tested, while one visit was made to
the control rooms at the other facility. During these visits, the
NEIC process observer: 1) reviewed the operating status of the pro-
cess; 2) validated the content of the process control sheets and
operating logs; 3) collected values for parameters not reported on
the standard control sheets; and 4) became familiar with process
operating and record keeping procedures. All questions regarding
process operation, record keeping, etc., were directed to the
Company's designated representative.
-------
V. TEST RESULTS
SURVEY DATA
From 9 to 11 one-hour Method 8 tests [Appendix G] were conducted
at each of the three acid plants and the Sinter Machine weak stream.
The additional tests at Acid Plants 1 and 2* were conducted because
of suspected problems with the TECO analyzer during some Method 8
tests. Results of the Method 8 testing [Tables 1 through 4] are
summarized below:
Method 8 Results
S02 Concentration (ppm)
Location Hours Data Average Range
Acid Plant 1
11
3,580
1,680 -
6,840
Acid Plant 2
10
2,270
990 -
3,750
Acid Plant 3
9
1,920
1,440 -
3,260
Sinter Machine
weak stream
9
8,700
3,870 -
15,300
a One-hour average
Sulfur dioxide concentrations exhibited large fluctuations at
all of the above sites with the results of individual one-hour tests
varying by as much as 63% to 91% from the average concentration at a
site.
* Ten Method 8 tests were conducted at Acid Plant 2 and eleven at
Acid Plant 1.
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34
Tables 1 and 2
SUMMARY OF METHOD 8, S02 DATA
BUNKER HILL COMPANY
Kellogg, Idaho
Start
Sample Volume3
S02 Collected S02
Concentration
Date
Time
m3
mg
ppmv
ACID PLANT 1
(STATION 48901)
5/21
1208
0.792
7,580
3,590
1605
0.800
9,570
4,510
5/22
0940
0.804
10,500
4,920
1156
0.826
10,200
4,620
1453
0.822
9,580
4,400
5/23
1013
0.817
3,820
1,760
- 1310
0,849
4,800
2,120
1612
0.820
4,580
2,100
5/24
1030
0.814
3,640
1,680
1340
0.830
6,290
2,850
1618
0.847
15,400
6,840
Avg.
3,580
ACID PLANT 2 (STATION 48902)
5/21
1335
0.786
5,800
2,770
1635
0.764
5,900
2,900
5/22
1053
0.809
7,010
3,250
1311
0.766
4,720
2,310
1638
0.822
3,310
1,510
5/23
1131
0.762
3,140
1,550
1423
0.780
2,050
990
1710
0.800
4,080
1,920
5/24
1034
0.824
3,990
1,820
1415
0.811
7,990
3,700
Avg.
2,270
a Sample volume on dry basis at standard conditions of 20°C (68°F) and
760 mm (29.92 in) Hg.
-------
35
Tables 3 and 4
SUMMARY OF METHOD 8, S02 DATA
BUNKER HILL COMPANY
Kellogg, Idaho
a
Start Sample Volume S02 Collected S02 Concentration
Date Time m3 mg ppmv
ACID PLANT 3 (STATION 48904)
5/15
1146
0.822
4,190
1,920
1550
0.809
7,030
3,260
5/16
1020
0.848
4,020
1,780
1430
0.828
4,640
2,100
1716
0.836
3,190
1,440
5/17
- 0943
0.832
3,440
1,550
1158
0.844
5,170
2,300
1418
0.830
3,340
1,510
1717
0.854
3,300
1,450
Avg.
1,920
SINTER MACHINE WEAK STREAM (STATION 48905)
5/15
1107
0.709
13,000
6,870
1456
0.583
5,980
3,870
1725
0.755
20,600
10,300
5/16
1025
0.867
18,300
7,920
1427
0.744
19,400
9,800
1750
0.736
13,600
6,950
5/17
1033
0.727
29,600
15,300
1341
0.731
21,700
11,200
1616
0.754
12,200
6,080
Avg.
8,700
a Sample volume on dry basis at standard conditions of 20°C (68°F) and
760 mm (29.92 in) Hg.
-------
36
Sulfur dioxide concentrations were also measured using TECO
pulsed-fluoresence analyzers [Appendix G]. From 27 to 35 hours of
concentration data were collected at the acid plants and Sinter
Machine, and 6 hours at Blast Furnace 1 using TECO analyzers [Table
5]. These data also indicate wide fluctuations in SC^ concentrations
at individual sites with short-term (15 min) average concentrations
varying by as much as 63% to 145% from the 1.5 to 9-hour average for
the day. Daily averages differed by as much as 11% to 50% from the
overall average S02 concentration measured at a site.
The fluctuations observed at Acid Plant 3 reportedly reflect
variations in the sulfur content of the Sinter Machine feed. Fluc-
tuations in tail gas S02 concentrations at Acid Plants 1 and 2 were
normally associated with a roaster being placed in service or being
shut down.
A comparison of Method 8 results with concurrent TECO data [Tables
6 through 9] show that the overall averages are in close agreement (^5%)
at Acid Plant 3 but differ by 15% to 32% at the other three locations.
These comparisons use only the first nine sets of Method 8 and concurrent
TECO data to be consistent with the requirements of the accuracy perfor-
mance specifications of 40 CFR 52, Appendix D. The TECO was able to
meet the accuracy performance specifications only at Acid Plant 3 and
did not consistently meet the calibration error and calibration drift
specifications [Table 10]. The analyzer did satisfy the zero drift
and response time specifications.
The stability and precision of the dilution system [Figure 3]
used with the TECO are considered the primary factors responsible for
the analyzer not consistently meeting all performance specifications.
Voltage variations in the electrical power supply could also have
affected analyzer response; however, no voltage data are available to
allow this effect to be quantified.
-------
37
Table 5
SUMMARY OF TECO, S02 DATA
BUNKER HILL COMPANY
Kellogg, Idaho
Daily Average S02 Range of S02
Sampling Location Hours of Concentration Concentrations
(Station No.) Date Data ppmv ppmv
Acid Plant 1
5/21
2.0
4,020
3,860-4,140
(48901)
5/22
6.75
3,750
2,480-5,350
5/23
8.0
1,380
690-2,250
5/24
8.25
2,880
1,140-4,070
5/25
2.0
2,590
2,120-2,970
Total
27
Avg.b
2,720
Acid Plant 2
5/21
3.0
2,920
2,310-3,220
(48902)
5/22
7.0
2,570
1,980-3,640
5/23
6.0
2,220
1,430-4,810
5/24
7.75
4,200
1,040-6,180
5/25
5.25
1,600
1,550-2,320
Total
29
Avg.b
2,800
Acid Plant 3
5/14
8.0
1,650
340-3,190
(48904)
5/15
9.0
1,880
880-3,130
5/16
9.0
1,640
840-3,290
5/17
9.0
1,580
600-2,490
Total
35
Avg.b
1,690
Sinter Machine
5/13
1.5
4,760
3,590-5,600
Weak Stream
5/14
4.0
3,450
1,930-7,490
(48905)
5/15
7.75
5,700
2,740-9,660
5/16
8.25
7,650
3,590-17,600
5/17
8.0
9,680
3,140-16,300
Total
29.5
Avg.b
6,970
Blast Furnace 1
5/26
6.25
1,840
1,030-3,860
(48906)
a Fifteen-minute average
b Time-weighted
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38
Tables 6 and 7
COMPARISON OF METHOD 8 AND TECO, S02 DATA
BUNKER HILL COMPANY
Kellog, Idaho
Start Average SO? Concentration (ppmv)a Difference'3
Date Time Method 8 TECO (ppmv)
ACID PLANT 1 (STATION 48901)
5/21
1605
4,510
4,160
350
5/22
0940
4,920
4,380
540
1156
4,620
4,240
380
1453
4,400
3,070
1,330
5/23
1013
1,760
2,000
-240
1310
2,120
1,440
680
1612
2,100
790
1,310
5/24
1030
1,680
2,340
-660
1340
2,850
2,820
30
1618C
6,840
3,900
2,940
Averages
3,220
2,800
410
ACID PLANT 2 (STATION 48902)
5/21
1335
2,770
2,560
210
1635
2,900
3,110
-210
5/22
1053
3,250
3,550
-300
1311
2,310
2,560
-250
1638
1,510
2,250
-740
5/23
1131
1,550
2,580
-1,030
1423
990
1,710
-720
1710
1,920
2,950
-1,030
5/24
1034
1,820
3,940
-2,120
1415
3,700
5,710
-2,010
Averages
2,110
2,800
-690
a One-hour average
b Method 8 minus TECO results
c Extra test, results not used to
calculate averages for comparison
-------
39
Tables 8 and 9
COMPARISON OF METHOD 8 AND TECO, S02 DATA
BUNKER HILL COMPANY
Kellogg, Idaho
Start Average SO? Concentration (ppmv)a
Di f ference*3
Date
Time
Method 8
TECO
(ppmv)
ACID PLANT 3
(STATION 48904)
5/15
1146
1,920
1,670
250
1550
3,260
2,860
400
5/16
1020
1,780
1,780
0
1430
2,100
1,970
130
1716
1,440
1,320
120
5/17
0943
1,550
1,610
-60
1158
2,300
2,410
-110
1418
1,510
1,490
20
1717
1,450
1,310
140
Averages 1,920
1,820
100
SINTER MACHINE WEAK STREAM (STATION 48905)
5/15
1107
6,870
6,120
750
1456
3,870
3,550
320
1725
10,300
8,150
2,150
5/16
1025
7,920
7,600
320
1427
9,800
8,500
1,300
1750
6,950
6,080
870
5/17
1033
15,300
12,400
2,900
1341
11,200
9,820
1,380
1616
6,080
5,520
560
Averages 8,700
7,530
1,170
a One-hour average
b Method 8 minus TECO results
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Table 10
EVALUATION OF TECO PERFORMANCE
BUNKER HILL COMPANY
KELLOGG, IDAHO
Results of Performance Specification Check
Parameter
Specification
Acid Plant 1
(48901)
Acid Plant 2
(48902)
Acid Plant 3
(48904)
Sinter Machine
Weak Stream
(48905)
Accuracy
<20% of reference
28.8
57.3
11.6
21.2
mean value
(50% gas)
Calibration Error
< 5% of each (50%
2.4
6.7
7.0
2.0
and 90% span)
(90% gas)
calibration gases
1.5
1.0
8.6
1.1
Zero Drift
< 2% of emission
0.48/0.0a
0.10
0.07
.19
(2-hour)
standard
Calibration Drift
< 2% of emission
3.6/5.6a
1.3
1.6
1.5
(2-hour)
standard
Response Time
15 minutes maximum
2.30
0.84
0.68
1.90
a Two values calculated at this station because of change in span gases.
-------
41
Inaccuracies in the TECO data can be mitigated by using the re-
sults of the Method 8/TECO comparisons conducted at each site to de-
velop an appropriate correction factor.* For example, the average
S02 concentration measured by Method 8 (3,220 ppm) was 115% of that
measured by the TECO (2,800 ppm) during 9 hours of valid concurrent
sampling at Acid Plant 1 [Table 6]. The TECO data collected at Acid
Plant 1 was, therefore, multiplied by 1.15 to bring it into closer
agreement with the Method 8 results. Likewise, all TECO data were
adjusted [Table 11] according to the Method 8/TECO correction factor
calculated for that sampling site.
Since the EPA regulation which is the subject of the present
remand contains a 6-hour average limitation of 2,600 ppm for the acid
plants, the adjusted TECO data were interpreted in terms of 6-hour
averages [Table 12]. For those days during which at least 6 hours of
data were collected, running 6-hour average SO^ concentrations were
calculated using 1-hour intervals. As indicated in Table 12, 6-hour
average concentrations in excess of 2,600 ppm were measured at Acid
Plants 1 and 2 with maximum 6-hour averages of 4,400 and 3,500 ppm,
respectively. The maximum 6-hour concentration measured at Acid Plant
3 was 2,080 ppm.
Gas flows were measured at the acid plants and the Sinter Machine
at approximately 2-hour intervals over the same time period during
which concentration data were collected [Appendix G]. Average flow
* No Method 8 testing was conducted at the blast furnace, therefore,
no adjustment factor was developed for this data.
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42
Table 11
SUMMARY OF ADJUSTED TECO, S02
BUNKER HILL COMPANY
Kellogg, Idaho
DATA
Sampling Location
(Station No.)
Adjusted
Hours of Daily Average S02
Data Concentration ppv
Acid Plant 1
5/21
2.0
4,620
(48901)
5/22
6.75
4,310
5/23
8.0
1,590
5/24
8.25
3,310
5/25
2.0
2,980
Total
27
Avga
3,130
Acid Plant 2
5/21
3.0
2,190
(48902)
5/22
7.0
1,930
5/23
6.0
1,700
5/24
7.75
3,150
5/25
5.25
1,200
Total
29
Avga
2,100
Acid Plant 3
5/14
8.0
1,730
(48904)
5/15
9.0
1,970
5/16
9.0
1,720
5/17
9.0
1,660
Total
35
Avga
1,770
Sinter Machine
5/13
1.5
5,520
Weak Stream
5/14
4.0
4,000
(48905)
5/15
7.75
6,610
5/16
8.25
8,870
5/17
8.0
11,200
Total
29.5
Avga
8,080
a Time-weighted
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43
Table 12
SIX-HOUR AVERAGE S02 CONCENTRATIONS
ADJUSTED TECO DATA, ACID PLANTS 1 THROUGH 3
BUNKER HILL COMPANY
Kellogg, Idaho
Location
Date
Time Period
Running 6-hour
Average S02 Concentrations
Acid Plant
1
5/22
0855-1640
4400
'
5/23
0905-1747
1840,1610,1350
5/24
0852-1758
2970,3280,3580
Acid Plant
2
5/22
0926-1746
1960,1840
5/23
1100-1804
1700
5/24
0848-1756
3360,3500
Acid Plant
3
5/14
0950-1835
1460,1630,1760
5/15
0841-1925
1670,1850,2060,2080
5/16
0850-1855
1610,1720,1660,1690
5/17
0844-1818
1830,1760,1700,1600
-------
44
rates for these sites are summarized below:
Flow Rate (STP, Dry)3
m3 (ft^)/min
Location
Average
Range
Acid Plant 1
444 (15,700)
393-475 (13,900-16,800)
Acid Plant 2
408 (14,400)
297-450 (10,500-15,900)
Acid Plant 3
659 (23,300)
552-736 (19,500-26,000)
Sinter Machine
weak stream
475 (16,800)
371-549 (13,100-21,000)
a Standard conditions are 20°C (68°F) and 760 mm (29.92 in) Hg.
Gas stream parameters (temperature, moisture, etc.) measured
concurrently with velocities are summarized in Table 13.
The following S02 emission rates have been calculated for the
Bunker Hill acid plants and sinter machine weak stream using the
average flow rates and S02 concentrations (adjusted TECO) measured
by NEIC during May 12-25, 1978:
Location
Average S02 Emission Rate
m. tons (tons)/day
Acid Plant 1
5.4 (5.9)
Acid Plant 2
3.3 (3.6)
Acid Plant 3
4.4 (4.9)
Sinter Machine
weak stream
14.8 (16.2)
No emission rate was calculated for the blast furnace because
there were no measured gas flow rates for that source.
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Table 13
SUMMARY OF GAS STREAM PARAMETERS
BUNKER HILL COMPANY '
Kellogg, Idaho
Acid Plant 1
Parameter (Station 48907)
Sampling Locations
Acid Plant 2
(Station 48903)
Acid Plant 3 Sinter Machine
(Station 48904) (Station 48905)
Temp. °K (°R)
Ave.
Range
% Moisture
Ave.
Range
% 02
Ave.
Range
% C02
Ave.
Range
324 (584)
306-334 (551-602)
2.3
1.1-6.5
7.8
5.3-10.3
0.0
0.0-0.6
Average Stack Pressure
mm Hg (in Hg) 695.4 (27.38)
Average Molecular
Wt (Dry)3 28.1
319 (575) .
306-329 (551-592)
10.4
8.9-13.1
8.3
6.5-10.9
0.1
0.0-1.0
692.6 (27.27)
28.3
326 (587)
316-335 (569-603)
1.4
1.1-2.0
11.9
9.0-15.7
1.9
0.0-2.9
700.3 (27.57)
28.7
410 (738)
370-461 (666-830)
6.5
2.3-8.4
20.2
18.7-21.0
0.2
0.0-1.2
695.7 (27.39)
28.8
a Individual readings varied from average by maximum of approximately 1%.
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46
COMPARISON OF NEIC AND COMPANY DATA
Company flow data extracted from the operating logs for Acid
Plants 1 through 3 [Appendix H] for the period of May 12 through 25
and the average for each sampling period was compared (after adjust-
ment for S02 content) to NEIC-measured flow data for the same period
[Table 14]. The comparison indicated that Company flow measurements
at Acid Plant 2 averaged approximately 7.0% low compared to the NEIC
data, while Company measurements at Acid Plants 1 and 3 were higher
by 24% and 30%, respectively.
The NEIC flow data were based on average gas velocities measured
using Method 2 with traversing by Method land have an expected accu-
racy of approximately ±10%5. The accuracy of Company flow data is
unknown, but the use of single point velocity measurements makes this
data questionable.
Both adjusted TECO data and concurrent Reich test results were
used to calculate an average S02 concentration (reflecting a 2- to
11-hour sampling period) for each day of sampling at the acid plant
tailgas streams [Table 15]. The overall average S02 concentrations,
based on the above daily averages agreed to within 17% for all three
acid plants. Less agreement was noted when the average concentrations
for a single day were considered. No direct comparison was made be-
tween Method 8 and Reich test results because the difficulty associated
with identifying concurrent pairs of data.
Company measured-S02 concentrations for the Sinter Machine weak
stream were in wide disagreement with NEIC measurements. During test-
ing at this location from May 13 to 17, the maximum Company-measured
S02 concentrations was 3,500 ppm, while the NEIC S02 concentrations
data (adjusted TECO) averaged 8,080 ppm.
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47
Table 14
COMPARISON OF NEIC AND COMPANY FLOW DATA
ACID PLANTS 1 through 3
BUNKER HILL COMPANY
Kellogg, Idaho
Average Flow Rate3 (STP, Dry)*3
Location Date Time Period NEIC Data Company Data
(hours) m3 (ft3)/min m3 (ft3)/min
Acid
Plant
1
5/21
1330-1730
408
(14,400)
518
(18,300)
5/22
0900-1630
453
(16,000)
580
(20,500)
5/23
0900-1630
436
(15,400)
546
(19,300)
5/24
0900-1630
464
(16,400)
563
(19,900)
5/25
0900-1100
453
(16,000)
546
(19,300)
Acid
Plant
2
5/21
1430-1730
405
(14,300)
368
(13,000)
5/22
0830-1600
419
(14,800)
402
(14,200)
5/23
0830-1600
419
(14,800)
362
(12,800)
5/24
0830-1600
399
(13,700)
416
(14,700)
5/25
0830-1030
416
(14,700)
357
(12,600)
Acid
Plant
3
5/12
1400-1800
690
(24,400)
787
(27,800)
5/13
1000-1200
690
(24,400)
874
(30,900)
5/14
1000-1430
620
(21,900)
872
(30,800)
5/15
0900-1800
676
(23,900)
874
(30,900)
5/16
0800-1630
642
(22,700)
857
(30,300)
5/17
0800-1900
645
(22,800)
860
(30,400)
a Flow rates measured by Bunker Hill at inlets to acid plants have
been adjusted to outlet conditions using the following inlet S02
concentrations: Acid plants 1 and 2 - 7.0%, Acid plant 3 - 5.0%.
b STP = Standard temperature 20°C (68°F) and 760 mm (29,92 in) Hg.
-------
VI. PROCESS EVALUATION
Company personnel indicated during the testing period that oper-
ation of the smelter and zinc plant were relatively normal. No upsets
or malfunctions occurred which would have greatly affected S02 emissions.
During the survey period, the lead smelter was operating near design
capacity, and the zinc plant was operating at about 70% of capacity.
Operating conditions for major pieces of smelter and zinc plant
process equipment are summarized in the Confidential Technical Appendix
to this report (EPA-330/2-78-0!8A)*. The Confidential Technical Appendix
also contains all process data collected by NEIC during the testing
program.
* A more detailed process evaluation will be presented in a future
NEIC report.
-------
VI. PROCESS EVALUATION
Company personnel indicated during the testing period that oper-
ation of the smelter and zinc plant were relatively normal. No upsets
or malfunctions occurred which would have greatly affected S02 emissions.
During the survey period, the lead smelter was operating near design
capacity, and the zinc plant was operating at about 70% of capacity.
Operating conditions for major pieces of smelter and zinc plant
process equipment are summarized in the Confidential Technical Appendix
to this report (EPA-330/2-78-098A)*. The Confidential Technical Appendix
also contains all process data collected by NEIC during the testing
program.
* A more detailed process evaluation will be presented in a future
NEIC report.
-------
50
REFERENCES
1. Code of Federal Regulations, Part 40, Title 52. Approval and
Promulgation of Implementation Plans, Section 52.676, Control
Strategy: Sulfur Oxides - Eastern Washington and Northern Idaho
Interstate Region.
2. Code of Federal Regulations, Part 40, Title 60. Standards of
Performance for New Stationary Sources, Appendix A, Reference
Methods 1, 2, 3, 6 and 8.
3. Code of Federal Regulations, Part 40, Title 52. Approval and
Promulgation of Implementation Plans, Appendix D, Determination
of Sulfur Dioxide Emissions From Stationary Sources by Contin-
uous Monitors.
4. Jahnke, J.A., Chevey, J.L. and Homolya, J.B. 1976. Quenching
Effects in S02 Fluorescence Monitoring Instruments. Environmental
Science and Technology 10:12, p 1246 - 1250.
5. Shigehara, R.T., Todd, W.F., and Smith, W.S. Significance of
Errors in Stack Sampling Measurements. Paper presented at 63rd
Annual Meeting of the Air Pollution Control Association, June
14-19, 1970 (APCA No. 70-35).
-------
APPENDIX A
REQUEST FOR SAMPLING SITE MODIFICATIONS
-------
U. 5 WVIRON MENTAL PROTECTION AGENCY
REGION X
Z
ID
o
T
1200 SIXTH AVENUE
SEATTLE, WASHINGTON 98101
"hko ? Mail St°P 514
AFK i i jo/3
Mr. E. Viet Howard
President
Bunker Hill Company
P. 0. Box 29
Kellogg, Idaho 83837
Dear Mr. Howard:
In our letter of March 3, 1978 we advised the Company that
the Environmental Protection Agency (EPA) p]anned to conduct
a sampling and monitoring program at your facility in early
May 1978. In Bill Boyd's letter of March 23 he noted that
our proposed May visit appeared to be acceptable to Bunker
Hill, but requested additional details and verification of
the purpose of the visit.
At this time we would like to inform you of the details and
purpose of the measurement program and to request the Cornpan
to make necessary ductwork modifications and other
arrangements required to conduct the program prior to t-he
commencement of sampling on May 8. We have attempted to
specify as clearly and precisely as possible what must be
accomplished, but we believe that a visit by Mr. Osag and Mr
Sims will be necessary to ensure that all the necessary
arrangements have been made. They will plan to be at the
Bunker Hill complex on or about May 2, 1978, for the purpose
of a pre-test inspection.
DESCRIPTION OF MEASUREMENT PROGRAM
The measurement program itself will commence on May 8, 1978
and should extend to approximately May 28, 1978. During thi
time we plan to measure:
1) Acid plant #1, £2 and S3 offgas-SO- concentration and
gas flow.
-------
_ o
DUCTWORK MODIFICATIONS
For each sample location Bunker Hill will be required ,to make
certain ductwork modifications to conduct the sampling.
These modifications are fully outlined in Enclosure 1 and
must be completed on or before May 1, 1978.
PROCESS DATA
To enable us to equate the results of the gas stream
measurements to specific process operations during the period
of sampling, certain process and production information will
be needed. This information is described in Enclosure 2.
It has come to our attention that operating personnel are
instructed to shut-off strip chart recorders during periods
when process equipment is shutdown. We find this highly
unusual and, for our purposes, an unacceptable practice,
since the strip charts do not then portray an accurate record
of plant operations. Therefore, it is requested that Bunker
Hill immediately continue to operate all strip chart
recorders continuously at all times.
PARTICIPANTS
We are not yet able to specify exactly which EPA personnel
will be involved in the sampling/monitoring program.
However, we intend to have two sampling teams of at least
four members each present in the facility. In addition,
since it is necessary to do the sampling and to
simultaneously observe the status of process and/or control
equipment, at least two additional people will be observing
equipment status. Lastly, one or two men will be present in
each mobile laboratory. Therefore we expect a total of 13 to
16 EPA people to be present.
Please inform us immediately if any piece of the process or
control equipment (i.e., blast furnaces, sinter machine, all
three acid plants) we have set for testing is scheduled to be
down during any of the proposed sampling days.
As you know, this test program is necessary to enable the EPA
to properly conduct the S0~ remand activity. Authority for
conducting these activities and for the advance arrangments
required by the Company is contained in Section 114(a) of the
Clean Air Act.
-------
2) Blast furnace offgac-SC^ concent r at i on and gas Clow.
3) Sinter machine weak stream-S0o concentration and gas
flow. 1
We will also need to conduct certain ancillary activities
necessary to assess the validity of the measurements and the
operating status of the relevant equipment.
The purpose of the program is to measure the tailgas SO
content of each acid plant to evaluate the current
performance of each acid plant and to document the impact of
the changes Bunker Hill has apparently performed on the acid
plants in the last 2 years. As we have noted before several
times, acid plant performance specifications must be included
as part of any response to the remand. We need to determine
whether Bunker Hill's acid plants are properly designed,
operated and maintained and to evaluate whether the acid
plant emission performance needs to be significantly
improved. As you know, we have requested Bunker Hill to
install continuous monitors on the acid plant tailgas but the
Company has refused to do so. The EPA sampling activity is
not a substitute for Company installed and operated monitors
and we once again request that Bunker Hill install and
operate continuous SC^ monitors on the tail gas of each
acid plant.
We also intend to measure the sinter machine weak stream and
blast furnace S0_ offgas concentrations and gas flows in
order to determine what SO total plant emission limit
shall be included in the response to the remand and to
determine the feasibility of scrubbing and other additional
SO controls for those streams. In our original total
plant emission limit calculation we relied on data provided
verbally by Bunker Hill personnel, which we presently believe
to be incorrect.
SAMPLING LOCATIONS
Specific locations where samples will be drawn are fully
detailed in Enclosure 1. We also request Bunker Hill to
provide 110 vac electrical outlets at each sample location
and to provide four parking sites, two close to the zinc
plant acid plants and two as close as possible to the lead
smelter acid plant. Each parking site will require 220 vac,
single phase, 50 amp service for a mobile laboratory.
-------
-'I-
If you have questions regarding any of the above matters,
please contact William T. Christian for legal matters or
Larry L. Sims for technical matters by phone at (206)-
442-1275 or (206) 442-1106, respectively. Thank you for your
cooperation in this matter.
Sincerely,
Donald P. Dubois
Regional Administrator
cc: William Boyd, Esq.
Gene Baker
-------
ENCLOSURE 1
SAMPLING LOCATIONS & DUCTWORK MODIFICATION
A. References -
Location
Drawing No.
Title
No. 1 Acid Plant Outlet
No. 2 Acid Plant Outlet
Smelter Acid Plant Outlet
Sinter Machine Weak Stream
Blast Furnace
B-1990 (REV E)
Plan & Elevation, Fan
to Towers-Zinc Plant,
5'-0", 3'-6" and 3'-0"
Diameter
(Same as for No. 1 Acid Plant)
D-1797 (REV A)
B-2097 (REV C)
90-10-003(REV 5)
90-10-037(REV 3)
S-l5-704(REV 3)
Duct, MK-S-39 and
MK-S-40, 4 '-6" Diameter
Duct, Section View B-B
& C-C, Lead Smelter
54" ID
New Flue & Fan System,
General Arrangement,
Blast Furnace to Baghor
New Flue & Fan System,
Sinter Tail Gas Flue,
Arrangement, Plan &
Elevation
Sinter Blast Furnaces
Dual Sinter Feed
System, General Arrange
ment
B. Sample Site Descriptions -
The following describes each location where measurements will be taken.
Each description specifies certain modifications such as drilling new
sampling ports and installing nipples which Bunker Hill is requested
to perform.
Note - Reference to "Method #'s" denotes EPA source test methods
contained in 40 CFR Part 60.
-------
-2-
No. 1 Acid Plant (Zinc plant)
A sampling location for the tailgas is available in the 36 inch diameter
stainless steel (SS) duct which connects the absorption tower with
the downcomer to the fiberglass reinforced plastic (FRP) ductwork leading
to the stack. Two 4.0 inch diameter ports are located on one'side of this
duct with a 2.0 ft. separation between the two ports. The distance
between the sampling location and the nearest upstream and downstream
flow disturbances are 40 and 10 ft. respectively.
It will be necessary to install ag additional 4.0 inch diameter sampling
port in the top of the duct at 90 to the existing downstream port (see
figure 1). The two downstream ports will be used to measure velocity
and S0? using a Method 8 train while the existing upstream port will be
used to measure SO2 concentration with the continuous monitor. The
upstream port must be equipped with a 4.0 inch diameter pipe nipple
with standard threads.
No. 2 Acid Plant (Zinc plant)
An existing sampling site is located in the 42 inch diameter horizontal
SS duct which connects the absorption tower with the downcomer to the
FRP duct. This site is similar to the one at the No. 1 Acid Plant;
i.e., two 4.0 inch diameter sampling ports are installed on one side of
the duct with approximately a 2 ft. separation between them. The existing
sampling location is less than 4 ft. downstream of a constriction in the
ducting (duct changes from 52 to 42 inch diameter). No velocity measure-
ments will be taken at this site. However,-the existing ports will be
used to monitor the SO? concentration of the acid plant tailgas. A
continuous monitor will be installed in the upstream port while a Method
8 train will be used at the downstream port. The upstream port must
therefore be equipped with a 4.0 inch diameter pipe nipple with standard
threads. In addition, a 2 ft. section of the guardrail (top rail only) must
be removed from the area directly behind the downstream port. ' The 2 ft.
section should be centered around the centerline of the port.
Two 4.0 inch diameter ports with a 90° separation must be installed in
the downcomer at a location 7.0 ft. above the platform. Both ports must
be accessable from the platform (see figure 2). This location is
approximately 20 ft. downstream of the S02 sampling site and will be used
to measure velocities.
-------
-A-
H n vJ H - <=X>, Po(\1"
_G
i$>cRP i I c N
-Vvj G.a
Gas
F Lou
^ **¦ *"
o< >o
E. * \ sT IM Q,
Po n. t\s
• A
3b
Dovj |\i c okv r. ^
'J
install H - r51 p tv. M \ p p u Hl
s) Dfi iaw
Figure 1. Sampling Site ot No. 1 Acid Plant
-------
-4-
T o P V \ p_ y|
F (\o n
M o. 1 Ac.1^ PLANT"
fM G K1 M - ^—0^ PcDf\T^
OcWtsl C-^r-^Cifiy
FIX
iNO,| ,'\ C. t D Pt/\MT
C>0 c_T
PLATI-oarA
C^ow m Con^T; (\
P i"\ o f-"V
No.l /\cib PlAmT
f- r\ c ih * \i \ \ivJ
1 $+
77T
GAS
f- L o v4
N, \i u^-j
3k. Pof\iS>
S •$ + - <0
' * ¦ / t ~? '
~ , 7
Pl/vT r-oK^
Figure 2. Velocity Measurement Site at No. 2 Acid Plant
! -V ; ¦')
-------
Smeltor Acid Plant
An existing sampling site is available in the 54 inch diameter TRP
downcomer which connects the outlet from the acid plant to the down-
stream fan. Two 4.0 inch diameter ports are now installed on the front
side (with respect to the platform) of the duct, one port 2 ft*, below the
other. This sampling location has clearances of approximately 10 and
30 ft., respectively, from the nearest downstream and upstream flow
disturbances. Both S0„ monitoring and velocity measurements will be
conducted at this site.
The upstream port requires a 4.0 inch diameter pipe nipple with
standard threads while two additional 4.0 inch diameter ports must be
installed at the same level as the existing downstream port. The
new ports must be installed at 45 to the existing port, one on either
side.
Sinter Machine Weak Stream
The sinter machine weak stream (flue B) will be sampled approximately
10 ft. upstream of the breeching with the high velocity flue. Two
4.0 inch diameter ports (90 separation) must be installed in the side
and top of the 42 inch diameter duct 10 ft. upstream of the connection
with the high velocity flue. These ports will be used to measure SO2
with the Method 8 train and velocity. A third port, equipped with a 4.0
inch diameter pipe nipple with standard threads, must be installed on
the side of the duct 2 ft. upstream of the other ports (see figure 3).
Blast Furnace
The blast furnace will be sampled in the gooseneck duct which connects
the furnace with the brick flue leading to the high velocity flue
(see figure 4). This location is the only practical sampling location
available. Five 4.0 inch diameter ports should be installed in the top of
the gooseneck at the location where the platform grating has been removed
to expose the ducting. The new ports should be placed in a line
perpendicular to the duct's axis with a separation between ports (center
to center) of D/5, where D is the inside dimension (width) of the duct,
and a separation between the horizontal walls and the nearest port of
D/10. Since it is not possible to verify which blast furnace will be
operating during the test period, the above modifications should be made
for both.
-------
-u -
'High vr.ioaiTT flue
IN .ST ML X
N p h 4 - p c a. T
Figure 3. Sampling Site at Sinter Machine V.'eak Stream
-------
-7-
S i o iZ \/1 n -jJ
ov
Q> o o-S G. N (I c. K. \- u w C_
f3 u A V P o
oA^PDHC-, ilT£
Q>(\\C- HUt;
> P>£ N I M Q,
f-o<\ >
.h --—**V-\ ^rvrtf
o C> D Q <5
I
I
1^ C.H
Goc^'G N £c ^
r'_ 0 ';_
Plat r- o
Figure 4. Sampling Site at Blast Furnaces
v
'/'
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ENCLOSURE 2
PROCESS OPERATING DATA
During the course of the sampling and measurement program it will
be necessary to collect certain process operating data. Tlns'data
is necessary to assess the validity of the measurements. The following
is a list of operating logs that must be supplied to EPA for each day
of the sampling program:
Location Operating Log Title
Zinc Plant 1. Daily Operating Report, No. 5
Roaster
2. Flash Roasters Daily Report
(Roaster 1-4)
3. Daily Operating Log Sheet
(Acid Plants 1 & 2)
Lead Smelter 4. Daily Operating Log Sheet
(Smelter Acid Plant)
5. Sinter Plant Operators Process
Control Sheet
6. Sinter Plant Process Control Sheet
7. Main Baghouse Operation Log
8. Lead Refinery Daily Report
9. Blast Furnace Process -Control Sheet
10. Blast Furnace Schedule Control Sheet
11. Casting and Loading Schedule
Control Sheet
12. Smelter Bedding Plant Work Sheet
13. Ore Preparation Schedule Control Sheet
EPA v/ill also require copies of the strip charts which indicate the
SO2 concentration and gas flow at both the zinc plant stack and the
smelter stack and copies of the acid plants' charts which indicate gas
flows and inlet S0£ concentrations.
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During the testing program, it will be necessary to have unres-
tricted access to the acid plant coilrol rooms (zinc plant and smelter),
the blast furnace control room, the sinter plant control room, and the
roaster control rooms.
In addition, EPA will need to discuss with responsible Bunker Mill
personnel the following items regarding continuous SO2 measurements
obtained by Bunker Hill. Specifically this is applicable to the smelter
main stack, the zinc plant main stack, the inlet and outlets of the
three acid plants and the sinter machine outlets:
1. Data Validation
a. Criteria used
b. Type of sample and instrument checks
2. Audit Procedures
3. Calibration
a. Calibration procedure
b. Schedule of calibration
c. Type of standards used and type of devices used in flow
calibration
d. Flow checks on dilution system, if any
4. Preventive Maintenance
a. Copy of procedure, or if done by vendor, copy of his procedure
b. System checks and replacements done, filters, etc., and
cleaning procedures
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APPENDIX B
PROJECT PLAN AND FIELD MODIFICATIONS TO PLAN
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PROJECT PLAN
BUNKER HILL LEAD SMELTER/ZINC PLANT SOURCE TESTING PHASE .
KELLOGG, IDAHO
MAY 8-28, 1978
I. OBJECTIVES
The objectives of the survey are to determine S0£ concentrations
and flow rates at the following five locations in the Bunker Hill
Smelter:
1. Tail gas from the No. 1 acid plant (zinc plant)
2. Tailgas from the No. 2 acid plant (zinc plant)
3. Tailgas from the No. 3 acid plant (lead smelter)
4. Sinter machine weak stream (lead smelter)
5. Blast furnace exhaust (lead smelter)
II. BACKGROUND
The Bunker Hill Company operates a combined lead smelter/zinc plant
at Kellogg, Idaho. On November 19, 1975, Region X of the Environmental
Protection Agency disapproved Regulation "S" of Idaho's State Implemen-
tation Plan (SIP), which limited sulfur dioxide (SOJ emissions from the
Bunker Hill complex, and substituted a replacement regulation. This
action was challenged by the Bunker Hill Company with the result that
the U. S. Court of Appeals (Ninth Circuit) remanded the regulation to
EPA for "further consideration of the technological feasibility of
certain modifications of petitioner's smelter operations which would
be required by the substituted regulations."
Region X subsequently requested that the National Enforcement
Investigations Center (NEIC) conduct tests at the five locations dis-
cussed above to develop data for use in the remand proceeding.
A reconnaissance of the Bunker Hill complex was conducted by NEIC
March 27-30, 1978, to evaluate sampling sites and identify process data
to be collected in conjunction with the testing. Region X subsequently
informed the Company of necessary sampling site modifications and pro-
cess data requirements. Testing has been scheduled for the period of
May 8-28, 1978. The following project plan has been developed for the
scheduled testing, but is subject to change in the field.
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2
III. SAMPLING
Data Requirements"
This sampling program is designed to provide approximately 40 hours
of S0? concentration data and intermittent concurrent flow data for each
of the three acid plant outlets and the sinter machine weak gas stream.
The determination of gas stream flow rates will require the measurement
of gas velocity, temperature, molecular weight, and moisture content.
Approximately six hours (3 @ 2-hour tests) of S0? emission data (average
concentration and emission rate) will be collected for the blast furnace
This will include concurrent determination of gas flow rates.
Sampling and Measurement Procedures
Sulfur dioxide concentrations at the acid plant outlets and the
sinter machine weak stream will be measured with TECO pulsed fluorescent
analyzers. During the testing at each site, the TECO analyzers will be
checked for compliance with the following performance specifications*:
Parameter
1. Accuracy*2
2. Calibration Error*2
3. Zero Drift (2-hours)a
4. Zero Drift (24-hours)a
5. Calibration Drift (2-hours)13—
6. Calibration Drift (24-hours)a—
7. Response Time
Specification
- <20 percent of reference mean value
- <5 percent of-each (50% and 90% span)
calibration gas mixture.
- <2 percent of span
- <2 percent of span
- <2 percent of span
- <2.5 percent of span
- 15 minutes maximum
a Expressed as sum of absolute mean value plus 95 percent confidence
interval of a series of tests.
The calibration error check will be conducted in Denver and all
other performance specification checks will be made in the field. The
test procedures presented in Appendix D of 40 CFR 52.2850 [Attachment A]
* Performance specifications are those indicated in Appendix D of 40 CFR
52.2850 with: 1) "span" substituted for "emission standard" for the
zero and calibration drift requirements 2) the 24-hour drift specifi-
cations adjusted to agree with 40 CFR 60 Appendix B, Performance
Specification 2. Monitoring will be conducted using a span concen-
tration of 5^000 ppm for the sinter machine weak gas stream and a span
of 500 ppm for the acid plant outlets.
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3
will be used to verify the monitoring system's ability to meet the above
performance specifications. The operational period specification will
not be addressed since the monitors will only be operated while, attended.
The accuracy performance specification requires that the average SCL
concentration measured by the TECO over a one-hour period be compared to
the results of a concurrent one-hour Method 8 sample. Nine such compar-
isons are required and will be performed. The analytical and computational
portions of Method 8 as they relate to determination of sulfuric acid
mist, as well as the requirement for isokinetic sampling, will be omitted
since only SCL data is desired. Sampling with the Method 8 train will
be conducted at a constant rate (0.5 scfm).
It is estimated that approximately four days will be required at
each sampling site to complete the performance specification check.
During the latter three days of this period, the monitor will also be
providing a continuous record (^30 hours in 10-hour intervals) of the
S02 concentration of the gas stream. An anticipated additional 10 hours
of SOp monitoring will be provided at each site following the completion
of the performance specification check.
In conjunction with the continuous S0« monitoring, gas flow rates
will be determined at one-hour intervals throughout the day. Method 2
(using an isolated S-type pi tot tube) with traversing according to
Method 1 will be used to measure gas velocities. Temperature measure-
ments will be collected with a thermocouple-potentiometer arrangement at
the same time as the velocity measurements.
A gas sample will be collected (Method 3, grab) concurrent with the
velocity measurements and analyzed with Fyrite analyzers (every third
sample will be analyzed using an Orsat analyzer) to allow calculation of
gas molecular weight. Moisture content of the acid plant tailgas streams
can be assumed to be zero while the moisture content of the sinter
machine weak gas stream will be determined from the Method 8 sampling
and from independent Method 4 sampling.
The blast furnace S0~ emissions will be measured with a Method 8
sampling train (3 0 2-hour runs), however, the analytical and computa-
tional portions of Method 8 as they relate to determination of sulfuric
acid mist, as well as the requirement for isokinetic sampling, will be
omitted since only S0~ data is desired. Sampling will be conducted at
a rate proportional to gas velocity while traversing according to
Method 1. Four gas samples will be collected (Method 3, grab) during
each two-hour sampling run and analyzed using either Fyrite gas analyzers
(three samples) or an Orsat analyzer (one sample). Moisture content of
the gas stream will be determined from the weight gain of the Method 8
train impingers.
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4
Sampling Locations
No. 1 Acid Plant (Station 01)
A sampling location for the tailgas is available in the 36-inch
diameter stainless steel duct which connects the absorption tower with
the downcomer to the fiberglass reinforced plastic (FRP) ductwork which
leads to the stack. Two 4-inch diameter ports are located on one side
of this duct with a 2 foot separation between the two ports. The dis-
tance between the sampling location and the nearest upstream and down-
stream flow disturbances are 40 and 10 feet respectively.
An additional 4-inch diameter sampling port will be installed in
the top of the duct at 90° to the existing downstream port. The two
downstream ports will be used to measure velocity and for the Method 8
train while the TECO will be installed in the upstream port. Sulfur
dioxide concentrations will be measured at the midpoint of the duct.
Twelve points will be used for velocity measurements.
No. 2 Acid Plant (Stations 02 and 03)
An existing sampling site (Station 02) is located in the 42-inch
diameter horizontal stainless steel duct which connects the absorption
tower with the downcomer to the FRP duct. This site is similar to the
one at the No. 1 Acid Plant (i.e., two 4-inch sampling ports are installed
on one side of the duct with approximately a -2 foot separation between
them). The existing sampling location is less than 4 feet downstream of
a constriction in the ducting (duct changes from 52 to 42-inch diameter).
Since the separation between this constriction and farthest sampling
port is less than 7 feet required by Method 1, no velocity measurements
will be taken at this site. However, the existing ports will be used to
monitor the SO- concentration of the acid plant tailgas. The TECO will
be installed in the upstream port while a Method 8 train will be used at
the downstream port. Sulfur dioxide concentrations will be measured at
the midpoint of the duct.
Two 4-inch ports with a 90° separation will be installed in the
downcomer to the FRP duct at a location 7.0 feet above the existing
platform. Both ports will be accessible from the platform. This
location (Station 03) is approximately 20 feet downstream of the S0?
sampling site (Station 02) and will be used to measure velocity.
Twenty-four sample points will be used.
Smelter Acid Plant (Station 04)
An existing sampling site is available in the 54-inch diameter FRP
downcomer which connects the outlet from the acid plant to the downstream
fan. Two 4-inch diameter ports are now installed on the front side
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5
(with respect to the platform) of the duct, one port 2 feet below the
other. This sampling location has clearances of approximately 10 and 30
feet, respectively, from the nearest downstream and upstream flgw dis-
turbances.
Both S02 monitoring and velocity measurements will be conducted at
this site. The existing upstream port will be used for the TECO while
the downstream port will be used for the Method 8 sampling. Sulfur
dioxide concentrations will be measured at the midpoint of the duct.
Two additional 4-inch ports will be installed at the same level as
the existing downstream port, each at 45° to the existing port. Velocity
will be measured at these ports using 24 sample points.
Sinter Machine Weak Stream (Station 05)
The sinter machine weak stream (flue B) will be sampled approxi-
mately 10 feet upstream of the breeching with the high velocity flue.
Two 4-inch diameter ports (90° separation) will be installed in the side
and top of the 42-inch diameter duct 10 feet upstream of the connection
with the high velocity flue. These ports will be used for the Method 8
train and velocity measurements (28 points). A third 4-inch port will
be installed on the side of the duct 2 feet upstream of the other ports
for the TECO.
Blast Furnace (Station 06)
The blast furnace will be sampled in the gooseneck duct which
connects the furnace with the brick flue which leads to the high velocity
flue. This location does not meet the minimum requirements of Method 1
(<1 diameter clearance between upstream flow disturbance and sampling
location), however, it is the only practical sampling location available.
Five 4-inch diameter ports will be installed in the top of the
gooseneck at the location where the platform grating has been removed
to expose the ducting. The new ports will be placed in a line perpen-
dicular to the duct's axis with an equal separation between ports
(center to center). Since it is not possible to verify which blast
furnace will be operating during the test period, the above modifi-
cations will be made for both. Twenty-five sampling points will be
used.
Sample Handling and Analytical Requirements
Much of the data collected during this survey will be in-situ
measurements; i.e., velocity and temperature measurements, Fyrite
analysis, S02 concentrations. This data will be recorded on the pre-
scribed forms (recorder paper) and handled according to established
Chain-of-Custody procedures.
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6
Only the peroxide catch (Impingers 2 and 3 with appropriate wash)
of the Method 8 trains used for the performance specification testing
and the blast furnace tests (^40 samples @ 1,000-ml/sample) will be
retained and returned to Denver in polypropylene [Nalgene] containers
under chain-of-custody procedures. Sulfate analyses will be according
to Method 8*. Approximately 14 sample blanks will also be retained for
analysis.
In addition to the above analytical requirements, 12 cylinders of
span gas (S0? in air) will be analyzed prior to the start of the survey
(within two weeks) and again at its completion to verify the S0? con-
centration. Analyses will be by the barium-thorin titration procedure
as required in Appendix D of 40 CFR 52.2850. It will also be necessary
to check the isopropanol to be used during the sampling for peroxide
impurities per Method 8.
Sampling Schedule
Sampling will be conducted simultaneously at two locations through-
out most of the survey. The No. 3 acid plant (lead smelter) and the
sinter machine will be tested first followed by the No. 1 and 2 acid
plants (zinc plant). It is anticipated that approximately seven days
(including set up and tear down time) will be required at each site.
The actual sampling program at each site will cover about a five-day
period and will include:
Performance specification checks of TECO
for response time and zero and calibration
drifts (2 and 24 hours). Flow measurements.
Performance specification checks for zero and
calibration drifts (2 and 24 hours) and-accuracy
(3 @ 1-hour Method 8 tests/day). Flow measure-
ments and monitoring of S0£ concentration.
Performance specification checks for zero and
calibration drifts (24 hours). Flow measure-
ments and monitoring of S02 concentrations.
The sampling at the blast furnace will either be conducted at the
end of the survey or, if possible, simultaneous with other testing. It
is anticipated that three days (including set up and tear down) will be
required to complete this sampling.
First Day
Second Through
Fourth Days
Fifth Day
* Barium-thorin titration
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7
IV. Quality Control (QC) Program
Methods 2, 3, 4 and 8 will be conducted according to the procedures
in Appendix A of 40 CFR 60 (unless previously noted). All calibration
requirements and QC checks identified in Appendix A will be followed.
This will involve calibration of the pi tot tubes, dry gas meters, orifices
and thermocouples both prior to the start of the survey and at its
completion. In addition, blank samples (one blank/day for each site) of
the peroxide solution used during the survey will be returned to Denver
for analysis. All peroxide samples saved as blanks will have been first
used as a second wash for Impingers 2 and 3.
Operation of the TECO continuous SO- monitors will be in accordance
with the calibration and QC procedures in Appendix D of 52.2850*. In
addition, the following QC procedures will be implemented:
1. An in-house span check will be performed on the analyzers at least
two times/day using 50% and 90% span gases. The length of the span
check will depend on the time required for the TECO to stabilize.
2. All span gases will be checked for SO- concentrations both before
the survey begins and at its completion.
3. A span check will be performed at least once per site with a span
gas of unknown concentration provided by the Center's Quality
Assurance officer.
The flow and pressure measurement devices used in the TECO condi-
tioning/dilution system will be calibrated according to the following
procedures:
1. Wet test meter - A calibration check of the meter will be performed
before and after the study using the NBS traceable wet test meter
at NEIC. The wet test meter has a range between 2 and 8 1/min. It
will be used in the calibration of limiting orifices.
2. Dry gas meter - The dry gas meter will be calibrated against a NBS
traceable wet test meter before and after the study. The dry gas
meter will be used to calibrate the rotameter used in the dilution
air systems. It has a range of 5 to 80 1/min.
* As previously mentioned, the 24-hour drift specifications have been
modified to agree with 40 CFR 60, Appendix B, Performance Specification 2.
In addition, "span" has been substituted for "emission standard" in the
zero and calibration drift specifications.
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8
3. Bubble flow meter - The bubble flow meter used in this study was
calibrated against a NBS standard by the manufacturer. Other
bubble flow meters used will be calibrated against this standard
bubble flow meter. The bubble flow meter will be used to calibrate
limiting orifices and to check the flow of the TECO. It has a
range of 0 to approximately 2 1/min. Other flowmeters will be
checked as needed during the study.
4. Rotameter - Rotameters used in this study will be calibrated against
the above mentioned standards. The rotameter will be used in the
air dilution system. It has a range of 500 ml/min to 30 1/min.
The rotameter will be calibrated (10 points) before the study and
after the study. During the study, 3 points on the calibration
curve will be checked at the beginning and end of the testing at
each site.
5. Orifices - All orifices used will be calibrated against the cali-
brated bubble flowmeter, wet test meter, or dry gas meter if
necessary. The orifices will be used in the S0? dilution flow
system. The range can vary depending on the capillary size. They
will be calibrated before and after testing period at each site.
Also they will be checked physically for clogging each day before
startup.
6. Pressure gages and vacuum gages - All gages will be checked against
a calibrated (NBS traceable) pressure transducer. The pressure
gages will be used in the dilution system. They have a range of 0
to 100 psi. The gages will be checked before the survey. The only
critical gage is the one in the S0? dilution system. It will be
checked at the beginning and end of testing period at each site.
V. PROCESS DATA
Copies of the following plant operating logs will be obtained by
NEIC for each day of the testing period.
Location Operating Log Title
Zinc Plant 1. Daily Operating Report, No. 5
Roaster
2. Flash Roasters Daily Report
(Roasters 1-4)
3. Daily Operating Log Sheet (Acid
Plants 1 & 2) Lead Smelter
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9
Lead Smelter 4. Daily Operating Log Sheet (Acid
Plant)
5. Sinter Plant Operators Process
Control Sheet
6. Sinter Plant Process Control Sheet
7. Main Baghouse Operation Log
8. Lead Refinery Daily Report
9. Blast Furnace Process Control Sheet
10. Blast Furnace Schedule Control Sheet
11. Casting and Loading Schedule Control
Sheet
12. Smelter Bedding Plant Work Sheet
13. Ore Preparation Schedule Control
NEIC will obtain copies of the strip chart which indicates the SOp
concentration and gas flow at both the zinc plant stack and the smelter
stack and copies of the acid plants' charts which indicate gas flows and
inlet S02 concentrations.
In addition, the NEIC will conduct a QC check of the S0~ measure-
ments obtained by Bunker Hill at the smelter and zinc plant stacks, the
inlets and outlets of the three acid plants and the sinter plant. This
QC check will include the following:
1. Data Validation
a. Criteria used.
b. Type of sample and instrument checks.
2. Audit Procedures
3. Calibration
a. Calibration procedures.
b. Schedule of calibration.
c. Type of standards used and type of devices used in flow
calibration.
d. Flow checks on dilution system, if any.
4. Preventive Maintenance
a. Copy of procedure, or if done by vendor, copy of his proce-
dure.
b. System checks and replacements done, filters, etc., and
cleaning procedures.
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10
VI. FIELD REQUIREMENTS
Personnel
3 Engineers
1 Chemist
8 Technicians
Vehicles
2 Mobile Laboratories-NEIC
2 Sedans-GSA Motor Pool, Spokane, Washington
1 Step Van-NEIC
1 Station Wagon-Rental, Spokane, Washington
Safety
Field personnel will adhere to NEIC and Company safety require-
ments. The following safety equipment will be worn by all NEIC employees
while on site (except when in the offices or mobile lab areas):
Hard hat
Safety shoes
Safety glasses (side shields not required)
Long sleeve shirts
Respirators with MSA-dust and fume filters (worn where posted)
Time Schedule
May 6-8 - Equipment and laboratories to study area
May 8-28 - Conduct sampling activities
June 30 - Draft report to Region
Final report available two weeks following receipt of comments
from Region.
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FIELD MODIFICATIONS TO PROJECT PLAN
During the actual testing, the Bunker Hill Project Plan was modi-
fied as indicated below:
1. The TECO analyzer was used to measure S02 concentrations at
the blast furnace instead of Method 8 and no flow measurements
were conducted at that site.
2. The performance specifications used to evaluate the TECO
analyzers were altered by omitting the 24-hour drift specifica-
tions and using the proposed acid plant emission limit (2,600
ppm) and the average Method 8 result at the Sinter Machine
weak stream (8,700 ppm) for drift calculations.
3. All performance specification checks were conducted in the
field.
4. Flow measurements were conducted'at 2-hour intervals vs.
the proposed 1-hour intervals.
5. Moisture content of the acid plant tailgas streams were not
assumed to be zero. Moisture was determined from results
of Method 8 sampling.
6. Flow measurements at Acid Plant 1 were conducted in the
downcomer to the FRP dust (Station 48907) instead of the
originally proposed site (Station 48901).
7. The method 8 train was used at the upstream port at Acid
Plant 1 (Station 48901) instead of the downstream port.
8. Span gases originally intended to be used for Quality
Control checks were used as calibration gases.
9. The TECO analyzer was used to determine dilution rates,
therefore, flow and pressure measurement devices in the
TECO dilution system were not calibrated according to the
procedures initially proposed.
10. No QC check of the Bunker Hill S02 monitors was conducted
because of the Company's objection.
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APPENDIX C
SAMPLING TRAIN DESCRIPTION
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STACK SAMPLING EQUIPMENT
The Scientific Glass Model AP-5000 modular STAOO-LATUR*'m sampling
train consists of a control unit, a sampling unit and a vacuum unit. The
units are connected together with quick disconnect electical and air lines,
and umblical cords.
The AP-500 control unit contains the following
1. Dual-inclined manometer (range 0-5" H20) for indicating the
pitot tube velocity pressure and the orifice pressure drop.
2. Temperature controls for the oven and probe.
3. A flow valve and a bypass valve for adjusting sampling rates.
4. Digital Temperature Indicator (DTI) which give an instant
readout from six (6) points; stack, probe, oven, impinger
outlet, meter inlet, meter outlet by the use of a selector
switch.
5. Umbilical cords (50 and 100 ft lengths) which interconnect
the control and sampling units.
6. Communications sets are wired through umbilical cord from
control unit to the sampling unit.*
The sampling unit is made up of three distinct sections; impinger
case, oven and probe. All three sections can be converted to form one
sampling unit or can be separated for unusual sampling conditions. Below
are the individual component descriptions:
1. Probe Sheath - Made of 316 stainless steel. The nozzle end
is packed with asbestos string. The ball joint (sampling
unit) end has a woven telfon 0 Ring as packing material.
* Separate communication system used during this test program.
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2. Probe liner - 5/8" O.D. medium wall glass (pyrex) or stainless
steel (316) tubing logarithmically wrapped with nicrome heating
element, having a resistance of 2 ohms/ft. The liner is insu-
lated with fiberglass and asbestos with a type K thermocouple
imbedded for sensing the probe temperature.
3. Filter Frit - Porous glass frit (coarse) banded to silicone
rubber.
4. Oven - Fiberglass insulated capable of maintaining 120°C
(248°F) in cold weather (0°C).
The vacuum unit (pump) is capable of drawing a high vacuum (50 cm Hg)
and a moderate volume (14 1pm) of air. The pump is rotary fiber vane type
which does not require lubrication, but oil bath filters are used for pump
protection.
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APPENDIX D
CHAIN-OF-CUSTODY
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ENVIRONMENTAL PROTECTION AGENCY
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
CHAIN OF CUSTODY PROCEDURES
June 1, 1975
GENERAL
The evidence gathering portion of a survey should be characterized by the minimum
number of samples required to give a fair representation of the water, air or solid
waste sampled. To the extent possible, the quantity of samples and sample locations
will be determined prior to the survey.
Chain of Custody procedures must be followed to maintain the documentation necessary
to trace sample possession from the time taken until the evidence is introduced into
court. A sample is in your "custody" if:
1. It is in your actual physical possession, or
2. It is in your view, after being in your physical possession, or
3. It was in your physical possession and then you locked it up in a manner so
that no one could tamper with it.
All survey participants will receive a copy of the survey study plan and will be
knowledgeable of its contents prior to the survey. A pre-survey briefing will be held
to re-appraise all participants of the survey objectives, sample locations and Chain
of Custody procedures. After all Chain of Custody samples are collected, a de-briefing
will be held in the field to determine adherence to Chain of Custody procedures and
whether additional evidence type samples are required.
SAMPLE COLLECTION
1. To the maximum extent achievable, as few people as possible should handle
the sample.
2. Water, air, or solid waste samples shall be obtained, using standard field
sampling techniques.
3. Sample tags (Exhibit I) shall be securely attached to the sample container
at the time the complete sample is collected and shall contain, at a minimum,
the following information: station number, station location, data taken,
time taken, type of sample, sequence number (first sample of the day -
sequence No. 1, second sample - sequence No. 2, etc.), analyses required and
samplers. The tags must be legibly filled out in ballpoint (waterproof ink).
4. Blank samples shall also be taken with preservatives which will be analyzed
by the laboratory to exclude the possibility of container or preservative
contamination.
5. A pre-printed, bound Field Data Record logbook shall be maintained to re-
cord field measurements and other pertinent information necessary to refresh
the sampler's memory in the event he later takes the stand to testify re-
garding his actions during the evidence gathering activity. A separate
set of field notebooks shall be maintained for each survey and stored in a
safe place where they could be protected and accounted for at all times.
Standard formats (Exhibits II and III) have been established to minimize
field entries and include the date, time, survey, type of samples taken,
volume of each sample, type of analysis, sample numbers, preservatives,
sample location and field measurements such as temperature, conductivity,
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2
DO, pH, flow and any other pertinent information or observations. The
entries shall be signed by the field samplei. The preparation and conser-
vation of the field logbooks during tne survey will be the responsibility
of the survey coordinator. Once the survey is complete, field logs will be
retained by the survey coordinator, cr his desjgnated representative, as a
part of the permanent record.
6. The field sampler is responsible for the care and custody of the samples
collected until properly dispatched ".o the receiving laboratory or turned
over to an assigned custodian. He njst assure that each container is in his
physical possession or in his view a: all times, or locked in such a place
and manner that no one can tamper witn it.
7. Colored slides or photographs should De taken which would visually show the
outfall sample location and any water pollution to substantiate any con-
clusions of the investigation. Written documentation on the back of the
photo should include the signature or the photographer, time, date and site
location. Photographs of this nature, which may be used as evidence, shall
be handled recognizing Cham of Custody procedures to prevent alteration.
TRANSFER OF CUSTODY AND SHIPMENT
1. Samples will be accompanied by a Chain of Custody Record which includes the
name of the survey, samplers' signatures, station number, station location,
date, time, type of sample, sequence lumber, number of containers and analy-
ses required (Fig. IV). When turning over the possession of samples, the
transferor and transferee will sign,"sate and time the sheet. This record
sheet allows transfer of custody of 2 group of samples in the field, to the
mobile laboratory or when samples are dispatched to the NEIC - Denver labora-
tory. When transferring a portion 0: the samples identified on the sheet to
the field mobile laboratory, the indi/idual samples must be noted in the
column with the signature of the person relinquishing the samples. The field
laboratory person receiving the samp'es will acknowledge receipt by signing
in the appropriate column.
2. The field custodian or field sampler, if a custodian has not been assigned,
will have the responsibility of prope-ly packaging and dispatching samples
to the proper laboratory for analysis. The "Dispatch" portion of the "Chain
of Custody Record shall be properly filled out, dated, and signed.
3. Samples will be prpperly packed in shipment containers such as ice chests, to
avoid breakage. The shipping containers will be padlocked for shipment to
the receiving laboratory.
4. All packages will be accompanied by t~.e Chain of Custody Record showing iden-
tification of the contents. The original will accompany the shipment, and a
copy will be retained by the survey coordinator.
5. If sent by mail, register the package with return receipt requested. If sent
by common carrier, a Government Bill of Lading should be obtained. Receipts
from post offices, and bills of ladir; will be retained as part of the perma-
nent Chain of Custody documentation.
6. If samples are delivered to the laboratory when appropriate personnel are not
there to receive them, the samples n„3t be locked in a designated area within
the laboratory in a manner so that no one can tamper with them. The same per-
son must then return to the laboratory and unlock the samples and deliver
custody to the appropriate custodian.
-------
3
LABORATORY CUSTODY PROCEDURES
1. The laboratory shall designate a "sample custodian." An alternate will be
designated in his absence. In addition, the laboratory shall set aside a
"sample storage security area." This should be-a clean, dry, isolated room
which can be securely locked from the outside.
2. All samples should be handled by the minimum possible number of persons.
3. All incoming samples shall be received only by the custodian, who will in-
dicate receipt by signing the Chain of Custody Sheet accompanying the samples
and retaining the sheet as permanent records. Couriers picking up samples at
the airport, post office, etc. shall sign jointly with the laboratory custodian.
4. Immediately upon receipt, the custodian will place the sample in the sample
room, which will be locked at all times except when samples are removed or
replaced by the custodian. To the maximum extent possible, only the custo-
dian should be permitted in the sample room.
5. The custodian shall ensure that heat-sensitive or light-sensitive samples,
or other sample materials having unusual physical characteristics, or re-
quiring special handling, are properly stored and maintained.
6. Only the custodian will distribute samples to personnel who are to perform
tests.
7. The analyst will record in his laboratory notebook or analytical worksheet,
identifying information describing the sample, the procedures performed
and the results of the testing. The notes shall be dated and indicate who
performed the tests. The notes shall be retained as a permanent record in
the laboratory and should note any abnormal ties which occurred during the
testingprocedure. In the event that the person who performed the tests is
not available as a witness at time of trial, the government may be able to
introduce the notes in evidence under the Federal Business Records Act.
8. Standard methods of laboratory analyses shall be used as described in the
"Guidelines Establishing Test Procedures for Analysis of Pollutants,"
38 F.R. 28758, October 16, 1973. If laboratory personnel deviate from
standard procedures, they should be prepared to justify their decision dur-
ing cross-examination.
9. Laboratory personnel are responsible for the care and custody of the sample
once it is handed over to them and should be prepared to testify that the
sample was in their possession and vie'./ or secured in the laboratory at all
times from the moment it was received from the custodian until the tests
were run.
10. Once the sample testing is completed, the unused portion of the sample to-
gether with all identifying tags and laboratory records, should be returned
to the custodian. The returned tagged sample will be retained in the sample
room until it is required for trial. Strip charts and other documentation
of work will also be turned over to the custodian.
11. Samples, tags and laboratory records of tests may be destroyed only upon the
order of the laboratory director, who will first confer with the Chief,
Enforcement Specialist Office, to make certain that the information is no
longer required or the samples have deteriorated.
-------
EXHIBIT I
EPA, NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Station No.
Dato
Timo
Scquenco No. *
Station Location
CiraU
Crimp.
.BOD
.Solids
.COD
_NulrienIj
Samplers.-
_Molafj
_Oil oriel Grease
_D.O.
_Bact.
_Ol'ner.
Romarks/Proiorvalive:
Front
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
£ ^ \
Back
-------
EXHIBIT'II
SURVEY, PHASE.
DATE
OF SAMPLE.
JION
M8ER
Analyses required
STATION DESCRIPTION
UJ
5
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>-
PRESERVATIVE
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a.
-------
EXHIBIT III
Somplors: __________________
FIELD DATA RECORD
STATION
NUMBER
DATE
TIME
TEMPERATURE
•c
CONDUCTIVITY
fx mhos/cm
pH
S.U..
D.O.
rng/1
Gage Hf.
or Flow
Ft. of CFS
•
1
•
i
-------
EXHIBIT IV
environmental protection agency
Office Of Enforcement
National enforcement investigations center
Building 53, Bo* 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
STATION
NUMBER
STATION LOCATION
date time
SAMPLERS: (s.gno/ur«;
sample irpE
Water
Comp Orob
Air
SEQ
NO.
NO OF
CONTAINERS
ANALYSIS
REQUIRED
Relinquished by: (s.SnotUre)
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Dispatched by: (s.gnoiure)
Method of Shipment:
Received by: (Signature)
Received by: (Signoture)
Received by: (Signature)
Received by Mobile Laboratory for field
analysis: (SignatureJ
Date/Time Received for Laboratory by:
Distribution: Orin -Accomnnm,
Dale/Time
Date/Time
Dale/Ti
inn
Dale/Time
Date/T
ime
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
L j
r'vji J Y- \r iC W\L V_
SAMPLERS: (Signature)
' , /
/ /V-V f f /' '*¦ £
STATION
NUMBER
STATION LOCATION
DATE
TIME
/ SAMPLE type
NO OF
CONTAINERS
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RfcOUIRED
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SEO
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Method of Shipment:
te'O. K
589 01
Distribution Orig — Accompany Shipment
1 Copy—Survey Coordinator Field Files
•CPO 679-010
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY St-UO^-
/^{VA//:.^9c1 a// CL. / hfo
SAMPLERS: {SignatureI
STATION
NUMBER
STATION LOCATION
DATE
SAMPLE TYPE
TIME
Woler
Comp Grab
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NO
NO OF
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489 04
Distribution ^ Orig — Accompany Shipment
* 1 Copy—Survey Coordinator Field Files
•GPO 679-040
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
r>
h'/L-L
SAMPLERS: (Signature) , j
/
SUTION
NUMBER
STATION LOCATION
DATE
TIME
SAMPLE TYPE
SEO
NO
NO OF
CONTAINERS
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489 00
Distribution. Orig — Accompany Shipment
1 Copy—Survey Coordinator Field Files
•GPO 679-040
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
-/?LL.
SAMPLERS. 1Signaturel ' t
A ¦
SIAIION
NUMBER
SIAIION IOCAIION
DATE
TIME
SAMPLE TYPE
SEO
NO
NO OF
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Date/Time
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Method of Shipment:
/A o. u
489 00
Distribution Orig — Accompany Shipment
1 Copy—Survey Coordinator Field Files
»GPO 679-040
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
SAMPLERS: /Signature]
*df,wA
STATION
NUMBER
STATION LOCATION
DATE
TIME
SAMPLE TYPE
SEO
NO
NO OF
CONTAINERS
ANALYSIS
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-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
/^oi'/rra M/LL
STATION
NUMBER
STATION LOCATION
DATE
TIME
SAMPLERS. (Signature)
Oo<&Q
&'
Sample type
Wale
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SEO
NO
NO OF
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40S 07
Distribution Ong — Accompany Shipment
1 Copy—Survey Coordinator Field Files
»GPO 679-040
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
SAMPLERS: (Signature) ,
STATION
NUMBER
STATION LOCATION
DATE
TIME
Sample type
SEQ
NO
NO OF
CONTAINERS
ANALYSIS
RtOUIRED
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Distribution Orig. — Accompany Shipment
1 Copy—Survey Coordinator Field Files
»6PO 679-040
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
t-iGAJKFR Mill ia-u.^64*,idah-v
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SEQ
NO
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489 15;
Distribution Orig — Accompany Shipment
1 Copy—Survey Coordinator Field Files
GPO 6 79 -OA 0
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
U;;-U O K-f1-— ^ i L (—
SAMPLERS: (Signature)
/~ ' .v / (
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STATION
NUMBER
STATION LOCATION
DATE
TIME
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NO OF
CONTAINERS
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-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
Pv >Q
M
I L(
SAMPLERS: (Signature/
STATION
NUMBER
STATION LOCATION
DATE
TIME
SAMPLE TYPE,'^'
SEO
NO
NO OF
CONTAINERS
ANALYSIS
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-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
u*-* }vrL >< /^> i L
SAMPLERS. (Signature)
A' . i
STATION
NUMBER
STATION LOCATION
DATE
TIME
sample type
NO OF
CONTAINERS
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analysis* (SignatureJ
Date/Time
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Date/Time
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Date/Time
/{)
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
/° Li.
SAMPLERS: (Signature)
A
we.
STATION
NUMBER
STATION LOCATION
DATE
SAMPLE TYPE
TIME
Water
Comp
G rob
SEO
NO
NO OF
CONTAINERS
ANALYSIS
REQUIRED
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\ |
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
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Date/Time
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Method of Shipment
G.Ob'
Distribution Orig — Accompany Shipment
489 18 1 Copy—Survey Coordinator Field Files
*GPO 679-040
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
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Denver, Colorado 80225
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Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
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Office Of Enforcement
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Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEV fj. 1. —. e«
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-------
APPENDIX E
TECO ANALYZER DESCRIPTION*
* Obtained from Instrumentation for Environmental Monitoring published
by the Lawrence Berkeley Laboratory, University of California,
Berkeley, California.
-------
INSTRUMENTATION AIR-S02
XBX- FOR ENVIRONMENTAL Source
M Thermo Electron 1
MONITORING March 1976
Stationary Source Monitor
Model 40 S02 Analyzer
PULSATING
ULTRAVIOLET
LIGHT
Class Stationary
Principle Pulsed Ultraviolet Fluorescence: Gas sample is illuminated by a pulsed xenon
of Operation are lamp attenuated with a monochromatic UV filter. The excited SO? molecules
subsequently emit longer wavelength UV radiation which is transmitted
through a guard filter to a photomultiplier. The output signal from the de-
tector is linear with SO2 concentration. Optional sulfur converter ox-
idizes H2S and other reduced sulfur compounds to SO2 by means of a low-
temperature catalytic process.
Lower Detectable 1 ppm
Limit
Range
5000 ppm
-------
(r'O
INSTRUMENTATION
FOR ENVIRONMENTAL
MONITORING
AIR-S02
Source
Thermo Electron ]
Page 2 March 1976
Interferences
INTERFERENCE DATA SUMMARY
Interferent
Concentration
ppm
Interference
Equiv., ppm
h7s
0.100
0.00g
NO,
0.500
0.00s
NO
1,000.0
2.0a'g
C°2
750.00
0.008
°3
0.500
0.00&
M-Xylene
0.194
0.0058
CO
50.0
0.005S
-0.005*
-0.0031
0.00
.Observed at 954 relative humidity.a,g
Calculated from quenching constants,f for 80% rela-
tive humidity.8
^Observed at 801 relative humidity.g
Multiparameter
Capability
Sampling
Performance
Operation
Requirements
Features
1% in 24 hrse
21 in 24 hrse
S02(H2S and other reduced sulfur compounds, with optional converter)
Method: Extractive. Gas sample is dehumidified with a permeation dryer
Volume: 0.4-1 liter/min (1-2 scfh)
Maximum Temperature Input: 50°C
Collection Efficiency: 10%
Accuracy: ± 0.5% relative to calibration gasa>c
Precision-± 0»5% full scale
Repeatability: ± 0.5%
Linearity: ±1% full scale
Noise: 0.5%
Lag Time: 10 sec*
Rise Time: 4 sec (90%)
Retention Time:
Fall Time: 4 sec (90%)
Zero Drift: <1% in 7 days,a
Span Drift: <1% in 7 days,3
9 #
Ambient Temperature Range: 0 C to 40 C
Temperature Compensation: None required
Relative Humidity Range: 0-100%
Calibration: External
Procedure:
Warm-up Tune: 20 min.
Unattended Period: 7 days to 1 month, depending on frequency of calibration
Maintenance: Replacement of particulate filter. Xe lamp life is over 1 year
during continuous operation.
Power: 150 watts at 115V AC (60Hz)
Weight: 40 pounds
Dimensions: 17 "W x 9"H x 23"D
Output: Analog display, also 0.1 V output
Training: No special training required. Instruction manual included
Options: sulfur converter (converts H2S) and other reduced sulfur compounds
to SO2•)External timer for automating sequence of zero, span, and
measurement.
-------
instrumentation
FOR ENVIRONMENTAL
MONITORING
AIR-S02
Soui ce
Thermo Electron 1
Page 3 March 1976
References
Cost^
Remarks
Address
(a) Manufacturer's Brochure RA-1-20M-675.
(b) Schwartz, F. P., Okabe, M., and Whittaker, J. K., "Fluorescence De-
tection of Sulfur Dioxide in the Air at the Parts per Billion Level",
Anal. Chem. 46, 1024-1028 (1974).
(c) W. J. Mager, D. J., and Helm, D, A. "Source Level SO2 Analysis via
Pulsed Fluorescence," Report ISA Aid 74402, pp. 9-18, presented at
APCA Meeting, Pittsburgh. Pennsylvania (August 1974).
(d) Zollner, W. J., personal communication, (July 9, 1975).
(e) Shen, T. T., Chem. Eng. 82, 109 (May 26, 1975).
(f) Okabe, H., Splitsome, P. L., and Ball, J. J., J.APCA 23, 514 (1973).
(g) Warner Carlson, private communication, June 25, 1976.
Model 40: $5950; catalytic sulfur converter: $2000; Timer: $100-800.00.
The pulse length of the Xe source is approx. 10 ijsec. Advantages of the Xe
arc lamp include its long working life compared to other UV sources. The
range limitation for this S02 monitor (Ref. C) is the result of absorption
"self" quenching by S02, which begins to become important at levels above
5000 ppm. Other workers (Ref. b) observed self quenching, at concentrations
on the order of 1600 ppm SO^, using a different excitation source. Dehumid-
ification of gas stream minimizes S02 fluorescence quenching by water (b,c)
"In situations where more accurate measurements are desired, emission
spectrographic techniques (Model 40) should be employed."e
Thermo Electron Corporation (TECO)
Environmental Instruments Division
85 First Avenue
Waltham, Massachusetts 02154
f6171 890-8700
-------
APPENDIX F
CALIBRATION DATA
-------
NEIC Procedure for Pi tot Tube Calibration
Introduction
The Type-S pitot tube is used by NEIC to measure stack gas
velocity during source sampling. The pitot tube coefficient.(Cp)
of this instrument is determined by calibration against a trace-
able National Bureau of Standards (NBS) standard pitot tube. The
Type-S pitot tube is calibrated on a probe sheath with a ^ inch dia
nozzle attached. All pitot tubes are calibrated from 305 m/min
(1000 ft/min) to 1524 m/min (5000 ft/min). Pitot tubes used during
tests will subsequently be recalibrated at a minimum of 3 points
within the velocity range observed during testing. Tubes which have
been damaged or suspected of being damaged during field use will be
recalibrated over the entire range (i.e. 305 to 1524 m/min).
I. Equipment Required
A. Flow System - Calibration is performed in a f»low system
meeting the following minimum requirements:
(1) The air stream is confined in a well-defined cross
sectional area, either circular or rectangular.
The minimum size is 30.5 cm (12 inches) diameter
for circular ducts and at least 25 cm (10 inches),
as the shortest dimension for rectangular ducts.
(2) Entry ports provided in the test section, shall be a
minimum 'of 8 duct diameters downstream and 2 diameters
upstream of any flow disturbance, e.g. bend, expansion,
contraction, opening, etc.
-------
-2-
(3) The flow system must have the capacity to generate over
the range of 305 m to 1524 m (1000 ft. - 5000 ft.)/min.
Velocities in this range must be constant with time to
guarantee steady flow during calibration.
B. Calibration Standard
A standard type pi tot tube either calibrated directly
by N.B.S. or traceable to an N.B.S. standard shall be
the calibration standard.
C. Differential Pressure Gauge
An inclined or expanded scale manometer shall be
used to measure velocity head (aP). Such gauges 3iall be
capable of measuring AP to within + 0.13 mm (0.005 inches)
H2O. A micro-manometer capable of measuring with 0.013 mm
(0.0005 in) H20 will be used to measure AP of less than
13 (0.5") H20.
D. Pi tot Tube Lines
Flexible lines made of tygon or similar tubing shall
be used.
E. Thermometer
A mercury in glass or other type thermometer checked
agains a mercury in glass thermometer is considered suitable.
F. Barometer
A mercury column barometer shall be available to determine
atmospheric pressure.
II. Physical Check
1. The openings are sharp and do not have a rolled edge.
2. The impact planes of sides A & B are perpendicular to
the Traverse Tube axis [Figure 2].
-------
-3-
3. The impact planes are parallel to the longitudinal tube axis
[Figure 3].
III. Calibration Procedure
The Type-S pitot tube shall be assigned an identification
number. The first digit of the number is the effective length of
the tube, followed by a dash and consecutive numbers for the number
of tubes of the same effective length, i.e. 5-1 signifies a five
foot pitot tube and is the number one tube. Calibration proceeds
as follows.
A. Fill manometer with clean oil of the proper specific gravity.
Attach and leak check all pitot tube lines.
B. Level and zero monometer.
C. Position the standard pitot tube in the test section at
the calibration point. If the flow system is large enough
and does no interfere with the Type-S tube the standard
tube may be left in the system.
D. Insert the Type-S tube into the flow system.
E. Checks for the effect of turbulance are made as follows:
1. Read AP on both Type-S and standard pitot tubes with
the standard pitot tube in place and compare with read-
ings when the standard tube is withdrawn from system.
2. Read aP on the Type-S tube at centerline of flow system,
then take readings while moving the tube to the side
of the system. This will define the boundary turbulance
layer.
3. Position the Type-S tube so that there impact openings
are perpendicular to the duct cross sectional area and
-------
-4-
check for null (zero) reading. Absence of a null reading at
this position indicates non-laminar flow conditions..
F. Read AP ^ and record on data table.
G. With the Type-S "A" leg orientated into the flow read aPs
and record on data table.
H. Repeat steps F and G until three sets of velocity data
have been obtained.
I. Remove Type-S pi tot tube arid rotate probe nozzle until it
aligns with side "B" impact openings.
J. Insert the Type-S pi tot tube and proceed as in steps F through
H.
K. Adjust flow system to new volocity and repeat F-J.
L. Record air temperature in the test system and barometric
pressure during testing.
IV. Calculations
1. At each "A"-side and "B"-side velocity setting, calculate
the three valves of Cp (s) as follows:
Where:
CPs ~ Type-S pi tot tube coefficient
Cp ^ - Standard pi tot tube coefficient !(NBS)
AP gtd - Velocity head, measured by Standard
pi tot tubing inches H2O
aPs - Velocity head, measured by the Type-S
pi tot tube, inches H^O
2. Calculate Cp, the average (mean of the three Cp(s)
valves.
-------
-5-
3. For each CP calculated in step 2, calculate a, the average
deviation from the mean as follows:
1
c(Side "A" or "B") = Cp (s) - Cp (A or B)
3
3
4. The pi tot is acceptable if:
(a) The "A" and "B" side average deviations calculated by
equation 2 are <_ 0.01.
(b) The difference of the "A" and "B" sides Cp calculated
by equation 1 is £ 0.01 for each individual velocity.
5. Calculate the test section velocity as follows:
V = KCp /T aP std
V—pm
PM
Where:
V = Average test-section velocity, ft/min
K = 5130 (constant)
Cp = Coefficient of standard pi tot tube
T = Temperature of gas stream °R
P = Barometric pressure, inches Hg
M = Molecular weight of air = 29.0
AP std = Average of the three standard pi tot
tube readings, inches h^O
V. Record Keeping
Flow system data and information on each pitot tube shall
be recorded in a bound book.
The flow system data shall include:
1. The tunnel cross-sectional area and length
up-stream and down-stream of the test site )ft.)
from disturbances.
-------
-6-
2. Time tunnel used (hrs)
3. Air temperature (°F) in flow system and barometric
pressure (inches Hg).
4. All checks for turbulance and flow distribution.
5. Velocity range (ft/min).
The pi tot tube information shall include:
1. I.D. number
2. Checks for physical damages, errors noted and
modifications.
3. Dates and surveys pi tot tubes were used.
4. Date of calibrations, coefficient and dates of
re-calibration.
The calibration records will be kept on file at NEIC. Copies of
the appropriate calibration dates will be furnished for each source
test project.
-------
SB
>
•A
^V
C=3
1
i>
I
±
Figure 1. Measurement of Type-S pitottube length (dimension "a'11) and impacvpiane
separation distance {dimension "b").
TRANSVERSE
TUBE AXIS
.IMPACT—>
PLANES (
'Figure 2. Type-S pitotitube, endt
'view; impact-opening planes per-
pendicular to transverse tube axis..
LONG ITU PINAL
' TUBE AXIS
A-S1DE PLANE
B-SIDE PLANE.
Figure 3. Type-S tube, top view; impact-open-
ing planes parallel to longitudinal tube axis.
From "A TYPE-S PITOT TUBE CALIBRATION STUDY" by
Robert F. Vollaro, October 15, 1975
-------
FOPM NHS-4-13
(Rtv !*-«)
U.S. DEPARTMENT OF COMMERCE
NATIONAL. EUREAU OF STANDARDS
WASHINGTON, D.C. 20234
-."i -7
NEM:pg
TN C-42979
213.08
2130608
REPORT OF CALIBRATION
March 24, 1976
on
Airflow Pitot-Static Tube
12" x 4 mm
submitted by
Environmental Protection Agency
National Enforcement Investigations Center
Denver Federal Center
Denver, Colorado 30225
Reference: Order No. WV-6-99-0516-H dated February 23, 1976.
The calibration was performed in the five-foot by seven-foot rectangular
test section of the NBS closed-circuit dual test section wind tunnel. The
tunnel provides an essentially uniform air stream with a very low turbu-
lence intensity. The tube under test was inserted into the air stream
through a hole in the tunnel wall and held in place by a clamping arrange-
ment with all fittings outside the tunnel. The tube was alined with the
flow and positioned so that the static holes were-approximately 8-1/2
inches from the tunnel sidewall. The boundary layer on the tunnel wall
was approximately 1.6 inches thick.
Calibration of the tube consisted of determining the calibration factor
K where K is defined as the ratio of the differential pressure indicated
by the tube under test to the differential pressure indicated by the NBS
laboratory standard. This was done by a direct comparison in which the
tube under test and the NBS tube were mounted in the tunnel, 16 inches
apart, and at the same distance from the tunnel sidewall.
The calibration factor K for a tube of this type may be dependent on
the Reynolds number per unit length, V/v, where V is the air speed and
v is the kinematic viscosity. This parameter is therefore given in the
attached table, along with the corresponding values of V in the units
requested, as the properties of the gas in which this instrument is
used may be an important consideration. The values of K tabulated are
the average of four independent determinations at each of the corresponding
values of V/\>.
For the Director,
ff, Chief
Aerodynamics Section
Mechanics Division, IBS
-------
TN G-42979 - 213.08
2130608 — 3/24/76
Page 2.
Table 1
Airflow Pitot-Static Tube
12" x 4 mm
Reynolds Number Per Meter True Air Speed K
V/ x 10" , m~ m/s
0.046 0.7 ].09
0.072 1.1 l.O
0.098 1.5 0.97
0.124 1.9 0.98
0.182 2.8 0.99
0.243 3.8 0.98
0.395 6.2 0.990
0.553 8.6 0.992
0.868 13.6 0.997
1.181 18.5 0.998
1.489 23.4 0.999
1.798 28.3 0.998
2.111 33.4 0.998
2.423 38.5 0.999
3.027 48.6 0.998
-------
liS Fnvironm-2ntnl Protection Agency
National Enforcc-irnt Investigations Center-Denver
Calibration Pi tot Tube: ID Number [2 5 !
Type-S Pitot Tube ID Number: ^- ~X
CP .
^.p
Standard
Pitot
7k, on
a oo
LSH
So
i, on
i - oo
75
j -CL£0
i
o
n^s.
10
¦Ap S-Type Pitot
A leg
"3 ^
3. 00
"3 00
¦3 ¦
2.3.C
L ip£T
,k££
USE"
U5
_US_
B leg
3.:on
3, 0 0
3,oo
a
..SO
Cp
A
10^
¦ ¦so#
B
MX-
• KQS
im.
> ftcm
22£.
¦ 79 s"
LL£
7*?T
115.
07b
n.7U
0 7k
0- ^
JS1
I./.S-
mu
0- 76.
i") 7k
r>..^
Q-33
0-3 ft
Q-3^
• 7??
JSi
• ftps
¦ KQZ
7^5"
¦7^7
jzss:
¦ 7^
J¥L
23±
¦ <<03
M:
m
7-79
-K03
¦ tot
o
.^0 7
.*0?
T- 7i. V-
ft =-62.? ,•>7 ^
6z4--fcxS)
Comments
During Pitot Calibration:
probe sheath attached k^Q
nozzle attached fy^C?
sampling'isokinetical ly
Performed By:
-%o?>
• %Q%
Leg Average Cp
Calibration Date:
-------
PITOT TUBE CALCULATION SHEET
Tube ID Number Calibration Date (e/Hlfr
By Checked By\
/'
£P
Std Tube
.r
EP"
a
diff
.OOO
(Test Section)
A I B
A 1 B
f.^o
S3H on 3
.ST7
.5*17
• OOO
.OOO
I.DO
S08
Vol?
¦ ODO
,OOO
« OOO
OHiob
- &So l
,?ojf
• OoO
. OOO
. OOO
O, 5bo
30^3^1
¦ to?
,?l O
> 001
.£>6 \
,oo|
o. O-^O
P-I3(= 2? '
• ?o?'
.tot
.DOO
,000
.000
o, no
IWL.HV
.7 ?C
,i?L
.ODO
. OOO
il 15, 1976
-------
US KnvironmcDUtl Protection Agency
national Enforcement InvesLicjations Center-Denver
Calibration Pitot Tube:ID Number hJ/3^" /
Fype-S Pitot Tube ID Number: jf-2-
cp_
.9?
$ -- U3i #3
(XSfc £>*)
AP
Standard
Pitot
.aP S-Type Pitot
c
)
7T- 7/^"V
Comments
A leq
B leq
A
B
/So •
•2-AO
$.£o ¦
.?/7
.8-17
2O
j2.l2o
. S77
.917
/.So
20..o
$.zo
,?/7
.5/7
/. DO
/,So
/-So
.¦gb?
/,So
/'So
,?og'
Aoo
/.So
/.So
,w
0,7(oO
/'. L<
US'
¦ f/s
SIS'
.?05-
• Sk5"
0.7bD
//JT
//S
•cftd"'
$05
O.Soo
¦nSo
• 75o
.swir
• Stog*
.7/50
¦~7L/S'
¦9<%
.?//
) O. Soo
.7
' .7465"
.87/
.{?//
o. MO
<300
">3Lo
."fo?
¦3lc£
• 3bo
?o?
O. MO
3(cO
.3LO
•5fc9*
.eb?-
n.no.
J7o
.17 a
n?t,>
...
>/7o
¦ 17 o
,7?6
•7%,
D.ffO
>nc>
, no
•7ft
. 7%,
n4-rvi- -.i • l_ _ i_ • _ .
¦ 9^7
• 9o7
Leg Average Cp
probe sheath attached ,
nozzle attached a/n
sampli ng * i sok i net i cal ly
'Performed By:_
Calibration Date:
-------
US F.rmronmental Protection Agency
Nat'onal Enforcement Investigations Center-Denver
Calibration Pitot Tube:ID Number
Type-S Pitot Tube ID Number:
cp $ ¦ 9 ?
^p
Standard
Pitot
fir /0
' /g
^P S-Type Pitot
A leg
o-
B leg
Cp
n./<
-0' /»c._
O ^ /Pi4
JJL
0-V7
221.
r> 77/
XhJU-
Q' ?
J 'fZ')'
&-% I)
S3 ¦ ,?Xo'.7
d ' #<2
O I XT.
/. 3L O
jCl
LI
/¦£<-
/•So
/ 7^
/' 7 f
&.7C/
O'fo
/ 2^
J.3LS
/
J-22A1_
M2S.
7>7S
6 -*r\ 3
n
n • $'
0 - *? 3o
f> • * M ¦'
6 '$}f-
O-Key
#- *0-
0 r* * o
£ey& 6 ^ . £e uJL / & **
/ / /*<«* ^
SH j
— r'
During Pitot Calibration:
probe sheath attached Cf/s
nozzle attached nPs. / ,/j -
sampling isokinet^caliy JJJ
Performed By:
o,qcC
O-boC
Leg Average Cp
0 ; V, /
Calibration Date: ^ '7 7
-------
rnvironm-jiiuti troiecuun Agency
tioiml Enforcement Investigations Center-Denver
libration Pitot Tubc:ID Mumbcr_
-S Pitot Tube ID Number:
^3
zL
Cp
,??
^ p
Standard
Pitot
-a P S-Type Pitot
c
)
(-am i-1)
Consents
A leq
B leq
A
B
3-00
3/0
3dfT
. 8b #¦
3 fO
3 to
.79£~-
mf'
2-DO
j3olT ¦
m?-
,9oX
/
2 3^'
^jT
.!?(>
n?f<
^•3
X3^
¦19/
.19/
/On
/ Go
/
.7 S3
111
/l179- ¦
¦119-'
0,-74,0
AX^
. /rZO
,112-
¦m-
C 5bo
• onuo
onsa
.?0?'
O.KoO
on
¦ *$£>3^
¦ °&o$ -
0>.^ba
D.1L&
£>1^0
¦ ?o3s
¦ ?0$.
0 L/oo
bMoo
.7»3-
Cl'icXln [^fiss&criebz-JL
o-
O./0O
0./60
¦1L1 *
. "767,-
roL&
O. /DO
D./OO
r?Ll>
<¦10-
'
'
^ n¦:4-^a- n\ x. •
r>W<
l$i»~
Leg Average Cp
probe sheath attached
nozzle attached
sarr.pl ing'i soki net ical 1 y
"lllL,cI Sy. sf] Calibration D?.te: ^3/P//^
. / // " / ~ ^
/ ** >
/
-------
FITOT TUBE CALCULATION SHEET
Tube ID Number
By.
Calibration Date
Checked By
—
AP
Std Tube
.r
(Test Section)
A 1 D
a
diff
. ool ,
£ oo
.793-
D
.¦3too
rt 1
.oo3
b
.003
/ So
' 5330.60
^3^3.10 '
. 17?'
.77/-
, oofT'
.000
0 '
,00% V
0.7 CO
3111. Lo '
.713~-
,7?.3,
.ODO .
•ool,
.OH y
• O.$bo
3017-23 -
. fo3>''
, OOO..
,000
. 0o5"~ j
0'9^c>
d~\7L-3'£^
¦ 783'
.7 83.
.OOO
. DOO
~~7 >
¦71,1.
, oco.
.DbO
.OOO
•
-
¦ /¦
1
pril 15, 1976
-------
tiS Fnvironmental Protection Agency
National Enforce-lrrit Investigation: Center-Denver
Calibration Pitot Tube:ID Number
Type-S Pitot Tube ID Number:
J&rs-j CP . 99
¦r< 7/a
A p
Standard
Pitot
-Ap S-Type Pitot
c
p
Lpcr^f 1*1 C1^ {^/v rr^
O^TS^)
Comments
A leq
B Ten
A
B
•3 do
^/
n9?
/rOO
/•(oO
)-(* 0
,7^3
rm
f'(oO
/.GO
r#3>-
.its
Ago
¦/•CoO
/¦60
r?fr3-
n$3
on
•7?3
; o. go
£.57 '
b^f'
.77$
1
1
i
o.2l
021
.77?
.77$
~~
( <9.5b
o.9-t
0.91
•77f?
<9. ?-£"
o<-/l
041 ¦
,773
,773
oy/
oH!
7^3
.77,3
O.X<
OV!
om
.773
773
During Pitot Calibration-
,7SV
•7S-V
Leg Average Cp
probe sheath attached
nozzle attached
sampling'isokinetically
- .a/q-
aa-V
Performed Bv:
y^O.aA
///?.
w,U,l
D-t;
'/Mh
o-
0
-------
PHOT TUBE CALCULATION SHEET
Tube ID Number ^3 Calibration Date
Checked By\\ . frJ^^.
AP
Std Tube
.7*
CF
O
diff
(Test Section)
A | B
A | B
£¦¦00
-?$3 I.7S5-?
.OOO
,003
•/.5b *
¦gz^i.-ss-
.?o9-
.-7??
?. 77
,1?3
.OOO
,c>co
. /
" . OOO
on^
33
.~>83
<000
ceo
¦ OOO ¦
i.:
O
o!
1
•1
s&sf. sy* •
.-7*7f
.T73
,000
tCcO
'OOO
1
l
«
r
¦ ¦ .»*¦¦*¦¦¦
April 15, 1976
-------
USJ l"iivironmenlal Protection Ayency
flational F.nrorcemrnt Investigations Center- Denver
Calibration Pilot Tube:ID Number
Type-S Pitot Tube ID Number: .rr-^3
Cp » Y9
Q>kSo(oropf/h
C2V&3L
AP
Standard
Pitot
>2wp S-Type Pitot
c
7'o r
Comments
A leq
B leq
A
B
-.9
<757
,767
a.sb
• 767
,76-7
h£6
;7.-53"
^ •
7^7
¦ 11/7
/CD
/ '
/
nif
'Til
/4jf
/-&jf
nif
•77/
/
/.u^
I (of
\~?7/
.77/
<9. 74o
/or"
/<
,77A
.772
f.Z-i'
/.,£iT
r?iz
¦ 11 X
(9.760
/¦O^
mi.'
¦17?
o.sbo
¦ ?3o
, ffso
nc9
•7fe?
¦ ?3o
nyi
¦ 7C,?
f~>,/Zcc>
•S3 O
>7CS
.17/
• o' -wo
• ,V/C
' . V/c
nsi
,1S1
¦ ytf-S"
. vo/r
.762
nt*x
C- 1X1o
. V/C3
• yo/T
.757
nur.
O. I/O.
. /?£>
.fto-
•70
1&
,/9o
.190
*7£3
•753
o.lID
¦ l?o
>i?o
•7^
¦7_£2>
T\ ^ *i . -i •
*76?
,7£5"
Leg Averacje Cp
j • awwt* vu i i u i l | u i ( •
probe sheath attached
nox.zle attached
ssm.pl ing' i sokin^Ljcal ly
'Performed By:
Calibration Date: ^
-------
PITOT TUBE CALCULATION SHEET
Tube ID Number
x /I
5-J>
Calibration Date
By
')
Checked By
£P
Std Tube
.r
CF
a
diff
. ooff
(Test Section)
A ! B
A | B
'¦ 5b
ni,7
,Oo/
,ooo
A 00
nil
¦ in
. DOO
. OOO
. OCJO
OJLO
. .?3
,172-
.77X
,DOD
, OOO
¦ 'DOC>
O* ^c>a
3o$9>£b
¦ l("9
.oof
rOOf
. ooo
o V-t/o'
£/37°0 •
7)(?o
OOZL
,oo£~
,ooo
' VJfO
.7-53
n£3
,000
.OOO
.ooo>
¦
il 15, 1976
-------
US Environmental Pro Lection A'jency
national F.nforcemsnt Investigations Center-Denver
Calibration Pitot Tube:ID [lumber - n! G> S- 1
Type-S Pitot Tube ID Number:
Cp 'C~i\
£-H.
p ^ c>'1. ° wn M ^
AP
Standard
Pitot
Ap S-T.ype Pitot
c
¦>
Comments
A leq
B leq
A
B
7., o o*
•3 . IS-
3j~2_o •
«~>*n
, ") V3
•
3. i:T
3, i
,")VC1
.IV ^
l.c o
"3. i £"
3,jir
.OVS
I. ^
7.IT" '
T-i^O •
,1°) 1
pss
.
-2. . \«T
. ")S 1
*
i< (a"?
•
•/1 ^ b
7 « ^
n i*~>
•
o
/,
l.\*S
. Its"")
POl
«
0,11
I, -L iT
1.
,~>~n
nil
l,a:T
1.1 IT
< ">")i
*n-n
«
o m
,-r^
0, To
' . Sr/ o
(nSS"~
,T)f^
_
,->s c
o s~o
A J
, V/ o
,-)*) S~~
rnP
.ivs-
<2»i.g
.-IWo
,:W 0
,r>Sn
COlcjQ-O -fV)pr/oomcl"t!£X'^
. "3 35"
,3^ o
V~>$3
-
e.l o
,3Vo
,3rf o
.iw?
1'
O^O
, o
, oS O
,TiV
» 0 °i c
c
nzk
(D < O
,CS C
lO So
.03V
•
r\ .. • n • i. ~ x. ^ • t_ _ l • .
r>"\3>
Leg Average Cp
probe sheath attached
nozzle attached jy
sampling'isokinetical l.y ^ 0
^Performed By: 0- Q
cA ^. Ihl
o Calibrarion Daz
-------
Tube ID Number
PITOT TUBE CALCULATION SHEET
Calibration Date 1X7/7
Checked By
ap
Std Tube
.r
(Test Section)
cf
A 1 D
a
diff
. 00^
3-00
<*'?/¦ 94 '
.799 '
D
.7? 7
H 1
. OOO
b
. oo3
/•5£>
• f&>iV'
,7fV
.for
. OO'-f
.oc>4
. OOO '
<9 ??
43Sx?X
.77/
.767
. 005"
DOO
/
r OOj^
- om
3^1.5?«
.777
.777
. 0OO
.CCD
, OOO
\'OSo
JofSLX '
.77? '
,7S?.5"
Do!
,Oco
.vof '
0.2.00'
/?>T7.S*/
¦1L /
,7^
>Oo3
,00
,00^
o.0
77^-
r)2>Y
.7-3 ST
. OOO
. 00c
, Ooo
¦
.
\pril 15, 1976
-------
t'S Environmental Protection Agency
Nationo.l Enforcement Investigations Center-Denver
Calibration Pi tot Tube:ID Humber
Type-S Pi tot Tubs ID Murnber: "
vj^fr / cp .99
Standard
Pi tot
3 ccr
£oo
/go
m£cl
/•DO
/> OO
0.7gr
one
Q*gh
o.gn
a
p.
7
^ P S-T.ype Pi tot
A leg
¦3-/0
3 /O
3>. /O
B leg
J? /O
P~3o
2-30
2-3 o
/6o
/¦ G?<9
/
/<1Xo
/¦^O
/ 0-n
3./o
9 3o
£-3o
*?-3o
CD
A
t~79/T
7fJT
B
.7??
JS3L
IB2_
/•Go
/Job
/.6 o
/¦2o
/• Po
a
0.?0
<0 fo
<9 */o
D Vo
nMO.
/ 2Q
offo
ofto
o&o
D.t/o
J3S-
¦7to,
.783'
,7£3
•7?3
r?y3
•7?3
.7?^
.222.
.7fl>
rm
,7?3
rr?3
¦785
.723
¦7?3
,7ft3
¦7?3
•7R3
.7^-3
• 7K3
During Pi tot Calibration: /
probe sheath attached a/o
nozzle attached a/A
.7&3
¦7S3
,223
¦783
•7&3
i2£2.
•7g3
¦7?3
¦Tflg'
¦7fr7
ff-CaStifntr* of M,
Comments
Leg Average Cp
sampling' isokinetically
Performed Bv:
tAa.
juh-
Calibration Date:
'i
U.IcVCSE
-------
PITOT TUBE CALCULATION SHEET
Tube ID Number S'H- Calibration Date
By Checked B\jAr)L^Ly£^
l?
Std Tube
.r
(Test Section)
CF
A 1 D
a
diff
, CO^
poo
fclfl.?? '
.7 ?£-
D
n?s
M 1
1 OOO
ts
,00 3
/¦£o
' S3&(,.i
,oco
,000
/
• .OOC2
one
3W39
m3
n?P>
-OOO
.oco
. oco
. . • o. So
3v?2.3
-------
lb I nvironmcnUil Prolecuon Agency
National Lu rorcc:n.-nt InvesLicjai ions CcnLcr- Dc-nvo
Calibration Pitot TubcrlD Number
fype-S Pi tot Tube ID Number: V
Cp ¦ 9?
ft- t>3! W °f f/$
CP.H 9b X^)
^ p
Standard
Pilot
Ap S-T.ype Pi tot
c
Consents
A leq
B leq
A
B
/, /fo •
•a.zS'
%3f.
rft/
2'&o
¦19/
-759
/. 6b
2 3D •
•7?/
¦199
AOO
/ *
/. toO ¦
,7P3
¦ 12$
/Mo
I.IcO
¦TitS.
\W3
/.'CO
(,(nO
t-
, ?/.r
n%">>
.7£3
,%/S
¦m
.7g3
) o.
. §75"
ȣho
¦ ifo
¦ lf\
-
¦ d q£o
* < L/oo
' . L/oo
.Ifft
¦ 7X3,
. ^OD
¦mo
n?3
¦7S3
D.3JZ>
DO
: '-/DO
.-)21
O/oo
,/6o
i fbO
• 7f?3
¦7^
,/bo
JLo"
¦ 7?a
¦ 75?5
JtoO
./Lb
• 7f?"3
• 7£3
n\4-aa *t l •
¦1?3
•7f?3
Leg Average Cp
probe sheath attached a!f>
nozzle attached
A/p
yC/
sampl ing' "i sokingt ical )y
Performed By: jACt^AaJ-?
/
7^52^
Calibration D?.te:
bM/iz
-------
PITOT TUBE CALCULATION SHEET
Tube ID Number
s-i
Calibration Date
Checked fC[(j
£P
itd Tube
. r
CP"
a
diff
.00.5"
(Test Section)
A J B
A 1 B
(.So
SS^o.lQ'
.7 ?f
,7 9L
.OOZJ
.6(W
/. oo
.7 83
,jg3
, ooo
• OOO
,000
0.~)LC>
3>§o\,gt0
ni7~
.773-
t OOO
,OC'D
i
, ooo
o. 5\o
311M. \6~
>7?3
n^x
, Ooo
.00/
, 00 I
-o.%Sb
£l'&0.31/ ¦
.7?3 '
¦!%.?>
, OoO
. Ooo
. 000 '
O. IDO
/378.? 7 "
.7 23
h23
vOCO
,OC.O
,000
¦
i
¦
pril 15, 1976
-------
US Environmental Protection Agency
Nation?.! Enforcement Investigations Center-Denver
Calibration Pi tot Tube:ID Number IV & S - I
Type-S Pi tot Tube ID Number: q - u
Cp ._SSL
p, , 6'ACmin%
Tit ~ 0> (o° f~
A p
Standard
Pi tot
.Ap S-Type Pi tot | Cp
Comments
A leq
B leq
A
B
P-co
3.XO
,7f3
.723
3 XC
¦7P-3
¦ ~)?2>
£ OO
3-ZO
,7f2>
-1$3
/• 57;
9~5<-
p-3^r
,7?/
-7f/
33 -Pe>
o.frl
¦7774
J
O. 0,-cs~o
O.C!?o
O.o£o
•1^3
-"TP"?
( IJ
ri ¦ i x.^ .
0.777
a?7t>
Leg Average Cp
probe sheath attached j/* ^
lozzie attached y< ^
;amp! i n g iso'-;inetjeaily
'"Perrormed Cy: yly—rTl--v^/S Calibration Dare: / ^ /J / 7V
"L?'.
iJCfD.
. -A, ^
-------
PITOT TUBE CALCULATION SHEET
Tube ID Number S ~ Q> ,
Calibration Date / //
Checked By
AP
d Tube
r
(S>Ecti on)
EP"
A 1 n
a
diff
O, o O
*.nc>
2
75C?
- D
O.T^
*
O.nn
y
o. on
To " •
'S3U7f7
0 79/
n.7$v
O.on
O.00"i
o. co*f"
' no
V 377^ 7
(O 77/
11.771
o.or>
O.fiO
.-),7V
3 7 CeS.^ft
0..7^5
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(9. nm
or nn
-------
ll-Vrnvironmonlal Protection Agency
Ilntional Enforcement Investigations Center-Ilcnvcr
"VI ibral ion Pitol Tube: ID Number hjftS- /
iype-5 Pi tot Tube ID Number: 3'Cz>
CP .9?
mm of ^
^ p
Standard
Pi tot
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Comments
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B leq
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probe sheath attached
nozzle attached
sair.pl ir.g'isokin^tjcal l.y_
Performed By:
j.A~y.
Calibration Date: (0/R/7R
-------
PITOT TUBE CALCULATION SHEET
Tube ID Number
By. /\Q../A>
Calibration Date ^/y/7'9
Checked B^\ /fc M . £Z7~>.'
IP
Std Tube
.r
(Test Section)
CF
A 1 D
a
diff
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-------
NEIC PROCEDURE FOR
CALIBRATION OF DRY GAS METER
AND ORFICE METER
Dry gas meters are used in source testing units to accurately
measure sample volumes drawn during testing. A critical orfice is
also installed to provide a known sampling rate so that isokinetic
sampling can be maintained. These units will be calibrated before
and after each sampling trip.
Calibration is accomplished by making simultaneous total volume
measurements with a calibrated wet test meter and the dry gas meter.
The wet test meter must be previously calibrated from a primary standard.
Calibration is performed follows:
1. Level wet test meter and adjust the water level to the
proper point.
2. Level and zero the manometer on sampling control unit.
3. Leak check unit and air hoses at 15 inch Hg (leakage rate must
be zero). Assemble vacuum line to the wet test meter.
~ *
(Caution: NO NOT Leak Check System by Plugging the Inlet to
the Wet Test Meter, this will cause internal damage to the
meter.)
4. Warm up control unit by operating vacuum pump for 30 minutes
with wet test meter connected in series.
5. Close the course valve and open the fine adjust (by-pass) valve.
6. Turn or vacuum pump, open course adjust valve and turn the fine
adjust valve until manometer reads 0.5" l^O (AH).
-------
-2-
7. Simultaneously record the dry gas meter reading, wet test
meter reading and time. Record temperature of wet test
meter, inlet and outlet temperature of dry gas meter and
atmospheric pressure during the test run.
8. Allow pump to run until the wet test meter indicates
exactly 5 cubic feet of air have passed through the system
(10 cubic feet when a AH of 2, 3 and 4 inches H^O are used)
and record time.
9. Repeat steps 5-9 for AH of 1", 2" 3" and 4" H^O.
10. Calibration record will be kept in a permanent file at NEIC.
Copies will be made for field use.
Calculations
Calculate the accuracy of the dry gas meter (y) as follows:
Vw Pb (td + 460)
y = Vd (Pb + AH (tw + 460)
13.6)
Where:
V e Volume of gas metered, wet test meter, ft.
w
3
Vj = Volume of gas metered, dry gas meter, ft.
P = Atmospheric pressure, inches Hg
b
t, = Dry gas meter temperature, °F (t^ in — out)
2
t = Wet test meter temperature, °F
If y 4 1.00 (+0.02) then gas meter will be taken to Public Service
Company of Colorado gas meter shop for adjustment and/or repair.
Orfice meter coefficient (AH@ = 0.317 AH
P, (td+460)
b
(twt-460) 6
-------
-3-
Where:
= Volume of gas metered, wet test meter, ft
Pjj = Atmospheric pressure
_ o_
= Dry gas meter temperature, F
tw = Wet test meter temperature, °F
9 =» Time elapsed, minutes
-------
Orifice Meter Calibration
Date Id-/7/77
Box Mo.
- /
Barometric pressure, Pb= in. Hg Dry gas meter No.
Ori fi ce
Manometer
setting,
AH
in. HoO
Gas volume
wet test
meter
V
ft3
Gas volume
dry gas
meter
v
ft3
Temperature
Wet Test
Meter
w'
°F
Dry gas meter
Inlet
*di'
'F
Outlet
do'
°F
Average
td'
°F
Time
0,
min
AH@
0.5
J.osT
J9
i(7f
Loo
— £/2u
1.0
xo~7
£L
L°!
U9
M.
Ml
/DC
2.0
10
//
S9
73
7/
IX
l!3L
/.Of
/m
3.0
10
lb,Ocf
1%
~>1
lie
9J1
/..0/
4.0
10
/O.O
£L
iu
&
Average
F-52-
/.o?
/.?o
Calculations
AH
0.5
AH
13.6
0.0368
V,. Pu (t,, + 460)
JidJSiiH XKHML
/??!>'I.
oCjf1 v./y* /-. o$fcp-y fry -/t/Cyv\
AH9
IJFfoK
0*
0.0317AH
Pk (tH+ 460)
(t., + 460)9
lii.
rT
.'24.! cy-f(/Co)l^
£
(&+ ¥&c\'f 7?
1.0
0.0737
_ :lM, \c7 ({& + HU>&S
tclUunt- ol3i\ (S'9 A Hko\
n x AO
f
n O'l n v^o f Y5i/fHi,d)/i 7)
2.0
0.147
,^2y _
fan 19-A ft/ 7^) L< / /-
Wi9 /o
1
3.0
0.219
y jj. ft (7b* lud)
££'SlLJL£22~>
to
L
4.0
0.294 J
/O C^(nA, +- bp
O,o^\~t *
-------
Orifice Meter Calibration
Date G>/d
Box No. ^ f
Barometric pressure, P^= in. Hg Dry gas meter No. -r^v
Ori fi ce
Manometer
setting,
AH
in. Ho0
Gas volume
wet test
meter
V
ft3
Gas volume
dry gas
meter
V
ft3
Temperature
Time
0,
min
y
AH@
Wet Test
Dry gas meter
Meter
Inlet
Outlet
Average
V
°F
°F
tdo'
°F
td'
°F
0.5
5
Coo
Gp.D
7?f
77
76. o
//fx
f'.Cfl
/w
1.0
5
^boo
L3.C>
7?
•7?
1?.^
/o%
l.fo-
2.0
10
JD.o9>d
t>Xo
19
?p-
?o f>
/a .o3
/.VL
/.??
3.0
10
to
o
?*/
?o
¥xo
?.?7
1,01
/.??
4.0
10
/O.GL/O
62. o
?l
ff.kf
¦'tSL
1-9/
Average
lot
'¦rt
Calculations
Y
m
AH
u>|>
•0)=
Vw Pb (t, + 460)
0.0317AH
i
+ 460)0 1
Vrf (Ph+AH ) It,., + 160)
Ph (tri+ 460)L
_ Vw J
0.5
0.0368
13.6 , .
O o3 O <- c> ff p^7.+ QC.^, H f/7
Soc'S(~LL) O -r VLd)
SM.C3 (7^+-M to) L -*> J
1.0
0.0737
^ 67.9.-5'-f
o C'^3i7r- I.o
3.coc>L-lM^3+.c57?>l)(b2--<- H(c&)
'ML3(rt.$iVLc?
*r i
2.0
0.147
1/D/2.V.L.1 (' <-r
o or.yr? / *--o P
/o 0$c/z4*l3+ /ui>(L'Z-tVL.o)
3.0
0.219
Q. CM"? vl 3 o
/o.C>75Y^.L?>4-, %\dh(U^-+ VUb
j?Vt*3C.?5+^c^
to J
4.0
0.294
/oiclu.^o, (&3.
o ocvn*H.o \ 'fLl+fU)?.U1
/c.d^oM (^3+-- w)(UL-tVbD)
^G3f o J
Where: V,., = Volume, wet test meter Cali
Volume Dry gas meter
Temperature, VJet Test Meter
Temperature, Dry Gas Meter
Atmospheric Pressure, Inches Hg
Time, minutes
Remarks: (3 /£ ^ & ° °
4/24/77
v3
TW
Pb
-0
bration by:
-------
Orifice Meter Calibration
Date !<)¦/(<}/l~?
Box No
Barometric pressure, Pb= in. Hg Dry gas meter No.
At
JL
Ori fi ce
Manometer
setting,
AH
in. HoO
Gas volume
-wet test
meter
V,
w:
ft*
Gas volume
dry gas
meter
V
ft3
Temperature
Wet Test
Meter
w'
5F
Dry gas meter
Inlet
ldi'
Outlet
'do'
•F
Average
td'
»F
Time
0,
mi n
AH@
0.5
/T
7V
77
/i.of/.o i
1.0
GO-
~>5"
1?
/>/
/,??£
2.0
10
/DJO
&9~
7?
7?
It
f,oX
2,ooo
3.0
10
fo, lo
Qn-
5M
W
Average
/O.of
Z.cCl
Zoo t
US"
4.0
10
/CKOp'
62^
?.77
box
',a n
/'fty
Calculations Y
AH@
AH
AH Vw Ph + 460)
13.6 Vh (Pk+ah ^ (t„, + 460)
0.0317AH
Ph (tH+ 460)
7.
(t,„ + 460 )G
L vw __
0.5
I ^ , 13.6 ^ N
0.0368 oO)
0 o?>\i*o>'lt b'3L-frV
_ 5" J
1.0
0.0737 | eyr-TJj ^'lX ~?L>* C-rM(cC2~}
n.o)
^•^-UV^C"-*4t=ct_ j5"~ _J
2.0
0.147 |/*x ut.n-(79+*/L,c*')
r),o<) f? * 7,0
! /O./oCz-'f-'i i+-
z.M.rz/??f«Vico)L /o J
3.0
0.219
fiVrX b"2-^ M
4.0
0.294 j/tf^-rUtod)
W0?( to)
c; /c? J
Calibration by
Checked by>
Where: V = Volume, wet test meter
Vd = Volume Dry gas meter
Tw = Temperature, Wet Test Meter
Td = Temperature, Dry Gas Meter . — « ,
Pb = Atmospheric Pressure, Inches Hg ^IdUiu'i. cx-Lm\ A^pXtZw
.0 = Time, minutes , _ . (/ 0 ' 1
A.z*v-ChecK®/S"Mt~OoCFM
Remarks: n _ . O " S^mZj
4? \Ci\o UoxC_^_ ^ I
,1 rO-7 4-MLc) — J r\ ) '
4/24/77
U" ^
e-.iiov
— / £> /
Y- .?L+.oO<46O) '' r
./ oo3n^o,f = iq/
5^ -1 -
-------
Orifice Meter Calibration
Date
,5£-T
6 Box No.
Barometric pressure, in. Hg Dry gas meter Mo.
Ori fi ce
Manometer
setting,
AH
in. HoO
Gas volume
wet test
meter
Vw»
ft3
Gas volume
dry gas
meter
V
Temperature
Wet Test
Meter
ft
d»
3
V
Dry gas meter
Inlet
di'
°F
Outlet
do'
°F
Average
'F
Time
0,
min
AH@
0.5
jToir
(ef-O
62.
7 t.O
lot>
£27
1.0
c>1.^
1L
22l
7 3-p
?¦ 7X
/'Ob
2.d3
2.0
10
/*>• oS
Uf.o
77
1£
7Lo
Ac I
J2.0 c>
3.0
10
/oo3
Gb.O
?o
11
tO ft
fo!
4,0
10
/D Q°
25.:
Avirrage
99/
/,0~L
2-o>
>r
'7
1.0
g^)7x/,c r^y.s>yi-
.?*/
¦SLfi.-fxj1'
2.0
0.147
/£> oSfcxI- U-KiH7V65>*4U>)
C? Q3i"7 X ^-o +
OtJL\(j (g-v^fec^L /o
'3
3.0
0.219 j
/g. d3^ c, I t-\9) ^o)
o g>3o*Q o r^s'^Vbc^) /g/;
o C/VlAU. O V/, ^"54 V(,C
4.0
0.294
/g-KT-t) , U <*?•/-/-Vlg,>
COT(-I4--X9-VLo)
/O
Where:
vS-
TW =
!<*"
Pb =
0 =
Volume, wet test meter
Volume Dry gas meter
Temperature, Wet Test Meter
Temperature, Dry Gas Meter
Atmospheric Pressure, Inches Hg
Time, minutes
J.
Calibration by:
Checked by
Remarks: ^ ^ CbecK is" " O.oo
4/24/77
-------
PROJECT NO.
THERMOCOUPLE CALIBRATION
Calibration Standard Os/g^
Pi tot Tube
I.D. No.
Calibration Temperature
°F
Thermocouple
Reading °F
s-x
^64
2C~G
S-3
JS?
s-y
Pt3
=257
fW
0-^7
?-P-
pt/
P^7
/o-f
W
MP
/0-%
2C>?
£<*(
'0~3
£so
/o-y
2G?
Date
Calibrated By_
Check By
js/pi/TtT
sA
V
--Z3 -7jr
-------
PROJECT NO.
THERMOCOUPLE CALIBRATION
Calibration Standard "ft" */
Pi tot Tube
I.D. No.
Calibration Temperature
°F
Thermocouple
Reading °F
tJoqbie:^ CkIA^%P=. --rhea
{Ci=.nr\D\j£-C\- A /? L ' oK^ Hi,
Y~>OCLOuiC>t£ L-OPr<-
'. o3~
Date
Calibrated By_
JL
Check By
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
Mr. Tim Osag
Field Operations Branch
Chief, Chemistry Branch
R. C. Ross V
DATE
May 18, 1978
Results from Pre-Survey Analyses of SO2 Calibration Gases - Bunker Hill Study
Background
SOg will be monitored by a continuous method during the Bunker Hill Study
which will entail the use of SO2 calibration gases in an air matrix.
40 CFR, No. 194, October 6, 1975, requires that these calibration qases be
analyzed in triplicate two weeks prior to start-up of the continuous moni-
toring to demonstrate stability and accuracy of the gases. The method of
analysis of these gases is directed by Method 6, 40 CFR 60.
Results
The results are presented on Table 1. The first column gives the cylinder
designation. The second column gives the concentration stated by the man-
ufacturer on the tank. The third column tabulates individual triplicate
determinations at NEIC; the fourth column averages these triplicate deter-
minations. The fifth column is the percent difference between the manu-
facturer's value and the average value determined at NEIC. The last column
is the standard deviation among triplicate determinations relative to
average concentration and reported in percent. These determinations were
conducted between May 8 and May 10. A bias of minus 1% in these results
may be expected because the titration determinations on QC standards were
consistently about 1% low. Using the average % deviation from Table 1 as
an estimate of the overall standard deviation, the overall precision of the
measurements can be estimated to be +4% at the 95% confidence level.
Methodology
Figure 1 shows the sampling train used to collect the gases. During sampling,
gas was fed into the manifold at approximately 2 liters per minute. The ex-
cess sample not sampled passed through a soap bubble flow meter so that excess
could be demonstrated at any time during a sampling run. Vacuum on the other
end pulled the sample at a constant flow rate of 1.079 + 3.5% throuqh the
impingers. A rate meter (calibrated rotameter) was placed in line to demon-
strate that the flow was constant. A drying tube with indicating Dryerite
was placed before the rotameter so that the rotameter would be protected
from moisture carried over from the impingers and also so that its calibration
would apply to SO2 in air on a dry gas basis.
-------
- 2 -
Impinger 1 contained 15 ml of 80% isopropanol (I PA). Impingers 2, 3, and
4 contained 15 ml of 3% H2O?. After a run, the contents of impinqers 2
and 3 were combined, brought to 100 ml in a volumetric flask, an aliquot
withdrawn and titrated with standardized BaCl using 2-3 drops of thorin
indicator and enough IPA added to the sample so that it was 80% IPA
before titration.
The titrant, BaC^sWas standardized against .02 H2SO4. The H2SO4 was
standardized potentiometrically against 0.02 N_ NaOH. The NaOH, in turn,
was standardized against 0.02 N potassium acid pthalate (primary standard
grade).
Air flow rates through the train were regulated by means of a calibrated
critical orifice. The vacuum on the end of the system was sufficient to
establish a critical pressure ratio' of 0.25 on the orifice. The flow in
the system was measured by means of a calibrated rotameter with round
stainless steel float. Leak checks were made by attaching a vacuum gauge
to the head of the impinger train, monitoring its stability at 10 inches
mercury (vacuum) for 30 seconds. Flows were timed for 20.0 minutes by
means of'a stop watch.
Calibrations of the rotameter and orifice were done against a soap bubble
flow meter using ambient air at 620 mm and 23°C.
Discussion
Method 6 specifies a dry gas meter with an accuracy of + 2% be used in the
sampling train for gas volume measurements. With a dry gas meter, after
all runs have been completed, the calibration of the meter must be shown
to be within 5% of the initial calibration or all runs are voided.
From my own knowledge of small dry gas meters, they are inaccurate at flow
rates much below several liters per minute. I talked to the area repre-
sentative for Rockwell dry gas meters and he said that for Model T-110,
which we have, the lowest flow rate where accuracy of + 2% could be ex-
pected is 10 scfm per hour—this corresponds to 4.67 liters per minute.
It was for this reason that a rotameter and orifice were used to measure
flow rate--from which total sampling volume was calculated. A meter does
exist with one full dial turn equal to 0.1 scfm but it is basically the
same meter inside as the T-110. The discrepancy between the stated require-
ments in Method 6 for the dry gas meter vs what is possible at a flow rate
of 1 liter/minute is what led to the choice of rotameter and critical orifice
set-up for flow measurements.
During the course of sampling it was noted that between runs the height of
the rotameter ball changed slightly. This seemed strange because the
critical orifice should have maintained a constant flow rate. Late on the
^Upstream pressure divided by downstream pressure
-------
- 3 -
second day of analytical runs by hooking up a mercury manometer in-line
and just before the rotameter it could be observed that by varying the
volume of excess calibration gas fed into the manifold over the ranqe
used in the analytical determinations, pressure changes at the rotameter
as high as 34 mm could be produced.
The observed readings on the rotameter ranged from 81.5 to 84 mm. An
average pressure drop of 20 mm was observed over the later determinations.
Therefore, corresponding to 82.75 mm on the rotameter and 597 mm pressure,
the average flow rate of 1079 ml/min at 597 mm Hg was used in all of the
calculations. This, after calculation, would account in an overall vari-
ability in the measurements of about +_ 3.5%.
Quality Control
All standardizations were performed at least in duplicate. The BaCl2 in
80% IPA titrant was restandardized daily with no change. Five audit sam-
ples from EPA, RTP were analyzed during the course of the work. These
concentrations were originally unknown to myself; results were as follows:
Sample Number Result, mg/dscm True, mg/dscm % Deviation
Sample number 5299 required only 1.7 ml of titrant and should not be included
in an assessment of accuracy since the limits of error on this titrant volume
are an order of magnitude larger than on the other determinations including
the other gas cylinder determinations reported here. On this basis, I had
a consistent bias of approximately minus 1%.
Replicate titrations were performed during the sample analyses with results
agreeing to better than 1%. Blanks of 3% H2O2 were titrated with BaCl2 and
results subtracted from sample values (blanks were almost negligible). IPA
was checked for peroxide by the procedure given in Method 6 and found to be
quite acceptable. 3% H2O2 was made fresh each day of analysis.
To examine collection efficiency, during three of the runs involving the
higher concentration calibration gases, the fourth impinger (Figure 1),
filled with 3% H2O2, was analyzed separately after the test. When the
contents were analyzed, no SO2 (as S04=) was detected in the fourth im-
pinger during any of these three determinations.
Leak checks were performed both before and after each sample run.
5299
4348
2141
7399
8253
133
5080
4320
1392
2570
137
5148
4347
1411
2593
-2.9
-1.3
-0.6
-1.3
-0.9
Richard C. Ross
-------
mple No
1 Scott
1 Scott
1 Scott
2 Scott
2 Scott
2 Scott
1 Scott
1 Scott
1 Scott
3 Scott
3 Scott
3 Scott
3 Scott
3 Scott
3 Scott
2 Linde
2 Linde
2 Linde
1 Linde
1 Linde
1 Linde
3 Linde
3 Linde
3 Linde
2 Linde
2 Linde
2 Linde
Table 1
Stated Cone. SO2 Found Ave Found Percent Change Relative
ppm ppm ppm from Stated Cone. SD*-%
2490 + 2% 2333
2353 2365 - 5 1.4
2410
2607 + 2% 2396
2481 2464 - 5.5 2.0
2516
997 + U 919
947 927 - 7 1.5
916
2534 + 2% 2602
2326 2485 - 1.9 4.7
2528
4500 + 1% 4560
4496 4510 + 0.2 0.8
4473
957 1095
1142 1130 +18 2.3
1155
971 1118
1118 1100 +13.3 2.2
1065
950 955
986 946 - 0.4 3.8
899
4329 4599
4625 4656 + 7.6 1.4
4745
-------
Sample No.
C-l Linde
C-l Linde
C-l Linde
C-3 Linde
C-3 Linde
C-3 Linde
Stated Cone.
ppm
4408
4395
SO2 Found
PPm
4578
4618
4555
4601
4734
4602
Ave Found
PP"1
4580
4640
Percent Change
from Stated Cone.
+ 4
Table 1
-conti nued
Relati ve
SD*-%
0.6
+ 5.7
1.3
*SD = Standard Deviation
Ave = 2.0
-------
VENT
TO HOOD
VACUUM &AUGE.
checks)
MIDGET BUBBLER
MIDGET IMPINGERS
DRYING TUBE
SOAP BUBBLE FLOW
METER
FROM GAS CYLINDER
RATE METER
Fio 1 - SO2 sampling train.
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
o Tim Osag DATE June 27, 1978
Field Operations Branch
*°m R. C. Ross
ubject Post-Survey Analysis of SC^ Calibration Gases - Bunker Hill
In accordance with the Bunker Hill study plan, the SO2 calibration
gases were reanalyzed after return to Denver. The method of analysis
was directed by Method 6, 40 CFR 60. Table 1, attached, lists the gases
analyzed, the suppliers stated concentration, individual and average
concentrations as determined here, and finally the percent change of the
concentrations found versus the supplies stated concentrations. This
data was previously transmitted on June 20th; there are no changes shown
in the results. Six replicate determinations of a gas standardized
against NBS SRMS demonstrated a precision of analysis of ±2% over a four
day period.
Methodology
Figure 1 illustrates the sampling train used to collect the samples.
A number 22 gauge needle was used to control the flowrate. The mercury
manometer just before the critical orifice served to indicate any pres-
sure changes. Rotameter 2 was used to indicate a constant flow through-
out the sample runs. The drying tube was inserted to protect the rota-
meter and critical orifice from condensed water.
The fritted bubbler normally used in Method 6 in the first impinger
was exchanged for an open type of bubble because of uncontrollable and
excessive frothing at this impinger. Rotameter number 1 was placed in
the system to show an excess of SO2 at the sampling manifold.
Before and after each sample run, a soap bubble flow meter (SBFM)
was connected to the head of the impingers to measure the flowrate through
the system. Readings at rotameter 2 and at the Hg manometer were re-
corded before, during and after each run. Barometric pressure and room
temperature were recorded for each run. Except for the RTP audit gas
(which was made up in nitrogen) the system was calibrated against ambi-
ent air entering the system through the SBFM. For those runs involving
the audit gas, the system was calibrated with nitrogen. Leak checks
were performed for each sample run. The critical pressure ratio* at the
limiting orifice was checked and found to be <0.4.
*Downstream pressure divided by the upstream pressure.
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2 -
Impinger 1 contained 15 ml 80% isopropanol (IPA) - water. Impingers
2, 3, and 4 contained 15 ml 3% H2O2 solution freshly prepared each day.
The combined solutions from impingers 2 and 3 were titrated against stand-
ardized BaCl after each run. Typically 10 minute runs with 15 minutes
purge times were used.
Discussion
The flowrates used were typically 1.05 liter per minute which for a
10 minute sample run would yield a 10 liter sample. Pressure at the mer-
cury manometer stayed at 25±/mm Hg below ambient pressure.
The results in table 1 reflect corrections made for pressure, temp-
erature, water vapor and the amount of SO2 removed from the volumetric
flowrate before passing through the metering critical orifice.
Reference solutions obtained from EPA, RTP indicate that the titer
value used to obtain the results in table 1 is about 0.5% low. This is
substantiated by the fact that although 0.01 equivalents of BaC12 were
added per liter of titratirig solution the titer value used, determined
by potentiometric standardization, was .00994 equivalents per liter.
Values obtained from post-survey determinations in some cases are
slightly different from those obtained on the pre-survey determinations.
Also the agreement between the manufacturers values and the post-survey
value on the average is slightly better than before. The difference
between the pre- and post values obtained is attributable to better con-
trol of the numerous variable effecting the measurements during the post-
survey determinations.
Quality Control
Reference solutions obtained from RTP demonstrate the titration
procedure to be accurate to better than 1%. The results of t.he audit
gas analyzed six times during these determinations had a standard devi-
ation of less than 1%; using two standard deviations as a criteria the
precision was better that 2%. The agreement between the average value
and the stated value shows that the analytical results for this cylinder
are consistent with the SRM's against which the audit gas was calibrated -
thus the average result appears to be highly accurate and indicative of
the other results in table 1.
R. C. Ross
cc: Meiggs
Young
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TABLE I
NEIC
Gas
Stated Cone.
Measured Cone.
Ave.
% Deviation
C.yl inder
ppm
ppm
Cone
from stated
QC-1
997
974
980
-1.2
1005
975
QC-3
4500
4470
4500
+0.1
4539
4507
A-l
1063
971
1061
1060
+9.5
1062
1066
A-2
957
1048
1040
i 9.0
1041
1039
A-3
950
950
960
+1
958
970
B-l
2490
2466
2440
1
ro
ro
2442
2396
2441
B-2
2607
2544
2540
-2.4
2582
2505
B-3
2534
2430
2450
-3.4
2442
2469
C-l
4408
4614
4620
4-4.8
4639
4610
C-2
4329
4539
4530
+4.6
4543
4610
C-3
4395
4609
4590
+4.5
4590
4579
RTP Audit Gas
+0.1
III 6/12
2268
2306
2370
6/12
2269
s = 24 ppm
6/13
2288
2s - 48 ppm (2%)
6/14
2251
6/14
2262
6/15
2242
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to
HC hakiometer
?' ROTAMETER 1
MIDGET IMPIiMGERS -
DRYING TUBE
ROTOI1ETER
SOAP BUEGLE FLOW
Merer*
LlMlTIMG ORIFICE
F.g 1 "
SO2 sampling train.
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