ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
EPA-330/2-78-003
The Environmental Impact of Emissions
from the
National Zinc Company
Bartlesville, Oklahoma
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
DENVER. COLORADO
MARCH 1978
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Environmental Protection Agency
Office of Enforcement
EPA-330/2-78-003
THE ENVIRONMENTAL IMPACT OF EMISSIONS
FROM THE
NATIONAL ZINC COMPANY
Bartlesville, Oklahoma
[July - September 1977]
March 1978
National Enforcement Investigations Center
Denver, Colorado
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CONTENTS
I INTRODUCTION 1
II SUMMARY AND CONCLUSIONS 3
III BACKGROUND 7
PLANT HISTORY 7
PROCESS DESCRIPTION 7
SURVEY AREA DESCRIPTION 8
IV SURVEY METHODS 9
MONITORING NETWORK DESIGN 9
MONITORING PROCEDURES 12
IN-PLANT EVALUATION 19
V SURVEY RESULTS 21
SULFUR DIOXIDE 21
PARTICULATES 21
REMOTE SENSING 35
BOTANICAL ASSAY 35
REFERENCES 39
APPENDICES
A QUALITY ASSURANCE AUDIT REPORT
B TSP FILTER CARD SAMPLE
C CHAIN-OF-CUSTODY PROCEDURES
D ANALYTICAL PROCEDURES
E METEOROLOGICAL DATA
F RAW SOy DATA
G RAW TSP DATA
H RAW SO, DATA
I RAW METALS DATA
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TABLES
1 TSP and SCL Standards 4
2 Sampling Station Descriptions 10
3 Instrumentation 11
4 Summary of S02 Data 22
5 Summary of TSP Data 29
6 Summary of SO. Data 30
7 Ambient Air Metals Analyses 32
8 Soil Metals Analyses 34
9 Soil pH and Average Metal
Concentrations 38
FIGURES
1 Sampling Station Location 2
2 SO £ Permeation Tube System 14
3 Greenhouse and Sparging Units 17
4 Daily TSP Concentrations - Station 1. . 24
5 Daily TSP Concentrations - Station 2. . 25
6 Daily TSP Concentrations - Station 3. . 26
7 Daily TSP Concentrations - Station 4. . 27
8 Daily TSP Concentrations - Station 5. . 28
9 Aerial Infrared Photography Coverage. . 36
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I. INTRODUCTION
During July 2-3, 1977, the National Zinc Company in Bartles-
ville, Oklahoma, experienced a malfunction during the start up of its
sulfuric acid plant which caused the Company to cease operations
temporarily. Residents north and northeast of the plant had fre-
quently complained of these plant emissions. However, during the
July 2-3 episode, these residents alleged that plant emissions caused
damage to vegetation, death of cattle, and adverse health effects to
people in the area. This incident resulted in a complaint to the
Regional Administrator, Environmental Protection Agency (EPA), Region
VI, and on July 22, Region VI requested that the National Enforcement
Investigations Center (NEIC) set up an ambient air monitoring network
in the vicinity of the plant as rapidly as possible to document peak
3-hour and 24-hour sulfur dioxide (SOp) concentrations prior and
subsequent to plant start up. NEIC began operating sulfur dioxide
(S02) monitoring equipment near the northeast corner of the plant
boundary on July 28, 1977. On August 2, 1977, the Company restarted
the plant. By August 16, 1977, five stations [Figure 1] were in
operation monitoring S02 and total suspended particulates (TSP). By
September 2, 1977, samplers for ambient air metals were also opera-
ting at Stations 1, 3, 4 and 5. These sites were used to document
peak 24-hour TSP concentrations and 24-hour sulfate (SO^) concen-
trations, and to determine concentrations of selected metals in both
soil and ambient air associated with the National Zinc Company op-
erations. In addition, the NEIC began to assess the impact on sur-
rounding vegetation of past and present emissions from the plant and
to evaluate the plant operations to determine if improvements in
operating procedures and/or air pollution control equipment were
required.
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1,000 meters
9)- Sampling station
igure 1. Sampling Station Location
National Zinc Co., Bartlesville, Oklahoma
July 28 - September 26, 1977
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II. SUMMARY AND CONCLUSIONS
During the period August 2 to September 26, 1977, the National
Enforcement Investigations Center (NEIC) conducted an investigation
of the sulfur dioxide (S02), total suspended particulate (TSP),
sulfate (SO^), and metals emissions from the National Zinc Company
plant in Bartlesville, Oklahoma, and the impact of these emissions on
the ambient air quality, soils, and vegetation in the area. Air
quality, meteorological, botanical, and soils data were collected
from a six-station network located around the plant.
Data from these stations were evaluated to characterize ambient
air quality in the area and to compare with National Ambient Air
Quality Standards (NAAQS) [Table 1]. The primary criteria used in
analyzing TSP data were 24-hour primary and secondary excursions;
24-hour primary and 3-hour secondary excursions were used for S0?
data. A primary excursion is defined as any 24-hour concentration
which exceeded the 24-hour primary standard for either TSP or SO^. A
secondary excursion is defined as either a 24-hour TSP concentration
which exceeded the 24-hour secondary standard or a 3-hour SO, concen-
tration which exceeded the 3-hour secondary standard.
c.
Where possible, ambient metals data were compared with values
measured by the National Air Surveillance Network (NASN) as reported
in National Trends HI Trace Metals ±n Ambient Air, 1965-1974.l
Metals concentrations in soils were compared with the mean values
found in the earth's crust as reported in Origin and Distribution of
the Elements.2 Sulfates data were compared with sulfates health
effects research data as reported in Statement of Sulfates Research
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Table 1
NATIONAL PRIME? AND SECONDARY AMBIENT AIR QUALITY STANDARDS FOR TOTAL
SUSPENDED PARTICULATES (TSPJ AND SULFUR DIOXIDE (SOJ
&
Pollutant
Type of Averaging
Frequency Parameter
Concentration
TSP
so2
Standard
Primary
Secondary
Primary
Secondary
Time
24 hr
24 hr
24 hr
1 yr
3 hr
Annual
Annual
Annual
Annual
Maximum
Geometric Mean
Maximum
Maximum
Arithmetic Mean
Annual
Maximum
ug/m3
260
75
150
355
80
1,300
ppm
0
0.03
0.5
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Approach.3 Potted plants exposed to ambient S02 levels near the
National Zinc Company plant were visually compared to similar potted
plants grown at a reference station approximately four miles south of
the plant. A similar comparison of trees in the area was made using
false color infrared aerial photographs.
In addition, an in-plant investigation of the process and air
pollution control operations was conducted by NEIC during the period
July 30 to August 2, 1977.
The results of the NEIC survey are as follows:
1. The July 2-3 S02 incident was due to operator error in that
one of the ore roasters was not maintained at a suffi-
ciently high temperature. Because of this, the offgas from
the roasters was not hot enough to allow for effective SCL
removal when fed through the sulfuric acid plant.
2. The plant did not cause excursions of the 24-hour primary
or 3-hour secondary S02 standard during the survey period.
3. The plant did not cause violations of the primary 24-hour
TSP standard during the survey period. Although the re-
sults show there were five excursions of the secondary
o
24-hour standard of 150 ug/m at Station 5, meteorological
data indicate the plant likely could have contributed
significantly to only one of these excursions (September 8,
1977).
4. Sulfate levels were found to exceed levels reported to be
statistically associated with adverse health effects. How-
ever, as there are currently no national ambient air qual-
ity standards for sulfates, these levels cannot be con-
sidered as excursions or violations.
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5. Since soil analysis showed the soil immediately downwind of
the plant to have substantially higher metals concentra-
tions than soil from a reference station several miles
away, it is concluded that these high metals concentrations
are probably a result of plant emissions. Of particular
concern are the high levels of lead and cadmium.
6. Plants grown in soil taken from near the National Zinc
Company plant were chlorotic, containing only 28% as much
chlorophyll as similar plants grown in soil from the ref-
erence station. Since soil analysis showed soil near the
plant had a lower pH as well as substantially higher metals
concentrations than the reference station soil, it is
concluded that reduced plant vigor may be the long-term
result of National Zinc Company emissions influencing soil
characteristics.
7. The botanical assay results are supported by false color
infrared aerial photographs taken of the area surrounding
the plant. These photographs indicate an increase in the
chlorophyll stress of vegetation in the area immediately
north of the plant. This is the area that, climatologi-
cally, is most often downwind from the plant.
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III. BACKGROUND
PLANT HISTORY
National Zinc Company, a subsidiary of Engelhard Industries, New
York, N. Y., produces zinc at their Bartlesville plant. The plant
first began operations in 1907 using horizontal retort furnace smel-
ters. From then until 1969, there were no emission controls on the
plant. In that year, S02 emissions were reduced with the installa-
tion of a Monsanto design sulfuric acid plant which recovers SO,, from
plant exhaust gases and uses it in the production of technical grade
sulfuric acid (H2$04) and oleum (H2S04 + S03). In 1973, the acid
plant stack height was increased by 25% to aid in the dispersion of
the remaining S02 in the exhaust gases. In 1976, the horizontal
retort furnaces were replaced by an electrolytic smelter; according
to the Oklahoma State Health Department, this process modification
reduced TSP emissions by 99.7%.
PROCESS DESCRIPTION
Zinc sulfide (ZnS) ore is first roasted, resulting in dry zinc
ore soli
containing 7%
3 3
oxide ore solids and about 453 m (16,000 ft )/min of exhaust gas
During normal operations, the zinc oxide (calcine) is fed into
an electrolytic process to produce zinc metal. The sulfur dioxide-
laden gas from the roasting process is routed to a sulfuric acid
plant and both technical grade sulfuric acid and oleum are produced.
The sulfuric acid plant is a standard contact sulfuric acid process
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8
that includes a four-stage converter and a single-stage absorber with
a Brink mist eliminator. The unit receives all of the exhaust gas
containing S02 and produces sulfuric acid and oleum. The offgas from
the absorber is the only S02 emission point from the National Zinc
roasters and sulfuric acid plant. Containing 1,000 to 1,600 ppm S02
during normal operation, these gases pass through the Brink high-
efficiency mist eliminator for acid mist removal prior to being
discharged into the atmosphere.
SURVEY AREA DESCRIPTION
The National Zinc plant is located on the western edge of
Bartlesville in a broad and featureless valley of the Caney River in
northeastern Oklahoma. A 61 m (200 ft) high mound rises about 1.6 km
(1 mi) to the north-northwest of the plant and there are some 61 m
(200 ft) high ridges rising about 3.2 km (2 mi) to the south and
south-southwest, just south of Sand Creek. These topographical
features do not have a significant effect on the meteorological
conditions in the area.
The climate of the Bartlesville, Oklahoma, area is characterized
by high mean surface wind speeds and good ventilation throughout the
year. Air stagnation conditions, which can lead to high air pollu-
tion concentration levels, are infrequent.4 The meteorological
condition which would be most likely to lead to high air pollution
levels in the area is wind direction persistence. A review of cli-
matological data for the area indicated that, for the survey months
of August and September, the predominant wind direction is southerly.
Stability conditions show a wide diurnal variation, particularly in
August, but are predominantly neutral. Based on this information and
some Oklahoma State Health Department (DSHD) dispersion modeling
results, the primary air quality monitoring stations were located
north of and within 1.6 km (1 mi) of the plant.
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IV. SURVEY METHODS
MONITORING NETWORK DESIGN
To measure ambient air quality and assess vegetation damage, a
network of five ambient air quality monitoring stations was operated
near the plant. A sixth background station for the botanical assay
was located approximately four miles south of the National Zinc
plant. Design of the network was based on the following:
1. Atmospheric dispersion modeling work conducted by the
Oklahoma State Health Department (OSHD) which indicated
that maximum ground level S02 concentrations from the 33 m
(100 ft) high sulfuric acid plant stack would be encoun-
tered about 400 to 500 m (1,300 to 1,600 ft) downwind from
the stack.
2. Climatological information obtained from OSHD and EPA
Region VI which indicated that, during the late summer and
early fall, the most frequent wind direction is southerly.
3. The alleged damage resulting from the July 2 to 3, 1977,
incident, which was within a triangular area (apex at the
plant) extending north for about 2 km (1.25 mi).
Based on the above information, a monitoring network of six
stations was established as described in Tables 2 and 3 and illus-
trated in Figure 1.
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10
Table 2
DESCRIPTION OF AIR QUALITY MONITORING STATIONS
NATIONAL ZINC COMPANY
BARTLESVILLE, OKLAHOMA
July 28 - September 263 1977
Station No. Location Description
1 The southeast corner of the Albert Jackson property
(10th Street and Rogers Avenue) near the northeast
corner of the plant property and about 400 meters
northeast of the sulfuric acid plant stack.
2 About 100 meters north of 14th Street and 200 meters
west of Virginia Avenue, across the railroad tracks
from the southeast corner of the plant property and
about 400 meters southeast of the sulfuric acid plant,
3 About 150 meters west southwest of the intersection
of Oklahoma Highways 23A and 123, about 1,000 meters
southwest of the sulfuric acid plant stack.
4 At the Osage Rural Water District pumping stations
north of Highway 60, just across from Phillips
Research Center building RB-1, about 2,000 meters
northwest of the sulfuric acid plant stack.
5 At the northeast corner of the intersection of Adams
Street and Adeline Blvd., about 750 meters north
northwest of the sulfuric acid plant stack.
6 Four miles south of the plant just off Rt. 123. This
site was a background station for bioassay only.
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Table 3
MONITORING INSTRUMENTATION
NATIONAL ZINC CO. DARTLESVILLE, OKLAHOMA
August 5 - September 26t 1977
Sta
No.
1
2
3
4
5
6
so2
Monitor
Lear Siegler
SM 1000
Bendix
Model 8300
Lear Siegler
SM 1 000
Bendix
Model 8300
Bendix
Type of
Recorder
Esterline-
Angus
Weather-
measure
Weather-
measure
Weather-
measure
Weather-
measure
High Volume
Sampler
General Metal
Works, Model
GMHS-2310
Accu-Vol with
Timer, Program-
mer and Trans-
ducer
ACCu-Vol
ACCU-Vol
ACCU-Vol
ACCU-Vol
Membrane Hourly Meteorology Rain Green- Sparg-
Sampler Averager Data Gage House ing
System unit
Research Appli-
ance Company
(RAC) Total
Particulate
Membrane
Sampler (#2349)
RAC
RAC
RAC
Monitor
Labs
Monitor
Labs
Monitor
Labs
Monitor
Labs
Monitor
Labs
Climet Weather- NEIC NEIC
Instruments measure
NEIC NEIC
NEIC NEIC
NEIC NEIC
NEIC NEIC
NEIC
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12
MONITORING PROCEDURES
Ambient SOp Monitoring
Three types of sulfur dioxide ambient air monitors were used.
At Stations 1 and 3, the Lear Siegler SMI000 Air Monitoring System
was used. This system is a tuned, second derivative spectrometer
which measures concentrations of SOp in complex ambient air mixtures.
The instrument directly measures the narrow band absorption of ultra-
violet radiation which is characteristic of and specific to the
ambient air S0? molecule. Measurements are performed in real time
without sample conditioning, secondary reactions, or sample destruc-
tion.
At Stations 2 and 4, the Bendix Model 8300TS Monitor was used
and, at Station 5, the Bendix Model 8301 SOp Monitor was used. Both
models are flame photometric detector systems with the Model 8300TS
also incorporating a hydrogen sulfide (HpS) scrubber.
The output signals of the SOp monitors were electronically time
averaged, so that hourly averages were transmitted to the recorder
charts.
A quality control program consisted of 1) daily visits (weather
permitting) to the monitoring stations to service the SO* monitors,
and 2) periodic calibrations of the monitors. On the Lear Siegler
SMI000 SOp monitors (Stations 1 and 5), a check of the span and zero
on the recorder was performed automatically every eight hours. On
the Bendix instruments, the zero check was done weekly and the instru-
ment was spanned during the quality control checks. The detector was
checked manually everyday by a calibrated DC voltage source. For all
SOp monitors, calibration curves were prepared at the beginning and
end of the survey using a modified Bendix calibration system
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13
[Figure 2] with National Bureau of Standards permeation tubes as the
SOp source. A quality assurance audit [Appendix A] was also per-
formed on September 1 to 2, 1977.
Particulate Sampling and Analysis
Ambient Participate Monitoring - A set of three General Metals
Works (GMW) high-volume (HiVol) particulate samplers was located at
each of Stations 1 through 5. A set of two Research Appliance Com-
pany (RAC) membrane samplers was located at each of Stations 1, 3, 4
and 5. The HiVols were used for TSP and sulfates sampling and the
membrane samplers were used for metals sampling. Soil samples were
also taken at Stations 1, 3, 5 and 6 for metals analyses.
Both the GMW and RAC samplers were run sequentially for 24-hour
periods beginning and ending at midnight. All pertinent data regard-
ing the HiVol sample filters was recorded on a card [Appendix B].
Each 20 x 25 cm (8 x 10 in) glass fiber filter was folded and placed
in the appropriate card which was, in turn, placed in an envelope and
sealed. RAC membrane filter data were entered into a bound log book
and the filters were placed in clean Petri dishes and sealed in
aluminum foil. Filters were maintained under NEK chain-of-custody
procedures [Appendix C] and returned to NEIC.
Quality control was maintained by measuring the flow rate of
each sampler at the beginning and end of each operating period. At
least once weekly, calibration curves were checked for accuracy using
standard calibrated orifice plates. Additionally, new calibration
curves were developed in any case where changes were made in the
sampling devices, such as head changes, motor replacements, etc. A
quality assurance audit was also performed on September 1-2, 1977
[Appendix A].
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Air
Out
Dri'cn te
Air
In
Membrane
Pump
Instrument
Sample Tube
1
Mixing Chambers
Flow
Meter
1-101/imn
Drierite Molecular
| /Sieve
I » i I
Teflon
Filter
Permeation
- Tube
Chamber
Figure 2. Modified Bendix S0« Calibration System
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15
Laboratory Particulate Analyses - All HiVol and membrane filters
were initially weighed in the NEIC laboratory to determine total
suspended participate concentrations [Appendix D]. Ten percent of
the filters were randomly selected for reweighing as a quality con-
trol check. Thirty-one HiVol filters and nineteen membrane filters,
mainly those associated with high TSP levels, were selected for
further analyses for sulfates and metals, respectively.
Sulfate analyses were performed on the 31 glass fiber HiVol fil-
ters. Filters were selected so comparisons could be made between
values measured at sampling stations located both upwind and downwind
of the National Zinc Company plant on any given day. Quality control
was maintained through replicate analyses of paired samples [Appendix D].
Metals analyses were performed on the 19 membrane filters. Five
sampling dates were chosen and samples from Stations 1, 3, 4 and 5
were analyzed so as to include both upwind and downwind sampling
locations. Metals analyses were also performed on a total of eight
soil samples from four of the sampling stations, including one from
the bioassay background station (Station 6). The accuracies of the
analyses were verified by the analyses of standard spikes [Appendix D].
Remote Sensing
On September 19, 1977, aerial photographs were taken of the
National Zinc Company plant and the surrounding area. The purpose of
this photo survey was to detect and document the presence of trees
displaying chlorophyllic stress. The trees in the area had purport-
edly been fumigated by S02 emissions from the National Zinc Company
facility a few weeks prior to the photo survey.
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16
The survey was conducted using an aerial camera with Eastman
Kodak Anochrome Infrared Film (2443) which was exposed through a
Wratten 12 (yellow) filter. This film has an emulsion layer that is
sensitive to the near infrared region of the optical spectrum where
chlorophyll is highly reflective. When foliage is stressed by dis-
ease, drought, air pollutants, etc., the chlorophyll levels within
the foliage are affected. Any change in chlorophyll levels can be
qualitatively detected with the infrared film even though the change
may not be detectable with the unaided eye or regular photographic
emulsions.
The photographic overflight was carried out at an altitude of
762 m (2,500 ft) above mean ground level resulting in an image scale
of 1:5000 on the infrared film. The flight lines were oriented in a
north/south direction.
The exposed film was developed by Texas Instruments Company,
Dallas, Texas, and photointerpreted by the NEIC's Technical Services
Branch.
Botanical Assay
Two bioassays were performed to determine the effects of emis-
sions from the National Zinc Company plant on selected vegetation.
An in-situ bioassay was conducted at all six monitoring stations
from August 13 to September 24, 1977, using small portable green-
houses [Figure 3]. The prism-shaped plywood structures measured
approximately 1.2x1.2x1.2m (4x4x4 ft). A cheesecloth-
shaped, plexiglas window allowed light for the plants.
Two types of greenhouses were placed at each station, exposure
greenhouses and closed control greenhouses. Except during heavy
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17
Plexiglas Window
Intake Fan
Removable Window Panel
Cheesecloth Shade
Exhaust Vents
Greenhouse
NT\
* \' \
To Closed Greenhouse
,Na HC03 Solution
55 Gallon Drum
Figure 3.
Vacuum Cleaner Pump
Sparging Unit
Greenhouse and Sparging Units for Plant Bioassays
(Binkley, 1977)
National Zinc Company
July 28 - September 26, 1977
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18
rains, the exposure greenhouses were left open at the top front by
sliding the window down halfway. Small intake fans drew ambient air
into the greenhouses through these openings and small screened vents
allowed air to escape. The closed control greenhouses were con-
structed similarly, but without the intake fans. To control tem-
perature and remove SQ~ the window was always closed and the air was
pumped through a chilled sodium bicarbonate (NaHCOO water bath into
the closed greenhouses.
Each greenhouse contained two Schefflera sp. and five Chrysan-
themum sp. At Stations 1, 3 and 5, a single potted Schefflera sp.
was also kept outside the greenhouses. The plants and potting soil
were obtained from a local greenhouse. All plants were checked
daily.
In addition to the in-situ bioassay, a laboratory bioassay was
conducted at NEIC using soil samples collected from near the National
Zinc plant (Station 1) and from the reference location (Station 6).
The soil samples were tested for pH after the soil was mixed with
distilled water on an equal-weight basis. Then the soil samples were
used to grow Pi lea sp. plants in controlled environment incubators
from September 7 to October 21, 1977. The plants were randomly
divided into two groups of 24 each and planted in the test soils.
Test conditions were 30°C (86°F) ambient temperature and 18 hr/day of
incandescent and fluorescent light. The plants were examined periodi-
cally and watered as necessary. At the end of the study period,
selected test plants were pulverized with a manual tissue grinder and
the chlorophyll was extracted in 90% acetone. The amount of chloro-
phyll in each plant was then measured using fluorometric techniques.
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19
Meteorology
At Station 1, a 10-m (30-ft) meteorological tower was erected to
collect data on wind speed, wind direction, temperature, dewpoint,
and barometric pressure. The data were collected by a Climet meteor-
ological data system in which the conditioned signals from the instru-
mentation were processed by an Esterline-Angus PD2064 minicomputer
and recorded on cassette magnetic tapes. Data from these tapes were
then processed by H. E. Cramer Co., Salt Lake City, Utah, into a
format satisfactory for use in data analysis and reporting [Appendix
E]. In addition to the cassette tapes, data were recorded in digital
form on printed paper tapes and analog form on Leeds and Northrup
strip charts. Rainfall was also recorded (on chart paper only) using
a Weather Measure tipping bucket rain gage.
IN-PLANT EVALUATION
NEIC personnel met with officials of National Zinc Company from
July 30 to August 3, 1977 to conduct an in-plant evaluation. During
this visit, the circumstances surrounding the July 2 to 3, 1977,
incident were reviewed and start up of the plant was observed.
The primary source of SCL at National Zinc is the offgas from
the ore roasting process. Control of SO-2 emissions is affected by
passing this gas through a standard contact sulfuric acid process
where much of the S02 is used to produce HpSCL. A necessary part of
this process is the conversion of SOp to SO-. The converter beds in
which this reaction takes place must be maintained in a specific
range of elevated temperatures. During normal operations, the offgas
temperature from the ore roaster is sufficient to maintain converter
temperatures within this range. During process start up, however,
preheaters must be used to maintain converter temperatures until the
roaster bed temperatures are high enough. Since the roaster bed
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20
temperatures often fluctuate during process startup, it is necessary
to monitor those temperatures and to turn the converter bed preheater
back on whenever necessary. The July 2 to 3, 1977 incident was
caused by a failure to operate the preheaters properly.
After observing and evaluating the plant start up, NEIC observa-
tions and recommendations were forwarded to Region VI in an August
19, 1977 report.
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V. SURVEY RESULTS
SULFUR DIOXIDE
The principal criteria for sulfur dioxide data analyses were the
primary 24-hour average and the secondary 3-hour average standards
established by the national ambient air quality standards as follows:
Primary - 24-hour SO, concentrations shall not
3
exceed 365 ug/m more than once annually
Secondary - 3-hour SO- concentrations shall not
3
exceed 1,300 ug/m more than once annually
Appendix F contains the raw S0£ data. Results [Table 4] show no
excursions of the 24-hour primary standard. One excursion of the
3-hour standard was recorded on September 11, 1977 at Station 3, with
an average of 2,325 ug/m . However, the value was recorded during a
period of extremely heavy rainfall, and when the wind direction was
not from the plant. It is believed that this value was caused by
moisture from the heavy rain interfering with the instrumentation.
PARTICULATES
Ambient TSP
The principal criteria for TSP data analyses were the primary
and secondary 24-hour average standards established by the national
ambient air quality standards as follows:
Primary - 24-hour TSP concentrations shall not exceed
3
260 ug/m more than once annually
Secondary - 24-hour TSP concentrations shall not exceed
3
150 ug/m more than once annually
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22
Table 4
SUMMARY OF SO SAMPLING RESULTS
NATIONAL ZINC COMPANY
BARTLESVILLEj OKLAHOMA
July 28 - September 26, 1977
Station
1
2
3
4
5
Total hrs
Sampled
1,179
1,182
1,132
1,041
1,050
No. hrs S02
Detected
78
2
2
10
90
Highest 1-hr
Value
yg/m
832
520
2,288
390
650
Number of
24- hour
Standards
Excursions
0
0
0
0
0
Number of
3-hour
Standards
Excursions
0
0
1
0
0
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23
The TSP data are presented in Figures 4 through 8. The indivi-
dual 24-hour values are plotted against the dates included in the
survey, beginning with August 2, 1977 and ending September 26, 1977.
Not all TSP sampling stations were on line as of August 2, so the
length of the records for each station varies from 48 to 56 days.
Lines indicating the primary and secondary 24-hour standards are also
included. Table 5 is a statistical summary of the TSP data.
Appendix G lists the raw TSP data.
From Table 5 it can be seen that no excursions of the primary
24-hour TSP standards (260 ug/m ) were recorded during the two months
of this survey. Six excursions above the secondary standard (150
3
|j/m ) were recorded, one at Station 1 and five at Station 5.
Sulfates
Thirty-one of the glass fiber filters from the TSP sampling were
selected for sulfate (S0~) analysis. Filters from downwind sampling
sites were analyzed along with the corresponding filters from upwind
sites. Most of the downwind filters selected showed TSP levels ex-
3
ceeding 100 ug/m . The results of the analysis are presented in
Appendix H. A statistical summary of those results appears in
Table 6.
The identification of Stations 1, 4 and 5 (north of the plant)
as "downwind" and Stations 2 and 3 (south of the plant) as "upwind"
[Table 6] was based on the fact that the prevailing wind direction in
Bartlesville is generally southerly during August and September.
However, because of normal meteorological variability, "upwind"
stations will not always be upwind and "downwind" stations will not
always be downwind. A review of the meteorological data shows that
for the days showing the greatest difference between upwind and
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25Q_
20Q_
CO
OL.
l/l
150
TOOL
Primary
Standard
Secondary
Standard
=1="
Sep 20
Aug 11
Aug 21
Aug 31
Sep 10
1
Sep 30
Figure^. Daily Particulate Concentrations - Station 1
.National Zinc Co., Bartlesville, Oklahoma
July 28 - September 26, 1977
ro
-Fi
-------
25Q.
150
0.
LO
100L
50.
0
Primary
Standard
Secondary
Standard
Aug 11
r
Aug 21
T
Aug 31
Sep 1C
Sep 20
Sep 30
Figure 5. Daily Participate Concentrations - Station 2
National Zinc Co., Bartlesville, Oklahoma
July 28 - September 26, 1977
ro
en
-------
Primary
Standard
250_
200.
150
Q-
t/1
Secondary
Standard
10CL
50.
nan
Illi ..111
BEE
iUV',.AJ ,i"l
iMwn.-1-j!
333BC
Sep 30
hMMMM>Mfe>| -
Aug 11 Aug 21
r
Aug 31
T
Sep 10 Sep 20
Figure 6. Daily Participate Concentrations - Station 3
National Zinc Co., Bartlesville, Oklahoma
July 28 - September 26, 1977
ro
en
-------
Primary
Standard
25CL
20Q_
0.
to
TOOL
Secondary
Standard
Aug 11
Aug 21
Aug 31
Sep 10
Sep 20
Sep 30
Figure 7. Daily Particulate Concentration - Station 4
.National Zinc Co., Bartlesville, Oklahoma
July 28 - September 26, 1977
ro
vj
-------
Primary
Standard
25CL
CL
1/1
20Q.
150
100.
50.
Secondary
Standard
Aug 11
Aug 21
Aug 31
Sep 10
Sep 20
I
Sep 30
Figure &. Daily Particulate Concentrations - Station 5
National Zinc Co., Bartlesville, Oklahoma
July 28 - September 26, 1977
00
-------
Table 5
STATISTICAL SUMMARY OF TSP DATA
NATIONAL ZINC COMPANY
BARTLESVILLE, OKLAHOMA
July 28 - September 26j 1977
29
Statistical
1
Station
2 3
4 5
3
vg/m
Geometric Means 79.2
1st Maximum 184
2nd Maximum 149
Minimum 30
No. of Primary 0
Standards
Excursions
No. of Secondary 1
Standards
Excursions
49.7 42.5
91 92
89 72
28 18
0 0
0 0
62.1 76.9
144 224
117 188
19 25
0 0
0 5
-------
30
Table 6
STATISTICAL SUMMARY OF SOd DATA
NATIONAL ZINC COMPANZ
BARTLESVILLE, OKLAHOMA
July 28 - September 26 3 1977
Station S04 TSP
vg/m
Arithmetic mean for Stations 1,45 11.0 89.5
Arithmetic mean for Stations 2, 3 7.3 44.7
Station 1 mean 8.65 95.6
Station 3 mean 7.1 43.4
Station 5 mean 14.3 81.0
-------
31
downwind sulfate concentration (August 8, 9, 13, 22, 26, 27, and 30),
there were persistent southerly winds. Also, although there is no
strong positive correlation between absolute levels of TSP and SOT,
the results do show that in general an increase in TSP from upwind to
downwind sites is accompanied by a corresponding increase in SOT.
Results of some epidemiological studies on sulfates identify an
association between ambient sulfate levels and adverse health
effects.3 However,' such statistical associations do not permit a
firm conclusion that a cause-effect relationship exists. Never-
theless, it should be noted that the SOT concentrations recorded
during this survey are comparable to levels ranging from 1.7 to 17.0
3
ug/m , which in various studies have been associated with adverse
health effects.
Metals
Ambient - The trace metals in air data are expressed as micro-
grams (|jg) per filter [Appendix I]. The only metals found by emis-
sion spectroscopy to be consistently above the detection limits were
zinc, lead, iron, and copper [Table 7]. There is a four- to six-fold
enrichment in zinc values comparing the upwind Station 3 with the
downwind Stations 1, 4 and 5. Lead enrichment ranged up to six-fold,
iron up to twenty-five-fold, and copper up to two-fold.
Based on the average measured flowrates, the highest lead concen-
tration was 2.5 (jg/m (September 8, 1977 at Station 4) and the mean
concentration for all stations and sampling days was less than 1.
ug/m . These values compare closely with an average value of 1 ug/m
determined at the National Air Surveillance Network (NASN) sites in
other industrialized areas from 1965 through 1975.1
-------
Table 7
AMBIENT AIR METALS ANALYSIS
NATIONAL ZINC COMPANY
BARTLESVILLE; OKLAHOMA
September 1977
32
Station Metal
No.
1 Zinc
Lead
Iron
Copper
3 Zinc
Lead
Iron
Copper
4 Zinc
Lead
Iron
Copper
5 Zinc
Lead
Iron
Copper
9/2
350
80
690
9
50
-------
33
The mean and maximum zinc concentrations for all stations were 3
and 13 |jg/m , respectively. Unfortunately, the report of NASN trace
metals data did not include zinc.
The highest and mean copper concentrations were 0.3 and 0.13
2
p/m . This data is consistent with the NASN mean value for copper of
3
approximately 0.1 |jg/m . The highest and mean iron concentrations
3
were 11.3 and 3.3 pg/m , respectively. The mean iron concentration
* ' 3
is somewhat higher than the NASN value of 1 pg/m .
Soils - The analysis of the 7 soil samples showed very large
enrichments of zinc, lead, cadmium, and copper at Stations 1 and 5
compared to Station 3 [Table 8]. The mean of the values from samples
3-02 and 3-03 were used as the upwind value as sample 3-01 was con-
taminated from the road nearby. The mean and maximum enrichment
factors for zinc were 50 and 85 comparing Stations 1 and 5 with 3.
The mean concentration of zinc in the earth's crust is 60 pg/g.2
Station 3 (mean - 450 pg/g) had values 7 times the crustal value,
but Stations 1 and 5 (mean - 22,500 pg/g) had values 375 times the
crustal value.
The mean and maximum enrichment factors for lead at Stations 1
and 5 compared to Station 3 were 24 and 31, respectively. The mean
crustal abundance of lead is 15 pg/g. The lead concentration at
Station 3 (mean - 68 pg/g) was 4.5 times the crustal abundance, but
Stations 1 and 5 (mean - 1,650 pg/g) had values 110 times the crus-
tal abundance.
The mean and maximum enrichment factors for cadmium at Stations
1 and 5 compared to Station 3 were 305 and 500, respectively. The
mean crustal abundance of cadmium is 0.1 ug/g. The cadmium concen-
tration at Station 3 (mean - 1 pg/g) was about the same as the
crustal abundance, but Stations 1 and 5 (mean - 350 pg/g) had values
3,500 times the crustal abundance.
-------
34
Table 8
SOIL SAMPLES METALS ANALYSIS - STATIONS 13 3, 5,
NATIONAL ZINC COMPANY
BAETLESVILLE; OKLAHOMA
July 28 - September 26, 1977
Metal
Analyzed
Zinc
Lead
Iron
Copper
Cadmium
Station - Sequence No.
1-01
13,900
1,300
54,100
330
137
1-02
33,000
2,100
57,800
640
350
3-01*
970
150
93,900
37
7
3-02
vg/<
304
58
32,100
18
<]
3-03
3
570
77
46,400
15
"
5-01
38,300
1,800
40,600
640
500
5-02
5,000
1,400
29,000
410
420
6-01
260
62
10,800
19
41
Disregarded because probable contamination from nearby road elevated the
concentration beyond expected value (see samples 3-02 and 3-03).
-------
35
The mean and maximum enrichment factors for copper at Stations 1
and 5 compared to Station 3 were 31 and 39, respectively. The mean
crustal abundance of copper is 30 ug/g. The copper concentration at
Station 3 (mean - 17 ug/g) was 0.6 times the crustal abundance, but
Stations 1 and 5 (mean - 510 ug/g) had values 17 times the crustal
abundance.
REMOTE SENSING
The false color infrared photographs that were taken during the
September 19, 1977 aerial surveillance mission were photointerpreted
tree-by-tree by NEIC personnel and the location of each tree exhibit-
ing chlorophyllic stress was plotted on U. S. Geological Survey
(USGS) 7.5 minute maps (Scale 1:24,000). Figure 9 shows the area
covered by the photographs. The cross-hatched area displayed the
greatest amount of chlorophyllic stress in the trees, having a
stressed tree density from 2 to 10 times that for other areas within
the photocoverage boundary. Since, climatologically, the most fre-
quent wind direction in the Bartlesville, Oklahoma, area is south-
erly, this area is downwind of the National Zinc plant more fre-
quently than any other area surrounding the plant.
BOTANICAL ASSAY
No morphological plant changes attributable to S02 were observed
during the in situ bioassay. There were no observable differences
among plants exposed to ambient air and plants grown in closed green-
houses supplied with sparged (S02 free) air, except for one exposed
Schefflera sp. from Station 2, which exhibited brown spots with black
rings on several leaves. However, no other plants exhibited spots,
and detectable S0? levels were recorded at this station for only two
^ o
hours during the entire survey (maximum level - 520 ug/m ).
-------
36
Virtually no
stressed tree
detected
rea where
(Chlorophyl
Virtually no stresse
trees detected
Scale 1:24000
Sand Creek
Figure 9. Aerial Infrared Photography Coverage
National Zinc Co., Bartlesville, Oklahoma
July 28 - September 26, 1977
-------
37
The effect of emissions from National Zinc Company on area soil
characteristics was investigated. Soil samples collected downwind of
the National Zinc plant at Stations 1 and 5 contained metals concen-
trations averaging 22,500 ug/g for zinc, 1,650 ug/g for lead, 350
|jg/g for cadmium, and 510 ug/g for copper. The average soil pH for
these stations was 7.90 [Table 9]. Upwind of National Zinc, at
Stations 3 and 6, metals concentrations were lower and pH higher
355 |jg/g for zinc, 65 |jg/g for lead, <1 pg/g for cadmium, 18 ug/g
for copper, and a pH of 9.33. Pilea sp. grown in soil with a pH of
7.16, from near Station 1 responded differently than similar plants
grown in soil from Station 6, which had a soil pH of 9.15. Pilea sp.
grown in soil from Station 1 averaged 0.5 cm taller in height than
Pilea sp. grown in soil from Station 6. However, the plants grown in
soil from Station 1 were chlorotic and contained only 28% as much
chlorophyll as did similar plants grown in soil from Station 6. In
summary, as Table 5 shows, the two soils had different pH values and
Station 1 had a much higher concentration of metals.
-------
38
Table 9
SOIL pH AND AVERAGE METAL CONCENTRATIONS
NATIONAL ZINC COMPANY
BARTLESVILLE, OKLAHOMA
July 28 - September 26, 1977
Station
1
3
5
6
NNE of
SSW Of
North
4 mi .
National
National
Zi
Zi
of National
south of
nc
nc
Zinc
National Zinc
pH
7
9
8
9
.16
.40
.65
.15
Zinc
23,450
437
21,650
260
Lead Cadmium
pg/g
1,700 244
68 <1
1,600 460
62 <1
Copper
485
17
525
19
-------
39
REFERENCES
1. National Trends in Trace Metals in Ambient Air, 1965-1974, EPA-
450/1-77-003, February 1977.
2. Wedepohl, K. H., "Origin and Distribution of the Elements," p 999,
L. H. Ahrens, Ed., Pergamon Press, London, England, 1968.
3. Statement of S"ulfates Research Approach, EPA-600/8-77-004, February
1977.
4. Holzworth, G.C., "Mixing Heights, Wind Speeds, and Potential for
Urban Air Pollution throughout the Contiguous United States," EPA-
AP-101, January 1972.
-------
APPENDICES
A QUALITY ASSURANCE AUDIT REPORT
B TSP FILTER CARD SAMPLE
C CHAIN-OF-CUSTODY PROCEDURES
D ANALYTICAL PROCEDURES
E METEOROGICAL DATA
F RAW SO, DATA
G RAW TSP9 DATA
H RAW SO/DATA
I RAW METALS DATA
-------
APPENDIX A
QUALITY ASSURANCE AUDIT REPORT
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
10 Quality Assurance Officer DAJE October 31, 1977
FROM Technical Coordinator
Inorganics and Air
SUBJECT Quality Assurance Support for the Ambient Air Quality Study in Bartlesville,
Oklahoma, September 1 and 2, 1977
I. Purpose
Sulfur dioxide and total suspended particulates were measured by continuous
instrumental and Hi-Volume sampling methods, respectively. An auditing
program was conducted to estimate data quality. The audit was conducted
independently of the routine operation of the sampling and testing network.
That is, checks were made by individuals other than the regular operators.
II. Approach
Six sets of samples were collected from the SOg calibration system utilizing
a bubbler box. See Table I. Prior to the sampling, the critical orifices
of the hypodermic needles were calibrated so that flow in 1/min could be
calculated. See Table II. The sampling was performed in order to verify
the calibration of the continuous sulfur dioxide monitors.
An orifice calibration unit with five different resistance plates was cal-
ibrated against a positive displacement primary standard (rootsmeter).
See Table III. This was done because a calibrated orifice unit is the
specified unit for calibrating the flow rate of both rotameter and flow-
rate recorder equipped samplers.
III.Results
The data in Tables IV and V show a slight positive bias of the values ob-
tained using the Pararosaniline Method compared to the S0£ calibration
system values (mean, +5.2%) and between the NEIC and RTP simulated values
(mean, +6.6%). The samples collected for Pararosaniline analysis were
collected in duplicate and the standard deviation of the duplicate values
in five out of the six sets of samples collected was quite small.
After the orifice calibration unit was calibrated against a positive dis-
placement primary standard (rootsmeter), the orifice assembly and field water
manometer was then used to measure the static pressure of two different
hi-volume samplers, Table VI.
-------
TABLE I - Sampling Data
Set
Run No.
1
1
1
2
2
2
3
3
3
4
4
4
5
5
6
6
Tube/Saiple
No. with TCM '
OA1
OA2
QA4
OA5
QA7
QA8
QA10
QA11
QA13
QA14
OA15
QA16
TABLE II - Needl
ml Tube/Sample ml
TCM No. with H709 H909
10
10
10
10
10
10
10
10
50
50
50
50
e (Critical
Needle No. Date & Time
QA3 50
QA6 50
QA9 50
QA1 2 50
Orifice) Calibration
Flow Time/0.1 1
Critical
Orifice No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
2
1
Data
Flow, I/mi
Expected
Cone. Range
0.1-0.2 ppm
0.1-0.2 ppm
0.1-0.2 ppm
0.2-0.3 ppm
0.2-0.3 ppm
0.2-0.3 ppm
0.3-0.4 ppm
0.3-0.4 ppm
0.3-0.4 ppm
0.4-0.5 ppm
0.4-0.5 ppm
0.4-0.5 ppm
0.1-0.2 ppm
0.1-0.2 ppm
0.2-0.3 ppm
0.2-0.3 ppm
Ave. Fl
n 1/min
Sample
Times
60 min
60 min
60 min
60 min
60 min
60 min
60 min
60 min
60 min
30 min
30 min
30 min
72.5 min
72.5 min
72 min
72 min
ow
9/1/77 AM
0.169
0.592
1
1
1
1
2
2
2
2
3
3
3
3
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
9/1/77
AM
AM
PM
PM
AM
AM
PM
PM
AM
AM
PM
PM
0.172
0.169
0.169
0.170
0.168
0.168
0.165
0.165
0.181
0.180
0.172
0.172
0.582
0.592
0.592
0.589
0.595
0.595
0.696
0.606
0.552
0.556
0.581
0.581
0.589 = V?
0.600 = V?
0.568 = 73
TABLE III - Calibration of the Orifice Against the Rootsmeter Data
Resistance Plate No. True Air Flow Rate (m3/min)
18
13
10
7
5
1.78
1.64
1.42
1.15
0.86
-------
3
TABLE IV - Pararosaniline Method vs SO? Calibration System Values
Camples
Pararosaniline
Method Values
Pararosanaline
Average Values
S02 Calibration
System Values
QA1
QA2
QA4
QA5
QA7
QA8
QA10
QA11
QA13
QA14
QA15
QA16
0.171 ppm
0.180 ppm
0.179 ppm
0.273 ppm
0.284 ppjn
0.628 ppm
0.588 ppm
0.168 j>pm
0.151 ppm
0.296 ppm
0.273 ppm
0.176 ppm
0.179 ppm
0.278 ppm
0.608 ppm
0.160 ppm
0.284 ppm
0.150 ppm
0.201 ppm
0.299 ppm
0.486 ppm
0.153 ppm
0.250 ppm
+14.8%
-12.3%
- 7.6%
+20.0%
+ 4.4%
+12.0%
TABLE V - RTF vs NEIC Simulated Values
S02 Quality Assurance
Material Samples
RTF
Values
NEIC
Values
Percentage
Difference
10627
20694
3D876
40346
50055
21 .90 ug/m3
48.23 ug/m3
80.17 ug/m3
114.70 ug/m3
155.40 ug/m3
18.52 ug/m3
52.46 ug/m3
98.75 ug/m3
129.64 ug/nP
160.40 ug/m3
-15.4%
+ 8.8%
+23.2%
+13.0%
+ 3.2%
TABLE VI - Orifice #5 vs Field Orifice Air Flow Rates
Hi-Volume Manometer True Air Flow Rate Air Flow Rate
Sampler No. Reading, in. H?0 m3/min, Orifice #5 m3/min, Field Orifice
43
65
6.0
5.9
1.23
1.22
1.20
1.19
-------
4
The true air flow rate versus the air flow rate measured via the field orifice
agreed very closely. A difference of 0.03 m3/min was detected for Hi-Volume
Sampler No. 43-and the same difference for sampler No. 65. The results show
that the flow rates that are being measured on the hi-volume samplers are
correct values.
IV. Discussion
The results from the six sets of samples collected for the sulfur dioxide
analysis, utilizing the Pararosaniline Method corresponded statistically
well with the values obtained through the S02 calibration system. Also
the NEIC values for the 3Q2 Quality Assurance Samples compared very well
to the known values obtained from the EPA Quality Assurance Laboratory in
Research Triangle Park, North Carolina.
Percentage difference values of less than +20% for SO? Quality Assurance
Samples are considered acceptable values. Since only one sample exceeded
20%, the level of confidence of analysis for the quality assurance samples
was good. None of the percentage difference values for the samples collected
for Pararosaniline Analysis as compared to the SOg Calibration System Values
exceeded +20%. The level of confidence comparing the two sets was well
within experimental error.
The zero and span were checked every eight hours on the Lear Siegler SO?
monitors and the zero was checked once a day on the Bendix instruments.
A standard curve was run once in August before the start-up and once in
September after the start-up.
The flow of the Hi-Volume samplers was measured before and after changing
the filters. The calibration orifice unit with five different resistance
plates should have been calibrated against a positive displacement primary
standard (rootsmeter) prior to the beginning of the survey.
V. Attachments - Methods Description
Sampling
Samples were collected using an absorber assembled set-up and sampling train
Three 23 gauge hypodermic needles 1 inch long were used as critical orifices
that produced a flow of approximately 5 liter/minute each. Six sets of
samples were collected with the first four sets being collected in triplicate
and the last two in duplicate. A soap-bubble meter was used to measure the
flow of the critical orifices of the hypodermic needles.
The respective mill inters of each absorbing solution were added to the
impingers. Aluminum foil was wrapped around the impinger tubes in order
to prevent deterioration from direct sunlight during and after sampling
The volume of air sampled was determined by multiplying the flow rate by
the time in minutes and recording the atmospheric pressure and temperature
The samples were removed from the impingers, stoppered, and iced at 4°C
-------
Calculations of Volume of Air @25°C and 760 mm Hg, liters
VR = V x P x 298
760 t+273
VR - flow rate corrected to STP
P = barometric pressure, mm Hg = 753.11
t = temperature of air sample, °C = 24
V = volume of air samples, liters = Vi = 0.589
V2 = O.COQ
V3 = 0.568
VR1 = Vn x P x 298
760 t+273
VRI = 0.589 1 x 753.11 x 298
mTff 760 24+273
VR1 = 0.589 x 0.991 x 1.003
VRI = 0.585 1/min
VR2 = 0.597 1/min
VR3 = 0.564 1/min
Analysis
The reagents and solutions were prepared as is outlined in Part 6, pp. 6
and 7 of the Federal Register, App. A, Title 40 - Protection of Environ-
ment. The stock sodium thiosulfate solution was standardized with the
primary standard potassium iodate as shown below:
N = W x 2.80
M
N = normality of stock thiosulfate solution
M = volume of thiosulfate required, ml = 41.58 and 41.55, Avg. = 41.56
W = weight of potassium iodate, grams =2.000
2.80 = IP3 (conversion of g to mg) x 0.1 (fraction iodate used)
35.67 (equivalent weight of potassium iodate)
N = 2.000 x 2.80
41756-
N = 0.1347
-------
The sulfite solution was standardized by adding excess 0.01 N iodine
solution and back-titrating with 0.0135 N sodium thiosulfate solution.
The working sulfite-TCM solution was prepared at the same time the iodine
solution was added to the flasks. The concentration of sulfur dioxide in
the working solution was calculated as follows:
ugS02/ml = (A-B)(N)(32.000) x 0.02
25
A = volume thiosulfate for blank, ml = 47.36 and 47.29, Avg. 47.32
B = volume thiosulfate for sample, ml = 21.10 and 20.90, Avg. 21.00
N = normality of thiosulfate titrant = 0.0135
32,000 = milliequivalents wt. of S02, ug
25 = volume standard sulfite solution
0.02 = silution factor
ug S02/ml = (47.32 - 21.00)(0.0135)(32.0QO) x 0.02
25
ug S02/ml = 9.10
Graduated amounts of the working sulfite-TCM solution were pipetted in a
series of 25 ml volumetric flasks (0, 0.5, 1, 2, 3, and 4 ml). Sufficient
TCM solution was added to each flask to bring the volume to approximately
10 ml. The total ug $02 in the solutions equalled the concentration of
the working sulfite-TCM solution in ug S02/ml times the ml working sulfite
solution added.
(ug S02 = ug S02/ml x ml added)
0 ug S02 = 9.1 ug S02/ml x 0 added
4.6 ug S02 = 9.1 ug S02/r:il x 0.5 added
9.1 ug S02 = 9.1 ug S02/ml x 1.0 added
18.2 ug S02 = 9.1 ug S02/ml x 2.0 added
27.3 ug S02 =9.1 ug S02/ml x 3.0 added
36.4 ug S02 =9.1 ug S02/ml x 4.0 added
The contents of the 30 minute and 1 hour samples were transferred quanti-
tatively to 25 ml volumetric flasks and rinsed with absorbing solution.
Analyses were delayed for 20 minutes to allow any ozone to decompose.
The samples that were collected in 50 ml of absorbing solution were trans-
ferred quantitatively to 50 ml volumetric flasks and diluted with absorbing
solution. 5 ml of the samples were then pipetted into 25 ml volumetric
flasks for chemical analyses. The volume was brought up to 10 ml with
absorbing reagent and analyses v/as delayed for 20 minutes to allow any
ozone to decompose.
A reagent blank was prepared by adding 10 ml unexposed TCM solution to a
25 ml volumetric flask. A control solution was prepared by adding 2 ml
of working sulfite-TCM solution and 8 ml TCM solution to a 25 ml volumetric
flask.
-------
To each flask containing either working sulfite-TCM solution sample,
control solution, or reagent blank, 1 ml of 0.6 percent sulfamic acid
was added and allowed to react 10 minutes in order to destroy the nitrite
from oxides of nitrogen. 2 ml of 0.2 percent formaldehyde solution,
followed by 5 ml pararosaniline solution was then added. All flasks were
brought to volume with distilled water and mixed thoroughly.
After 30 minutes and before 60 minutes, the absorbances of the working
sulfite-TCM solutions, samples (denoted asA), reagent blank (denoted as Ao)
and the control solution were read at 548 nm using a 1 cm optical path length
cell. Distilled water, not the reagent blank was used as the reference.
Five S02 Quality Assurance Material Samples were requested and received
from Quality Assurance Laboratory in Research Triangle Park, North Carolina.
They were prepared by Polysciences, Inc. and were analyzed along with the
working sulfite-TCM solutions, samples, control solution, and reagent blank.
The S02 Quality Assurance Samples were diluted to 50 ml with absorbing
solution and prepared for analysis in the same manner as the field samples
collected in 50 ml of absorbing solution.
Standards (Working Sulfite-TCM Solutions)
0 ug SOo/25 ml
4.6 ug 502/25 ml
9.1 ug S02/25 ml
18.2 ug S02/25 ml
27.3 ug S02/25 ml
36.4 ug S02/25 ml
Reagent Blank/25 ml
Control Sol 'n/25 ml
Absorbance
0.124
0.222
0.324
0.545
0.714
0.911
0.125
0.562
Samples
QA1
QA2
QA4
QA5
QA7
QA8
QA10
QA11
QA13
QA14
QA15
QA16
Absorbance
0.463
0.488
0.480
o.m
0.666
0.703
0.744
0.720
0.164
0.161
0.196
0.189
-------
8.
SOg Quality Assurance Material
10627
20694
30876
40346
50055
Absorbance
0.136
0.158
0.188
0.208
0.228
ug SOo/m3 = (A-Ao) x (IP)3 l/m3 x (Ba)ug/^ x D
'
A = sample absorbance
Ao = reagent blank absorbance
103 = conversion of liters to cubic meters
Ba = calibration factor, I/slope
D = dilution factor
For 30 minute and 1 hour samples, D = 1
For 24 hour samples, D = 10
VR = the sample volume corrected to 25°C and 760 mm Hg
St = sample time
Example: Sample Calculation (Sample QA1 )
ug S02/m3 = (0.463 - 0.124)(1Q3)(46.29) x 1
(0.585)(60)
ug S0?/m3 = 447
ppm S02 = 447 ug/m3 (3.82 x 10~4)
ppm SO? = 0.171
Example: SO? Quality Assurance Material (10627)
ug S02/m3 = (0.136 - 0.124)(103)(46.29) x 10
300
300 = sample volume per time value provided by the EPA Quality Assurance
Laboratory in Research Triangle Park, North Carolina
ug S0?/m3 = 18.52
Calibration of the Orifice
The true air volume measured by the positive displacement primary standard
was calculated using the five resistance plates as shown below:
Va = (Pa - Pm) x Vm
(Pa)(T)
Va = true air volume at atmospheric pressure, mj/min
Pa = barometric pressure, mm Hg
Pm = pressure drop at inlet of primary standard, mm Hg
Vm = volume measured by primary standard, m3
T = time, mi n
-------
*
-------
q =.
10
ORIFICE CALIBRATION ^-
=. *i»i
Orifice Calibration Unit Number
Roots Meter Number
Laboratory Temperature_
Motor Number
Pressure
nunllg
Voltage
vac
DATE °\-\-T-l
OPERATOR
Verified by
Plate
No.
16
>3
is
"1
5
Volume
of Air
Passed
ft
3
m
YW.
5,*0
b.oo
5.**
5,oe
5-00
Time
of
Total
Airflow
(min.)
T
^.k4
-------
o
OJ
CO
2;
zi
11
15
14
13
12
11
10
9
8
ORIFI
TE
EMP.
VOLTS
NAME
_ORIFICE. CALIBRATION CURVE
^OOTSMETE
oc
Tirr
JTV^
:[::
:i:1:
BAROMETER
i
DATE
mm
Hg,..
T:
;.bi
i-tr
4z
...
'.\'jr.i
:\.~:-. \-
mtm^::
:]-;>:rtrt_
=S
IS
:).-::'!-: !
0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2.0
-------
12
For resistance plate no. 18:
Va = (753.11 - 44.0) x 5.00 m3
(753.11 HZ-649 min}
Va =1.78 m3/min
D. David Vietti
-------
APPENDIX B
TSP FILTER CARD SAMPLE
-------
HI-VOl DATA RECORD
(Continued)
PARTICIPATE DATA - For Lob Use Only
rilfi_r Gro&& wgl
Filler lore Wgt
NCI Poinculcte '^gi ___
InmaJ r* *nin
Final *n mm
Pnrticula'e Conccn[ro'ion_
Toial SamoiFng li*nv
Qtoms
_ grams
ENVIRONMENTAL KO'SCT.ON AGENCY
O7flCE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTE?
Bldg 53 Bo«. 25277, Oonvei Fec'erol Center
Denver. Colorado 30215
HI-VOL DATA RECORD
SUIIO:.
CLOG, ff£A' '.C
i'O? S...' P. ' O ..
c oc% PE.T'^G
is.0 .,-.
'i'£i..r/ i'
-------
APPENDIX C
CHAIN-OF-CUSTODY PROCEDURES AND RECORDS
-------
ENVIRONMENTAL PROTECTION AGENCY
NATIONAL ENFORCEMENT INVESTIGATIONS CEMTER
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 Ho. 1, second sample - sequence flo. 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,
-------
E-2
DO, pH, flov; and any other pertinent information or observations. The
entries shall be signed by the field sampler. The preparation and conser-
vation .of the field logbooks during t.-.e survey will be the responsibility
of the survey coordinator. Once ths 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 -.0 the receiving laboratory or turned
over to an assigned custodian. He r.-jst assure that each container is in his
physical possession or in his view z: all times, or locked in such a place
and manner that no one can tamper with it.
7. Colored slides or photographs should De taken which would visually show the
outfall sample location and any wate- pollution to substantiate any con-
clusions of~the- investigation. Writ:en documentation on the back of the
photo should include the signature
-------
E-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
testing procedure. 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 view 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 v/ill first confer with the Chief,
Enforcement Specialist Office, to make certain that the information is no
longer required or the samples have deteriorated.
-------
E-4
EXHIBIT I
EPA, NATIONAL
E Station No.
ENFORCEMENT INVESTIGATIONS CENTER
1 Dale Time Sequence No.
9 Station Location
u
*
=^ BOD
Jfi Solids
COD
Nutrient?
«
Melafs
Oil ani| Greece
DO.
Barf.
OlW
Samplers:
V
Gr?b
C*>rnp.
Romarb/Projorvative:
Front
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
£
X
Back
-------
EXHIBIT'II
SURVEY, PHASE.
DATE
: OF SAMPLE.
'ANALYSES REQUIRED
MION
IMBER
-
STATION DESCRIPTION
'
TOTAL VOLUME ' |
TYPE CONTAINER
PRESERVATIVE '
%
*
.
"
,
. .
NUTRIENTS |
Q
O
to
0
O
U
U
o
t
f
t/>
Q
~j
o
(/)
<
0
t
SUSPENDED SOLIDS |
ALKALINITY |
O
Q
I
D.
! CONDUCTIVITY' |
| TEMPERATURE' |
0
u.
6
u
<
h
O
>
| FECAL COLIFORM ]
| TURBIDITY 1
UJ
1/1
<
UJ
01
o
O
Z
<
_i
o
| METALS |
U
<
£3
t
\n
UJ
o
u
Lo
i_i
a.
ez
Cu-
>-j
X
1
| TRACE ORGANICS I
0
r
^.
taJ
=L
1
Ui
-------
XH II
Samplers:,
FIELD DATA RECORD
STATION
NUMBER
'
DATE
t
TIME
TEMPERATURE
c
CONDUCTIVITY
^mhos/em
-
"
PH
S.U..
/
D.O.
mg/l
i
GcgcHl.
or Flow
Ft. or CFS
* i
-.
i
'
i
i
1
\
i
I
i
«
t
i
* i
i
4
-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
E-7
SURVEY
2>><\('-"':r O,L
StATlON
NUMBER
Z OO 1
TO'?'
/ OC /
"-30 '
^of
Too/
f- W
STATION IOCA1ION
-£^'/^£vz -*&:<
7'jc. v -~/?/~> /<-'* r^/vir '<
/
if
ft
if
II
.
DATE
?^3/7-
^'^/^
^4-4,
9/i *2'T>
^ll^f-p
vfcfa
9//3h^>
Relinquished by: (stature) ^
Relinquished by: (Signature)
Relinquished by: fSignofu.-ej
Relinquished by: (Signature)
Dispatched by: fs.gnciurej
Date,
TIME
SAMPLERS: (Signature)
SAMPLE irPE
Wa-er
Comp
Grab.
Air
*
X
s,X
W
V
^
V
SEQ
NO
0'
c^
o?
Qf
P*
(.' y
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NO OF
CONTAINERS
/
:
'
/
/
/
/
ANALYSIS
REQUIRED
-*-'?t_j '. / - r
"^Z*.^'*^
'---i&^r?*'
-^~j^n f'ii^~*Z. f? .' V^'" !'
"^ / ^ j. _
- L» / - r ~ --
~"r gr^rjZ-
' fj"'\j^:lt v "-"" '
c;^) / j, ,-.. / -^
^;t^51;;>'-
Received by: 'Signature)
Received by: ,'-'gna>urey
Received by: ;signoiure)
Received by Mobile Laboratory for field
analysis: (stgrotui»i
/Time
Received for Laboratory by: - "
.Method of Shipment:
Date/Time
Dote/Time
Dote/Tfme
Date/Time
Date/Time
/ ? j
Distribution: Orig. Accompany Shipment
1 Copy Survey Coordinator Field Files
GFO S79-O4O
-------
APPENDIX D
ANALYTICAL PROCEDURES
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53. BOX 25227. DENVER FEDERAL CENTER
DENVER, COLORADO 80225
10 Deputy Chief DATE October 31, 1977
Chemistry Branch
FROM Trace Elements Coordinator
SUBJECT National Zinc, Bartlesville, Oklahoma
Low-Vol Filters
Fifteen membrane filters representing three subject air sampling stations
from each of five days were selected for analysis. In addition, a fourth
station yielded two samples plus two blanks for four of the same five days.
One fourth of each of these samples and blanks were prepared per APHA Methods,
of Air Particulate Sampling and Analysis. That method was to digest one
quarter portions of the filters with 3 mis of concentrated nitric acid, heat
to fuming, add 3 mis of 70% perchloric acid, and heat again to white fumes,
cool and dilute to 25 ml. One ml of each of the resulting solutions was then
diluted to 10 ml with deionized water and analyzed by inductively-coupled
argon-plasma (ICAP) emission spectroscopy. One ml of each of the solutions
was also used for selenium analysis by graphite furnace atomic absorption
using the method of standard additions. In addition, nine other quarter
portions (three stations for three days each) were analyzed by x-ray fluor-
escence (XRF).
Other observations can be made using the ICAP data attached (Table I);
however, without flow data to calculate total masses, I will attempt no in-
terpretation. Note that mercury data are not included since the method of
sample collection and preparation makes any results questionable. By way
of quality assurance, three blank filter quarters were spiked with known
amounts of each of the twenty elements programmed into the ICAP emission
spectrometer. Table 2 lists the percent recoveries following the nitric/
perchloric acid digestion and subsequent analysis. All recoveries were
reasonable save those for tin, mercury, and selenium, which is not surprising
considering the volatility of some of the salts of these metals. MQDC values
also appear in Table 1.
Soil Samples
Seven soil samples were collected, two from the vicinity of the station 1
air sampler, three from station 3, and two from station 5. Those samples
were dried at room temperature, strained through a number 20 sieve, and mixed
well. A representative portion of each was then ground to less than 300 mesh
using a rotary mill. Approximately 250 mg portions were then digested using
the same nitric/perchloric digestion procedures as used for the membrane
filters and diluted to 2S ml. Analysis was done on 1:10 dilutions of these
solutions using ICAP only; the results appear in Table 3. Note the relatively
high zinc values for stations 1 and 5 compared to the upwind station 3 values.
The MQDL values listed differ from those for the membrane filter samples
-------
- 2 -
because of the difference in matrices in addition to the possible changes
in operating conditions since the soil samples were analyzed at a later
date than the membrane filters.
William L. Abbott
Attachments
-------
Page j__ of 4
ANALYTICAL DATA REPORTING SHEET
Name of Survey
Analyses
Performed
_Project Number -49-4
Station Number \ Station Description
Dates
Units
9/2/1
5/3/
77
en
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80
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360
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-------
"ame of Survey
station Number 3
Page ? of 4
ANALYTICAL DATA REPORTING SHEET
_Project Number 404
JStation Description
23 ft 132
Dates
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9/2/77
9/3/77
0/7/77
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-------
Page 2± of ^
ANALYTICAL DATA REPORTING SHEET
ame of Survey 6/J/?ncSWU.iT
Project Number 4Q4
station Number -4
JStation Description
Dates
...nalyses
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Units
9/1/77
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-------
TV* <2 L £ I
ANALYTICAL DATA REPORTING SHEET
Page _ of
Project Number 494-
Station Number <" Station Description Al>/*M5 4 ADfu^E BLVO
Analyses
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-------
Page J_ of J_
Hame of Survey
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ANALYTICAL DATA REPORTING SHEET
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Page ' / of i
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-------
APPENDIX E
METEOROLOGICAL DATA
CODE FOR FOLLOWING TABLES:
WS - Wind Speed (meters/sec)
T - Temperature (°F)
DP - Dew Point (°F)
WD - Wind Direction (°)
SG - Sigma (°)
P - Pressure (inches of Hg)
Station ID of 6011 is the same as Station 1
Day Hour Min Sec
Time - 00 00 00 00 (Day 01 is July 28, 1977)
-------
ftVEPrtGE MHE 60 H1NUTES
__ _ ID
01 10:uS:OQ HPIJCOO
£011 01 11 :00: 00 HP
him ni 1 jjflii- no HP
6011 01 13: 01) ' 00 HR
tOll 01 14:OOfOO HR
f/l)M._..0! 1.5:.nn.!.00,.H.R
60 11 01 IfcJOO :00 HR
6011 01 17:00:00 HR
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COI1 01 19: 00 : 00 HR
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6011 , 01.,.2.1.-.00.:..OO...KR
eon at 22:00:00 HR
6011 01 23:00)00 HR
ftlMl 02 OOJOOiOO HR
(Oil 02 01 .'00 tOO HR
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r,oit t\-j nt'.nmnn H"
eon 02 07:00:00 HR
6011 02 08:00:00 HR
LOU o? 04 inn mo HP
eon 02 10:00:00 HR
ecu 02 1 1 ) oo 100 HP
f-n\l ()> \2- nO l.OO-.HR
bCII 02 13:00:00 HR
601 1 0! 1 4:00 : 00 HR
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bOll 0.' 17)00:00 HR
fcO.1 1 0 2-J.S J 00 : 00-HR
COII 02 19:00:00 HR
eoil 02 20iOUiOO HR
i.rtii 02.3ijno;flo MR
eoil 02 22:00:00 HR
C011 02 23:00:00 HR
tn 1 1 03 QQ; QD i ao HR
eoit 03 01:00:00 HR
C01 1 03 02:00: 00 HR
toil 01 O1?: 00 : no HP
6011 03 04:00:00 HR
eon 03 05:00:00 HR
£01 I 03 06: 00 ! 00 HR
6011 03 07:00:00 HR
(Oil 03 08:00: 00 HP
66.23
66.79
e>9 R i
60.81
61 67
63 13
63 14
63.1 1
63 83
63.96
63.68
63.65
63.62
64 50
65.35
65.97
66.95
66 . no
64 92
64.49
63.64
64 .07
. . 67.23
66.56
66.47
tlfi
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2.78
34 60
31.67
43.89
341 . 51
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29 28
29 30
P
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-------
Rainfall Measurements from Tipping Bucket Rain Gage at Station
Date Amount (inches) Date Amount (inches)
8/1/77
8/2
8/3
8/4
8/5
8/6
8/7
8/8
8/9
8/10
8/11
8/12
8/13
8/14
8/15
8/16
8/17
8/18
8/19
8/20
8/21
8/22
8/23
8/24
8/25
8/26
8/27
8/28
8/29
.18
0
0
.07
.07
0
0
0
0
0
.13
.09
0
1.13
.16
0
1.34
.19
1.72
0
0
0
.31
0
0
0
0
1.63
0
8/30
8/31
9/1/77
9/2
9/3
9/4
9/5
9/6
9/7
9/8
9/9
9/10
9/11
9/12
9/13
9/14
9/15
9/16
9/17
9/18
9/19
9/20
9/21
9/22
9/23
9/24
9/25
9/26
9/27
0
0
0
0
0
0
.01
.04
0
0
0
.12
.51
0
.37
.94
.38
.33
0
0
0
0
0
0
0
0
0
0
0
-------
APPENDIX F
RAW S02 DATA
-------
F-J
SO, DATA
IMTJOIML ZINC COiSPMY AHDTUDT AW QUALITY SURVElt
rt, Oklahoma
No. 0-1 1-2 2-3 3-1 4-5 5-6 6-7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-18 18-19 19-20 20-21 21-22 22-Z3 23-24
August 1, 1977
1 <0.05°<.05 «.05 <.05 <.05 < .05
2
3
f
5 August 2, 1977
1 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 «0.05 <0.05 <0.05 -=0.05 <0.05 -=0.05 <0.05 <0.05 <0.05 <0.05
3
4
5 August 3, 1977
1 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 --0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
2
3
6
5 August 4, 1977
1 <0.05 <0.05 <0.05 <0.05 <0.05 ^O.OS <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 «0.05 <0.05 <0.05 *0.05
2
3
4
5 August 5, 1977
1 <0.05 <0.05 <0.05 <0.05
-------
Table l-'-l (Continued)
DATA
UJKifj' A1K QL
Cj Oklahoma
SO., DATA
zmc coiiViwr foiiuKm- AIK QUAUTY MHVI.Y
Station Hour-
No. 0-1 1-2 2-3 3-4 4-5 5-6 6-7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-1B 18-19 19-20 20-21 21-22 22-33 23-24
August 9, 1977
1 <0.05 -D.05 O.05 O.05 O.05 O.05 <0.05 O.05 0.11 0.1 0.13 0.23 0 09 0.07 0.11 0.32 0.27 0.2 0.08 <0.05 <0.05 <0.05 <0.05
-------
Table f-l
.70,,
NATIONAL KINi: CUHfAHY AHIIIUH'f Ml! IJIMI.ITY :,UhVhY
Bari.LoauiL1.Of Oklahoma
Slat ion HQUIL.
Ho. 0-1 1-2 2-3 3-4 4-5 5-6 6-7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-18 18-19 19-20 20-21 21-22 22-23 23-24
August 16, 1977
1 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 0.14 0.09 0.11
2 <0.05 -0 05 <0.05 <0.05 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3
-------
Table f'-J (ConLinued)
SO. DATA
ll,\TTONi\L 7.1 NC COMPANY UnnihNT ftlli QUALITY MHIVKY
Hr,rt.i<:;vi LL~
S Id 11 on !i°5!£_
No. 0-1 1-3 2-3 3-4 4-5 5-6 6-7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-18 18-19 19-20 20^21 ~2\-22 22-23 23-24
August 23, 1977
1 -0 05 <0.05 -0.05
2 -0.05 -=0 05 =0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3
4 <0.05 <0.05 <0.05 :0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
5 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
August 24, 1977
1 <0.05
2 "=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3
4 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
5 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 «0.05 <0.05 <0.05 <0.05 <0.05
August 25, 1977
1 <0.05
2 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3
4 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
5 <0.05 <0.05 <0.05 --0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 0.04 <0.05 0.04 0.03
August 26, 1977
1 <0.05
2 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3
4 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
5 <0.05 <0.05 <0.05 <0.05 <0.05 0.04 0.04 0.03 <0.05 0.12 0.12 0.12 0.12 0.12 <0.05 <0.05 <0.05
August 27, 1977
1 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
2 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3 <0.05
4 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
5 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 0.08 0.12 0.10 0.13 0.12 0.07 <0.05
August 28, 1977
1
2 <0.05 <0.05 <0.05 <0.05 '0.05 <0.05 <0.05 <0.05 <0.05 <0.05 :0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3 <0.05 <0.05 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
4 <0.05 <0.05 <0.05 <0 05 <*0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
5 --0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
August 29, 1977
1
2 <0.05 -0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3 -=0.05 <0.05 ^0.05 <0.05 <0.05 <0.05 <0.05 <0.05
4 <0.05 <0 05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
5 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
-------
Table l'-l (Continued)
50., DATA
NATIOML ZINC COMPANY folBTENT AIR QUALITY SURVKY
Bai'tlesvillc, Oklahoma
S ta 11 on Hour
»» O7! I7?2^3IP44^55^66^7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-18 18-19 19-20 20-21 2T-22 22-23 23-24
August 30, 1977
' <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0 05
2 <0.05 --0.05 <0.05 -0.05 <0.05 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0 05 <0 05 <0 05 <0 05 <0 05
3 -'0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0 05 <0 05 <0 05 <0 05
-------
fable I'-l (CtmLinued)
SO DATA
IMTIOML ZL1C COtiPAIlY AIIBFCIIT AIR QUALITY SURVEY
Oai'Ller.villc, Oklancira
Station Hour
No. 0-1 1-2 2-3 3-4 4-5 5-6 6-7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 1~T~18 18-19 19^20 20-21 21-22 22-23 23-24
September 6, 1977
1 -'0.05 <0.05 <0.05 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 '0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
2 -'0.05 ^0.05 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 '0.05 '0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 '0 05 <0 05
3 '0.05 -0.05 =0.05 --0.05 -0.05 <0.05 <0.05 <0.05 -"0 05 -'0 05 <0.05 <0 05 -0.05 '-0.05 <0.05 <0.05 --0.05 <0.05 <0.05 <0.05 <0 05 <0 05 --0 05 <0 05
4 -0.05 <0.05 -0.05 <0.05 <0.05 --0.05 <0.05 <0.05 =0.05 -O.C5 <0.05 <0.05 <0.05 -0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0 05
5 '0.05 -=0.05 <0.05 '0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
September 7, 1977
1 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <=0.05 <0 05 <0 05 <0 05 <0 05
2 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 --0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 -'0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3 -0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05
4 -0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0 05 <0 05
5 -0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
September 8, 1977
1 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 0.06 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05
2 -=0.05 =0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0 05 <0 05 <0 05
3 -0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0 05 <0 05
4 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 0.09 0.13 0.08 <0.05 <0 05 <0 05
-------
Table r-1 (Continued)
SO,, DATA
NATIONAL r,lt!< riVIPAllY 'AMIUrh'T /I//.' QUALITY fillKVKY
S in L i on . Hour
Mo. 0-1 1-2 2-3 3-4 4-5 5-6 6-7 7-0 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-18 18-19 19-20 20-21 21-22 22-23 23-24
September 13, 1977
1 <0.05 0.06 0.10 <0 05 0 06 0.09 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
2 --0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3
-------
Table F-J (Conli tilted)
SO,, IMT4
NATIONAL ZJNC COtirANY 'A11BIKHT AIR ()UALl'fY SUliVKlf
Bai'tlasviLLc, Oklahoma
Station Hour
Mo. 0-1 1-2 2-3 3-4 4-5 5-6 6-7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-18 18-19 19-20 20-21 21-22 22-23 23-24
September 20, 1977
1 <0.05 -=0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 Or> <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 =0.05 <0.05 <0.05 <0.05 <0.05 <0.05
2 <0.05 <0 05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05
3 <0.05
-------
Table /'-J (Continued)
.90., DATA
ZINC CtVil'ABV AMIUINT All! QUALITY MJKl'HY
Bai-lLc.sviUc,, OkLnhoiaa
Station Hmir
No. 0"-1 ~2 2T3~3-4 4-5 5-6 6-7 7-8 8-9 9-10 10-11 11-12 12-13 13-14 14-15 15-16 16-17 17-18 18-19 19~-2Q 20-21 21-22 22-23 23-24
September 27, 1977
1 -0 05 <0 05 -0 05 <0.05 <0.05 <0 05 <0.05 <0.05 <0.05 <0.05 <0.05 '0.05 <0.05 -=0.05 '0.05 '0.05 <0.05 -=0.05 «0.05 <0.05 <0.05 <0.05 <0.05 <0.05
2 0 05 <0.05 '0 05 '0.05 '0.05 <0.05 <0.05 <0.05 <0.05
3
l\
5 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 <0.05 -=0.05 <0.05 -=0.05 <0.05
-------
APPENDIX G
RAW TSP2 DATA
-------
Table 5-1
TSP DATA
NATIONAL ZINC COMPANY AIR QUALITY MONITORING SURVEY
Bartlesville^ Oklahoma
Sampling
Date
(1977)
Aug.
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
Sept.
1
2
3
4
5
6
7
1
76
107
78
149
65
103
101
126
47
55
80
74
117
126
68
88
44
67
113
59
106
104
88
32
77
74
89
84
184
140
55
83
132
2
41
49
36
42
63
37
44
55
36
44
38
43
51
38
57
60
69
57
41
37
56
49
63
72
70
66
91
Station
3
yg/m3
52
48
46
41
33
41
47
41
37
42
37
30
38
54
34
55
37
38
32
45
31
64
52
57
54
23
34
30
38
42
56
65
62
52
66
92
4
48
29
40
86
61
25
59
50
60
38
76
50
66
107
109
82
28
41
74
81
100
117
101
75
51
57
91
5
58
94
104
112
57
67
57
61
61
90
40
51
44
61
92
85
93
61
89
109
90
28
51
64
78
73
97
112
93
54
80
122
-------
Table G-l (Continued)
TSP DATA
NATIONAL ZINC COMPANY AIR QUALITY MONITORING SURVEY
Bartlesville3 Oklahoma
Sampling
Date
(1977)
Sept.
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
1
131
105
86
44
59
39
30
34
46
48
70
124
85
107
86
98
84
105
2
89
81
71
29
28
32
38
33
40
49
51
58
44
74
62
Station
3
yg/m3
72
65
38
37
18
23
30
31
28
34
38
40
59
53
41
55
53
4
144
85
78
62
72
19
24
44
59
49
44
42
98
101
117
96
77
64
5
151
170
76
60
81
32
25
35
61
67
103
188
115
94
92
108
155
224
-------
APPENDIX H
RAW S02 DATA
-------
Table H-l
SULFATE' DATA
NATIONAL ZINC COMPANY AIR QUALITY MONITORING SURVEY
Bartlesville, Oklahoma
Date
(1977)
3
5
8
9
13
14
16
19
20
22
26
27
30
31
11
Station
No.
1
3
1
3
1
3
5
1
3
4
2
1
3
1
3
5
3
1
3
5
3
5
3
5
3
5
3
1
3
1
3
TSP
yg/m
Aug.
107
52
149
46
103
41
94
101
47
86
63
74
30
126
54
44
37
67
38
85
45
109
57
90
54
64
30
89
38
Sept.
44
38
SS
yg/m
5.8
4.4
12.2
11.8
9.9
5.8
13.5
10.5
6.1
12.2
8.1
5.2
3.5
7.4
5.3
12.8
12.1
13.1
13.0
14.6
8.7
17.8
6.7
12.3
4.4
14.8
3.0
3.7
5.5
10.1
11.2
-------
APPENDIX I
RAW METALS DATA
-------
Table 1-1
METALS DATA
NATIONAL ZINC C014PAHX AIR QUALITY MONITORING SURVEY
Bcu?tlesville3 Oklahoma
Analyses
Performed
Sn
As
Sb
Zn
Pb
Cd
3
Fe
Mn
V
Cu
Ni
Cr
Y
Mo
Se
W
Filter #
Residue Wt
Sn
As
Sb
Zn
Pb
Cd
B
Fe
Mn
V
Cu
Ag
Ni
Cr
Y
rio
Se
W
Fi 1 ter #
Residue l-lt
2
<3a
<65
<59
350
80
<6
<12
690
<21
<17
9
<75
<28
2
<74
<6
-------
Table I~l (Continued)
METALS DATA
NATIONAL ZINC CCXIPANX AIR QUALITY MONITORING SURVEJf
Bartlesville 3 Oklahoma
September 1977
Analyses
Performed
Sn
As
Sb
Zn
Pb
Cd
B
Fe
Mn
V
Cu
Ag
Ni
Cr
Y
Mo
Se
W
Filter #
Residue V/t.
Sn
As
Sb
Zn
Pb
Cd
B
Fe
Mn
V
Cu
Ag
Mi
Cr
Y
Mo
Se
V!
Filter #
Residue Wt
2
<8
<65
<59
42
<69
<6
<12
40
<21
<17
<7
<13
<75
<28
2
<74
<6
<1^0
31^
<8
<65
<59
720
140
<6
<12
720
<21
<1 7
32
<13
<75
<28
2
<74
<6
<110
23
13,600
3
<8
<65
<59
400
130
<6
<12
640
<21
< 17
16
<13
<75
<28
3
<74
<6
<110
27
16,100
4
yg/filter
Station No.
<8
<65
<59
380
76
<6
<12
330
<21
<17
33
<13
<75
<28
4
<74
<6
-------
Table 1-2
14ETALS DATA (SOIL SAMPLES)
NATIONAL ZINC COMPANY AIR QUALITY MOSITOBING SURVEY
j Oklahoma
Station Number - Sequence No.
Analyses
Performed
Sn
As
Sb
Zn 13
Pb 1
Cd
B
Hg
Fe 54
Mn
V
Cu
Ag
N1
Cr
Y
Mo
Se
W
U
1-01
13
130
47
,900
,300
137
74
-
,100
820
108
330
10
26
66
6
53
<220
<80
<71
1-02
17
150
65
33,000
2,100
350
<7
-
57,800
930
83
640
17
40
64
4
100
620
94
<71
3-01
16
120
48
970
150
7
43
-
93,900
830
130
37
<2
64
50
9
<50
<220
<80
<71
3-02
<10b
34
14
340
58
<1
76
-
32,100
380
65
18
<2
<8
41
1
<50
<220
<80
<71
3-03
vg/g
<10
42
17
570
77
<1
140
-
46,400
650
83
15
12
8
42
<.2
<50
<:2o
<80
<71
5-01
17
190
76
38,300
1,800
500
24
-
40,600
580
103
640
16
70
49
4
70
<220
102
<71
5-02
10
98
<10
5,000
1,400
420
51
-
29.000
500
73
410
4
9
41
2
<50
<220
<80
<71
6-01
<10
<30
<10
260
62
<1
140
-
10,800
420
74
19
<2
<8
67
6
<50
<220
<80
<71
MQDLfl
10
30
10
2
8
1
7
-
2
3.
1
1
2
8
3
0.2
50
220
80
71
a liininnan fy.
-------
|