v>EPA
United States
Environmental Protection
Agency
Environmental Sciences Research EPA 600 2 79 116
Laboratory June 1979
Research Triangle Park NC 2771 1
Research and Development
Evaluation of
Stationary Source
Particulate
Measurement
Methods
Volume V.
Secondary Lead
Smelters
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR) .
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the ENVIRONMENTAL PROTECTION TECH-
NOLOGY series. This series describes research performed to develop and dem-
onstrate instrumentation, equipment, and methodology to repair or prevent en-
vironmental degradation from point and non-point sources of pollution. This work
provides the new or improved technology required for the control and treatment
of pollution sources to meet environmental quality standards.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/2-79-116
June 1979
EVALUATION OF STATIONARY SOURCE PARTICULATE
MEASUREMENT METHODS
Volume V. Secondary Lead Smelters
by
J. E. Howes, Jr., W. M. Henry, and R. N. Pesut
Battelle, Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201
Contract No. 68-02-0609
Project Officer
Kenneth T. Knapp
Emissions Measurement and Characterization Division
Environmental Sciences Research Laboratory
Research Triangle Park, N.C. 27711
ENVIRONMENTAL SCIENCES RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
RESEARCH TRIANGLE PARK, N.C. 27711
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DISCLAIMER
This report has been reviewed by the Environmental Sciences Research
Laboratory, U. S. Environmental Protection Agency, and approved for publica-
tion. Approval does not signify that the contents necessarily reflect the
views and policies of the U. S. Environmental Protection Agency, nor does
mention of trade names or commercial products constitute endorsement or
recommendation for use.
n
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ABSTRACT
As part of an overall program to evaluate the EPA Method 5
procedure for measurement of particulate emissions as detailed in
the Federal Register, Vol 36, No. 247, December 23, 1971, an experi-
mental study was made of its specific applicability to secondary lead
plant emissions. The study was carried out with two Method 5 sampling
train systems operated simultaneously at a single point in the stack
emission stream. A series of six statistically designed tests was
conducted over a 5-day period to obtain data on the reliability of
Method 5, the sensitivity of the method to variation of such key
parameters as sampling system temperature, filter media, and particulate
loading and to characterize the chemical composition of the emissions.
Comprehensive chemical analyses were made of particulates
collected in the sampling system and from the baghouse control to ascertain
if the sampling mode affected the composition of the particulate emissions.
Essentially 100 percent of the particulates were accounted for by the
chemical analyses. Compositional analysis of the gaseous species present
in the stack gas stream also were performed. The results of the
particulate and gas analyses do not indicate any chemical interactions with
the sampling system components of the Method 5 train.
ill
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CONTENTS
Abstract ill
Figures/Tables vi
1. Introduction 1
2. Conclusions 3
3. Recommendations 5
4. Objectives 6
5. Experimental Work and Results 7
6. Discussion 25
References 26
Appendices
A. EPA Method 5 Federal Register, December 23, 1971 27
B. Stack Gas and Sampling Data 01
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FIGURES
Number Page
1 Gas Flow Diagram-Blast Furnace Secondary Lead Smelter. . . 8
2 Lead Blast Furnace . . \ " . . . , 9
3 Velocity Pressure and Temperature Profile of Stack,. ... ,11
4 Temperature Measurement Points .... 14
TABLES
1 Emission Source Characteristics 12
2 Randomized Test Pattern for Study of Effects of System
Temperature - Filter Media - Secondary Lead Plant Data . . 16
3 Particulate Collection'Data - Secondary Lead Plant .... 18
4 Analysis of Variance - Filter Media/Sampling System
Temperature Experiments - Secondary Lead Plant
19
5 Analysis of Particulate Emissions from Secondary Lead
Smelter(a) 20
6 Chemical Analysis of Particulate Emissions from Secondary
"' Lead Smelting Process 21
7 Cation/Anion Balance in Secondary Lead Plant Emission
Samples 22
8 Gas Chromatographic and Mass Spectrometric Analysis of
Gaseous Emissions from Secondary Lead Smelter 24
B-l Stack Gas Data - Secondary Lead Smelter B-l
B-2 Sampling Data - Secondary Lead Plant B-2
VI
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1. INTRODUCTION
The Clean Air Act as amended in 1970 provides the impetus
for programs to improve the air quality in the U.S. through research to
broaden the understanding of the effects of air pollutants, research
and development of techniques to control emissions, and the enactment
of air quality "regulations to protect the public welfare. Pursuant to
Section 111 of the Act, the Environmental Protection'Agency (EPA) on
December 23, 1971, promulgated Standards of Performance for New Stationary
Sources (amended) for fossil-fuel fired steam generators, incinerators,
Portland cement plants, and nitric and sulfuric acid plants^ '. On
March 8, 1974, similar performance standards were issued for asphalt
concrete plants, petroleum refineries, storage vessels for petroleum
liquids, secondary lead smelters, secondary brass and bronze ingot ^>
production plants, iron and steel plants, and sewage treatment plants
All new and modified sources in the preceding categories are required to
demonstrate compliance with the standards of performance.
The performance standards are intended to reflect "the degree
of emission limitation achievable through the application of the best
system of emission reduction which (taking into account the cost of
achieving such reduction) the Administrator determines has been adequately
demonstrated"^ J.
Compliance with required performance is determined by testing
procedures specified with the standards. The use of the procedure called
"Method 5 Determination of Particulate Emissions from Stationary Sources"^
is specified in all instances where particulate mass emission measurements
must be made. A copy of the Method as promulgated is given in Appendix A.
The Method 5 procedure consists of isokinetic extraction of a sample from
the emission stream with a heated probe and collection of the particulates
on a heated filter. With the recent exception of fossil fuel-fired
power plants(5), the same sampling system operating parameters have been
adopted for all stationary sources.
The source categories subject to Method 5 particulate measurements
include diverse processes which encompass a wide range of the following
emission characteristics; moisture content, gas temperature, gas composition,
particulate concentration and composition, and flow dynamics. Interaction
of these emission properties with the Method 5 sampling technique can
produce significant variations in the results .of particulate emission
measurements. The following are examples of some of the reactions which
may affect particulate measurements.
(1) S03 or H2S04 in emissions can condense to form sulfates
which increase the mass of collected "particulates".
The S03-H2S04 dew point is dependent on S03 concentration
and moisture content of the emissions.
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(2) The filter particulate catch may present a surface for
reactions with gaseous emission components such as SOX
and NOX. Reactivity would be dependent on particulate
loading and composition and on gas composition of the
emissions as well as interactions with the filter media.
(3) Changes in gas temperature in the sampling system may
alter the apparent particulate concentration through
condensation, or volatilization.
Such interactions with the sampling process must be recognized
and controlled if Method 5 is expected to yield reliable particulate
measurements for individual source categories.
The work presented in this report was performed as a part of
an EPA program to study the applicability of the Method 5 procedure to
measurement of particulate emissions from a variety of stationary sources.
Specifically, this work addresses the question of whether Method 5 provides
an accurate, reliable measurement of particulate emissions from secondary
lead smelters. Volumes I, II, and IV in this series cover similar studies
of cement plants, oil-fired steam generators, and basic oxygen steel making
furnaces, respectively. Volume III is on gas temperature control during
Method 5 sampling.
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2. CONCLUSIONS
The following conclusions regarding the methodology for deter-
mining particulate emissions from secondary lead plants may be drawn from
this study.
SAMPLING SYSTEM TEMPERATURE
Operation of the Method 5 sampling system with probe outlet and
filter box temperatures of 93°C (200°F) and 149°C (300°F) yielded equivalent
mass loading results based on statistical differences in the particulates
collected at the two different sampling system temperatures. Therefore, it
is concluded that operation of the sampling system at the minimum tempera-
tures recommended in Method 5 produces representative mass emission measure-
ments and that variations from 93 to 149°C do not affect the results.
FILTER MEDIA
Sampling with MSA 1106 BH glass filter as specified by Method 5
and the ADL quartz-type filter yielded no statistically significant differ-
ences either in respect to particulate mass loading or in the compositions
of the collected emissions.
CHEMICAL INTERACTIONS
The Method 5 sampling train system did not induce compositional
changes in the particulate collections. Samples taken from the probe and
filter sections of the sampling train were compared compositionally with
grab samples and with samples taken from the stack emission control
baghouse collector and were found to be similar in chemical compositions.
PRECISION
The precision (repeatability) of particulate mass emissions by
Method 5 on the basis of paired sampling tests was found to be about 1.5
percent when the two systems were operated simultaneously at a single fixed
point in the stack. This precision was attained over a 5-day sampling
period despite considerable variation in the particulate emission loadings.
COLLECTION EFFICIENCY
Examination of the impinger collections revealed only a very small
fraction (0.4 percent of the Pb — which constituted the probe and filter
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section loadings was transported through the filter. Approximately 26
percent of the total As passed through the filter and was collected in
the impingers.
PARTICULATE EMISSION COMPOSITIONS
The major components of the particulate emissions was found to
be lead, probably as PbS04. and/or PbCl2 which constituted 80 to 85 percent
of the emissions. .Other ..heavy, metals -were Sn, . Cd,, Zn,. Sb,,.. and As, again
probably present as chlorides and/or sulfates and in quantities of about
4, 1, 1, 0.5, and 0.5 percent of the particulate emissions. Organics, as
indicated by the carbon contents of the emissions and by the extracts from
the impinger solutions, constitute less than one percent by weight of the
emissions and these are comprised mostly of relatively low molecular weight
aliphatic compounds, carbonyls, esters, and diacids.
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3. RECOMMENDATIONS
The results of this study indicate the EPA Method 5 is a satis-
factory procedure for measuring particulate emissions from secondary lead
plants and that no modifications are required to obtain representative
and reproducible mass emission measurements.
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4. OBJECTIVES
The objective of the overall EPA program is the evaluation
of the applicability and reliability of Method 5 (conducted as specified
in the Federal Register, December 23, 1971) for the determination of
particulate mass emissions from'stationary sources for which performance
standards'have been promulgated. The portion of the overall program
covered by this report is aimed at evaluation of Method 5 performance
when the procedure is applied to secondary lead smelters. The study
sought to identify any characteristics of the sampling method or unique
properties of process emissions which would adversely effect particulate
measurements and, if possible, recommend appropriate corrective measures
in sampling methodology.
A secondary objective in this program is the characterization
of the emission species particularly in regard to heavy metal concentrations,
6
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5. EXPERIMENTAL WORK AND RESULTS
EXPERIMENTAL APPROACH
An experimental plan was drawn up to test and evaluate the
sensitivity of Method 5 to key sampling variables,' including temperature,
filter media, loading and to determine the specific chemical composition
of the particulate emissions. The approach used was similar to that
employed previously^6) and consisted of concurrent sampling at a single
point in the stack with two Method 5 sampling train systems operated
under the chosen conditions of study. Experiments were carried out in
a statistically designed test pattern to permit the significance of
observed differences to be assessed. The Method 5 sampling procedure
as detailed in the Federal Register was strictly adhered to in the
experimental tests except for stack profiling and, of course, the use
of the planned variations designed to test the sensitivity of the
method and to reveal potential problem areas.
Filter and probe collections were analyzed gravimetrically for
mass loadings and in detail chemically to detect changes, if any, induced
by the collection process. The sampling catches were compared compositionally
with grab samples and with collections from the baghouse.
Descriptions of the secondary lead emission source, experimental
testing, and test results are detailed in the following sections.
PROCESS AND SAMPLING SITE DESCRIPTIONS.
Secondary Lead Smelting Process
This experimental study was performed at a secondary lead plant
which uses a blast furnace for the smelting and refining process. The
furnace is fed nearly continuously with coke, cast iron scrap, batteries,
limestone, a silacebus slag;, drosses and other lead-containing residues.
About 10 charges are fed each 8-hour shift with a 7100 pound charge yielding
about 4800 pounds of lead. Figure 1 shows the gas flow through the plant.
Air is blown into the furnace to burn the coke in. the feed. The heat of
combustion melts the lead and the coke reduces the lead oxides. The off-gas
from the furnace is combusted in an afterburner to oxidize any odiferous
compounds and to incinerate oily and sticky materials which'may blind the
fabric filters. The off-gas is cooled in three air-cooled cyclones in
series which also remove most of the dust. The remaining dust is removed
in a baghouse. The 'gas is then exhausted through a 156-ft high stack.
A sketch of the blast furnace is shown in Figure 2. The furnace,
rated at about 77 tons/day, is loaded from the top and tapped for lead
recovery at the bottom of -the hearth. Slag, which normally floats on the
surface of the lead, also is drawn off near the bottom of the furnace. The
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Charge
i—i.
1^
Air
After-
burner
300 F
Dust
Air-cooled cyclones-
Baghouse
--Sample
r- 11 / / r
Fan Stack
Blast
furnace
Sla:g
Lead
Figure 1. Gas- flow diagram blast furnace secondary lead smelter.
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Water jacket-
Flue
Shaft
****'*.;^£i£
D
/f VBustle pipe
// Lead well
\g / ,-Draw pot
Figure 2. Lead blast furnace.
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main gas stream leaving the blast furnace is heated to about 650 C (1200 F)
in an afterburner with a natural gas flame in which most of the hydro-
carbons and some CO in the exhaust gas are burned. The gas then passes .
through three forced air and water-cooled cyclones which also remove some
particulates. The gas stream is cooled from about 650 C to about 150 C
in the cyclones by heat transfer and by dilution with leakage air. Each
volume of gas from the blast furnace is diluted with about 11 volumes of
air in the exhaust system.
The sampling experiments were conducted at roof level (about 34
ft above ground) on the 46.9m (154-ft) stack after the gas from the blast
furnace had passed through a baghouse. The diameter of the stack was
about 1.22 m (4 ft) with two 7.62 cm (3-inch) diameter portholes, set
at 90 degrees from each other and about 4 ft above roof level, providing
access for the sampling probes. The velocity, pressure drop and temperature
profiles of the stack are shown in Figure 3. The general emission
characteristics of blast furnace stack emissions are given on Table 1.
With the high volume of air dilution into the stack the gas composition
is essentially that of ambient air except for the C02 and small amounts
of S02 and CO. Particulate content varied from about 134 to 378 rag/Mm-5
during the test runs carried out over a 5 day period. During the 5 day
sampling period the plant operators were having considerable difficulty
with the emission control system, and the particulate emissions varied
considerably, being well above the highest level of 6.4 mg/Nm^ obtained
in 1972 at this plant by Battelle personnel. !
Sampling Equipment
Particulate sampling was performed with two identical Method
5 sampling trains operated concurrently. A single Type S pitot tube
positioned equidistance between the sampling nozzles was used to measure
velocity pressure of the stack gas. With the exceptions listed below,
the trains consisted of components assembled as described in the Federal
Register, Sections 2 and 3 of the Method 5 procedure.
Temperature Measurements
The glass connectors from the probe outlet to the filter and
the filter outlet to the first impinger were modified to permit additional
measurements of gas sample temperature. The probe outlet-to-filterholder
connector contained a thin-wall thermocouple well which extends about
5.1 cm (2 inches) into the outlet end of the probe. The filterholder-to-
impinger connector was fitted with a bi-metal dial thermometer. The tip
of the thermometer was positioned about 1.3 cm (0.5 inch) from the filter-
holder frit.
Filter Materials
Mine Safety Appliance (MSA) 1106 BH glass fiber filler materials
and Arthur D. Little experimental quartz filters were used throughout the
test series.
10
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Sampling Nozzle locations
1.88 1.98 1.73
+ +
68 68 6
0.94 1.30 1.32 1.24
+
67 68 68 67
Measurement Points,
cm from sampling port
4.0
12.8
23.6
39.4
82.6
98.3
109.1
117.9
PORT 1
Upper numbers are
Velocity pressure In
CM HO.
Lpwer numbers are
gas temperature In *C.
117.9 CM
Stack Diameter
Figure 3. Velocity pressure and temperature profile of stack.
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TABLE 1. EMISSION SOURCE CHARACTERISTICS
Flue Gas Conditions
Temperature 61-74 C (142-165F)
Volumetric flow' 49277 Nm3/hr (29,000 DSCFM)
Average AP 1.47 cm (.58 in) H20
Static pressure 0.76 cm (0.3 in) H20, negative
Flue and Port Dimensions
Flue size - 1.22m (4 ft) diameter
Port diameter - 7.62cm (3 in)
Composition of Stack Emissions
3
Particuiates ^216 m&/Nm (a'v&. )
N 78.5%
2
0: 18.5%
C02 2.3%
CO 65 ppm
SOx 30° PP*
Moisture ^3 percent
12
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Impingers
In some runs, the first impinger was loaded with 6N HN03
and the second with IN NaOH to collect any volatile metals which might
pass through the box filter.
Gas analyses for C02 and 02 were performed with Fyrite equipment.
In addition grab samples were taken with an evacuated glass gas sampling
bulbs for mass spectrometric analysis of gases and low molecular weight
organic species.
SAMPLE COLLECTION AND ANALYSIS PROCEDURES
Particulate Sampling
In all tests, particulate sampling was performed concurrently
with two identical sampling train units (designated A and B) each with
a separate operator. Sampling system equipment and operating conditions
used in the tests were varied in accordance with a statistically designed
experimental pattern.
All sampling was performed at a fixed-point at the center of
the duct in an area of nearly uniform velocity. Sampling probes of the
two systems were inserted into the duct through two ports, situated
in the stack at a 90-degree angle to each other, so that the pitot tube
attached to one of the probes was positioned equidistance between the
sampling nozzles. The separation between the pitot tube and each nozzle
was about 2.5 cm (1 inch).
At the start of each test day, the laboratory calibration of
the gas metering components of both sampling systems was checked by
setting the orifice manometer (AH) to the meter box calibration factor (AH@)
and measuring the flow rate through the dry gas meter over a 5-minute period.
A flow rate of 0.021 m^/min (0.75 cfm) confirmed that the gas metering
system remained in calibration.
The preparation of the particulate collection trains for all
tests was performed as specified in Paragraph A.1.2 of Method 5.
In performance of the tests, sampling trains were operated as
described in Paragraph 4.1.3 of Method 5 with the exception that readings
of AP, AH, stack temperature and sampling system temperatures were recorded
at 10-minute intervals. The velocity head (AP) for both systems was deter-
mined from one pitot tube and nomographs were used to obtain the proper
sampling rate (AH). Temperature measurements were obtained at the points
shown in Figure 4.
The sampling period for each test was 150 minutes and the total
dry gas sample volumes at isokinetic sampling rates ranged from about 3 to
5.5Nm3.
13
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Probe outlet.
Probe
Mid-point
impir.ger
Figure 4. Temperature measurement points,
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After completion of the tests, the trains were again leak
checked, sealed to prevent contamination, and transferred to the sample
recovery area.
Sample Recovery and Analysis
Filters were removed from holders, sealed in Petri dishes
and immediately placed in a desiccator. The probe and nozzle were
disassembled with washed separately. First, the probe was first rinsed
with acetone without brushing, then rinsed with acetone while slowly
inserting' and removing a Nylon brush in a rotating fashion. The acetone
wash and brushing were continued until visual Inspection indicated that
all particulates were removed. The brush was thoroughly flushed with
acetone prior to removal from the probe. The probe wash (usually about
100 to 150 ml) was collected in an Erlenmeyer flask sealed onto the probe
outlet ball joint. Particulates were recovered from the nozzle and the
inlet half of the filter holder by alternately brushing and rinsing with
acetone. The wash solutions from all three components (probe, nozzle, and
filterholder) were combined for analysis.
At least one 200 ml acetone blank was obtained each day from the
wash bottle dispenser. All acetone wash solutions and blanks were stored
in glass bottles with Teflon-lined caps for transfer to the laboratory
for analysis.
The filters and particulate catch were desiccated at least 24
hours (usually longer) prior to weighing. Acetone wash solutions were
evaporated to dryness in a reverse airflow, clean hood and the residues
were desiccated to a constant weight (usually 24 to 48 hours).- Residues
and filters were weighed to the nearest 0.1 mg.
All calculations were performed as described in Section 6 of ,
Method 5.
TEST DESCRIPTIONS AND RESULTS
Variables selected for study were the sampling system temperature,
the filter media, and the particulate loading. These, together with
. detailed chemical analyses of the particulate catches and gaseous emission
to indicate potential chemical interactions (and possible formation of
pseudo particulates) should indicate the reliability and sensitivity of
Method 5 to the measurement of emissions from secondary lead..plant operations.
The randomized test pattern for the study of the effects of
the system variables temperature and filter media is shown in Table 2.
An additional test pair was run wherein the filter in one system was ,
changed midway through the 4-hour test period to assess the- effect of,
particulate loading.
The experimental tests were carried out over a 5-day period when
the plant was operating at full capacity. Some difficulty was being
encountered with the emission control equipment during this period which
resulted in overall higher and more erratic stack emissions than normally
anticipated.
15
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TABLE 2. RANDOMIZED TEST PATTERN FOR STUDY OF EFFECTS OF SYSTEM
TEMPERATURE - FILTER MEDIA - SECONDARY LEAD PLANT DATA
Test
Replication Block Number
1 1 l(b)
1 2 2(b)
2 1 3(c)
2 2 4(c)
3 1 5(d)
3 2 - 6(d)
System A
Temperature, C
149
93
149
149
93
149
Media
ADL
ADL
ADL
MSA
ADL
MSA
System B
Temperature, C
149
93
93
93
149
93
Media
MSA
MSA
MSA
ADL
ADL
MSA
(a) Both System A and System B are Method 5 trains.
(b) Tests 1 and 2 confound temperature with Blocks.
(c) Tests 3 and 4 confound temperature/filter with Blocks.
(d) Tests 5 and 6 confound filter with Blocks.
16
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Particulate Measurements
The particulate collection data obtained in the seven paired
runs are given in Table 3. Sampling and stack gas data for the runs are
presented in the Appendix B.
The analysis of variance of the six runs (1 through 6) to study
filter, and temperature effects is shown in Table 4. The conclusions drawn
from the statistical analysis are that neither variation of the filter media
(MSA and ADL) nor the sampling system temperature (at 93 and 149C) had a
statistically significance on the particulate mass results. Analysis of
the variation in the six test pairs shows good repeatability with an
overall coefficient of variation of 1.48 percent.
In Run 7, the System B box filter was changed midway through
the four hour sampling period. System A filter was unchanged. The
good agreement in the pair of results indicates that there is not a
significant effect of mass loading or of reaction of the stack gases
with the particulates catch on the filter.
Compositional Analyses
Probe and Filter Residues. Selected particulate catches from
the probe, filter, and impinger segments of the sampling train, together
with a bulk sample and a sample taken from the baghouse, were analyzed in
detail to ascertain the compositions of the emissions.
Metallic elements were analyzed semiquantitatively by optical
emission spectrography and the results obtained are shown in Table 5.
These data indicate no great differences among the probe, filter catch,
baghouse, or grab sample compositions. Selected additional probe and filter
catch samples together with the grab sample and a baghouse sample were
analyzed quantitatively and the results obtained are shown in Table 6.
Again no major differences are observed among these samples. From
averages of the quantitative data from Table 6 the cation, anion, and C
values total 96.2 percent with presumably additional oxygen in the form
of metallic oxides making up the difference between 96.2 and 100 percent.
Cation-anion ratio given in Table 7 show an imbalance of 0.171 (0.913 -
0.742 = 0.171) which if attributed to oxygen gives a content of 1.4 percent.
With the value for the additional undetermined oxygen and the Table 5
average values for cations, anions, and carbon compositional balance of
97.6 percent is obtained. This value, within analytical error, is
sufficiently close to 100 percent to indicate that no other elements are
present in more than trace amounts.
Impinger Residues. Total impinger catches (extracted organics
plus aqueous residue) averaged approximately 7 percent of the front half
particulate catch. The impinger catches collected in 6N HN03 and IN NaOH
were examined analytically to determine if potentially volatile metallic
elements such as Pb and As, were carried through the filter. Organic
extracts were analyzed gravimetrically and by infrared spectrometry.
17
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TABLE 3. PARTICULATE COLLECTION DATA - SECONDARY LEAD PLANT
Temperature C
Run No
1A
B
2A
B
3A
B
4A
B
5A
B
6A
B
7A , .
•B(a)
Filter
142
149
94
97
92
149
94
149
148
96
92
151
' 123
118
Probe Out
148
148
95
93
94
148
94
148
148
99
92
148
122
120
Filter
ADL
MSA
ADL
MSA
ADL
MSA
MSA
ADL
MSA
MSA
ADL
ADL
' ADL
ADL
Particulate Catch, mg
. Filter
766.1
732.9
305.6
390.9
488.7
459.9
377.8
354.3
414.0
397.8
949.6
972.1
691.1
693.6
Probe
344.5
298.8
160.8
138.8
125.3
135.6
90.2
99.3
177.5
178.9
325.9
232.0
165.1
140.3
Total 1
1110.6
1031.7
556.4
529.7
614.0
595.5
468.0
453.6
591.5
557.7
1275.5
1204.1
856.2
833.9
Particulate .
,oadlng, nig /Mm
209.0
203.8
159.3
158.9
180.5
182.5
133.6
134.4
170.0
166.2
377.8
369.8
290.6
293.9
(a) Filter changed midway through 4 hour test.
18
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TABLE 4.- ANALYSIS OF VARIANCE T FILTER MED LA/SAMPLING SYSTEM
TEMPERATURE EXPERIMENTS - SECONDARY LEAD PLANT
Source of Degrees of Sum of
Variation Freedom Squares
Filter Media (F)
Temperature (T)
F x T
Reps
Blocks/Reps
Remainder
Total
1
1
1
2
3
3
11
2.4200
0,2450
6.1250
28,291.3067
46,806.0300
46.3500
75,152.4767
Mean
Square
2.4200
0.2450
6.1250
14,145.6533
15,602.0100
15.4500
6832.0433
F(a)
Ratio Conclusion
0.1566 Not Significant
0.0159 Not Significant
0.3964 Not Significant
—
—
__
—
(a) For an F-ratio with 1 to 3 degrees of freedom, any calculated value of F exceeding
5.54 Is significant at the 90 percent confidence level, exceeding 10.13 Is
significant at the 95 percent confidence level, and exceeding 34.12 is significant
at the 99 percent confidence.
19
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TABLE 5 . ANALYSIS OF PARTICULATE EMISSIONS FROM SECONDARY LEAD SMELTER*"*
Height Percent o£ Elenent In Sample
Sample fb Sn Zn A. Na K Si Fe Sb Cu Cd Mg Mn Bl Cf Al V HI C* B» B Ho Ag
Filter ~ " '
(3A) 10-60 1-3 0.3 0.3 2-1, I 0.2 0.1 0.2 0.03 0.5-1 =60.001 0.003 0.003 «O.OOl 0.003 *0.001 SO.OOI 0.03 «.001 «.00l *0.00l *O.OOOS
Filter
(38) 40-60 1-3 0.3 0.3 J-4 1 0.2 0.1 0.2 0.03 0.5-1 «0.001 0.001 0.003 «0.001 0.003 *0.001 S0.001 0.03 1Q.001 *0.001 ^0.001 *O.OOOS
Prube
(3A) 40-60 1-30.3 0.2 2-4 1 0.5 0.3 0.2 0.03 0.5-1 0.01 0.005 0.003 O.OOS 0.2 *0.001 0.003 0.03 S0.001 performed by optical emission «pscera.copy
-------
TABLE 6. CHEMICAL ANALYSIS OF PARTICIPATE EMISSIONS FROM
SECONDARY LEAD SMELTING PROCESS
Weight Percent In Sample
Pb Sn As Cd Sb Zn S0° Cl" HC03" C N P pH
Method 5 Filter (LA) 59.5 2.09 0.20 0.62 0.21 0.52 7.53 19.3 ND .15 — 0.05 4.4
Method 5 Filter (2B) 60.1 2.11 0.24 0.64 0.31 0.53 4.61 23.4 1.0 -- -- 0.07 5.4
Method 5 Probe
Residue (1A) 55.1 2.07 0.18 0.75 0.22 0.59 6.50 20.7 0.22 1.7 — 0.06 4.8
Method 5 Probe
Residue (2B) 55.7 2.27 0.20 0.55 0.22 0.70 6.09 21;6 0.43 — -- 0*06 5.2
Crab Sample of
Stack emissions 60.5 2.05 0.22 0.64 0.27 0;47 6;92 .34 .21 0.07 4.7
Baghbuse Catch 61.2 1.97 0.22 0;66 0.25 0.46 5.94 22.4 0.44 -- -- 0.06 5.1
21
-------
TABLE 7. CATION/ANION BALANCE IN SECONDARY LEAD PLANT EMISSION SAMPLES
Cation
Pb=
Sn=
Zn=
=
Cd
Sb=
As=
Na~
K~
Si=
Ca=
Fe=
Al =
Totals
Percent
58.7
2.1
0.55
0.65
0.25
0.21
3.0
1.0
0.2
0.05
0.2
0.2
67.11
Equivalent Anion Percent Equivalent
0.567 S0.= 6.20 0.129
A
0.071 Cl~ -21.5 0.606
0.017 HCOl 0.4 0.007
j
0.012 Totals 28.1 0.742
0.006 Total cation = 0.913
0.008 Total anions = 0.742
0.13 Difference = 0.171: calculated as
0- = 1.4 percent
0.026 L
0.040
0.003
0.011
0.022
0.913
99
-------
Organic constituents were determined from chloroform-ether and
acetone extracts from selected impinger washes. By weight these constituted
about 9 to 15 percent, respectively, of the total residues in the impinger
washes. Infrared spectrometric analysis showed the chloroform-ether
extracts to be principally a complex mixture of carbonyl components with
relatively short chains (aliphatics - high Ctt^), a small amount of aromatic
structure, some ether structure, and a small amount of hydroxyl. The
acetone extract primarily consisted of sulfonic acids.
Inorganic analysis of the HNC>3 and NaOH impinger solutions were
made by optical emission spectrography. The results show that about
0.4 of the total lead was collected in the impingers. However, about 26
percent of the total arsenic passed through the filter and was collected
in the impinger.
Gaseous Components
Grab samples were taken of the stack gases by use of evacuated
sampling bulbs and these were analyzed by gas chromatography and gas mass
spectrometry. The results obtained are given in Table 8.
Except for the hydrocarbons found in Sample 1, the following were
not detected and were less than 2 ppm in both samples: C2H2, C2H4, 02^,
C2H8, C4H10, C5H1Q, C6H14, CH3OH, C2H5OH, COS, CS2, H2S and HC1. As stated
previously, the principal component of the highly diluted stack gas in air.
An S02 level of 200 to 400 ppm was found plus about 65 ppm of CO. No HC1
nor free chorine were detected.
23
-------
TABLE 8. GAS CHROMATOGRAPHIC AND MASS SPECTROMETRIC ANALYSIS OF
GASEOUS EMISSIONS FROM SECONDARY LEAD SMELTER
Sample ; Volume percent
007-07 N2 A H2 S02 C6HA C4H1Q C^ CO CH
1 2.3 18.1 78.5 0.94 0.06 0.04 0.02 0.04 0.02 62 4
2 2.4 18.8 78.5 0.94 0.06 0.02 <0.01 <0.0l 0.01 67 4
-------
6. DISCUSSION
The parameters selected for study - sampling system temperature,
filter media, and filter loading — were those deemed most likely to
have an effect in the application of Method 5 to the determination of
particulate mass emissions from secondary lead plants. However, results
of this study indicate that these factors within the limits investigated
to not ^significantly-effect-the mass emission results- obtained with Method
5. Unfortunately, during the sampling period, emissions from the secondary
lead plant studied were higher than normal. Therefore the study results
must be qualified somewhat by this fact. For example, at a lower particulate
loading, the effects of the reaction of S02 or 803 with the filter medium
could result in a detectable error.
The chemical analysis provide important data which corraborate
the findings of the particulate mass measurements. The probe and filter
catches have essentially the same composition as a grab sample and a sample
of the baghouse catch which also indicates that the particulates collected
by Method 5 are representative of the emission source and that no alterations
occur during sampling.
25
-------
7. REFERENCES
r-
1. Federal Register, Volume 26, No. 247, pgs 24876-24895, Thursday,
December 23, 1971.
2. Federal Register, Volume 30, No. 47, pgs 9308-9323, Friday, March 8,
1974. . . •
3. Federal Register, Volume 30, No. 177, pg 32852, Wednesday, September
11, 1974.
4. Reference 1, pgs 24888-24890.
5. Reference 3, page 32856.
6. Evaluation of Stationary Source Particulate Measurement Methods —
Volume 1, Portland Cement Plants, EPA-650/2-75-051a, June 1975.
7. Sittig, M., Environmental Sources and Emissions Handbook, Noyes Data
Corp., Park Ridge, New Jersey, pp 331-333 (1975).
26
-------
APPENDIX A
EPA METHOD 5
Federal Register, December 23, 1971
27
-------
AUL£S AND ftEGULATtONS
1.1.4 niter HoWor—Pyrei " glata with
haarflnc ayateca capable of maintaining mini-
mum tamper*, ture otf 325* r.
4,1,5 impin(rer» / GoodCMcr—Pour Implu-
r*r* eoan«ow»d in aerie* with glaaa bnJl joint
AttLnta. The Hist, third, tod fourth knplc-
(•n are otf the GrwaburB-amlUs design,
modified by replacing the np with a H-lccU
*E>g!e.-s tube ert*ndlug to one-half 1"k. The second Iro-
ptnger U of the Qreenburg-Smith design
With Uia-Btandard Up. A ooDHaiaer ma? be
«ed in place of the impiagert provided mai
taw raotflture content of the alack gaa oan
a*iU be determined.
2.14 Metering ryaMem—Vacuum gauge.
leak-free pump, t&ennometcra capable oj
meewtulog temperature to wrthln 6* P., dry
KM meter wtth 2-fc accuracy, and reJated
equipment, or equivalent. 05 required to
maintain AH iBoklneUc a-ampLing r*t« and to
determine aaniple volume.
•2.1.7 B&rotneur—To meagre atmospheric
pressure to ±0.1 Inohee Bg.
2.3 Sample recovery.
22 1 Probe bruah—At leart as long a*
probe.
322 Glass vuh bottles—TV
2.2.3 QIaee tample ator&£o ci.mainera.
2.2.4 Graduated cylinder—3SO ml.
2.3 Analysis.
33.1 Class weighlDg dl&hea.
2.3.2 Deciccator.
2.3.3 AnuJyticaJ beJaflce—Tto mraiiirn to
±0.1 mg.
3.3.4 Trip bflhvnoe—300 g. o&paolty. to
znaafiure to ±0.06g.
3. Reagents.
a.i 6*mp;tiig
3.1.1 Fillers—Glau fiber. USA 3100 BH'.
or equivalent, numbered for IdontLfloaUon
and preu-e'.ptied.
3.1.2 Silica pel — IirtloaiLne typ«. 0-lf
meih. dried &i 175* c. <3W P.) fcr 2 hours
3.1.3 WB.U.T
3.1.4 Cru^bod Lee.
8.2 Sample recovery.
3.2.1 Act-lone-—Keu^eni gnwle.
3.3 AiuOyslfi
3.3 1 Wutor.
IMP1HCEP TRAir. OPTIOHAL. BAY BE REPLACED
AH EQUIVALENT MfiOENSL*
6—DITCRMIWATION or
Lanadtoixs PkoM OTATIOHABT
1. Prtnrlp/e and opp/tcobiliry.
11 Principle. P&rucui«t« m*t with
ajiarp. t«p«rtd IrtMlin^ edge
3 1.2 Probe— Pyrei' pl«ao with a heating
tyviejn capable of malntAlamg a minimum
P.UI t«mpcr&-,ujT o: 2SO' P. ai rtic exn end
durtiic emn~.pling to prevent condensation
tr*jtn. oorurricp. W"ben lanyth Htniuiuon*
itjrtjuter Uik:: iUx-..' B ft 1 are emooui.it-red at
Uuipcrj'.UTfc. Ickfi UIAU 600* P.. Incoloy 025 >,
IT oquifbleiu ma;, be uaed. Probe* for e Trade Lame.
•Dry ualng Drier!
l at 70' F — 10* F.
more ice during the run to keep ihe temper-
ature or the g-iAu leaving the last Lmplnp»-r
as low as ^,iaallj!i- and prtTintUly ol 70* > .
or leis Temper.. Hires abo* e 70' P may peii::t
In doEiugc uj trie dry pas mricr from «H:UT
moisture coi:deii£&tlon or cicti^Jvc heat.
*,1 3 P:ir::cu:n:e train operation For each
run. record tUc dnta required on the exomp:c
sheet ihoft?. ::. Figure 5-2 Thk; reudii.u^ ar.
ench lAmp^-iiy p«. -.:.t. at least c\cry 5 minute.
and w^e;i LU-i.l-i-a:.: change In st^-vK co: -
ri*T.iou& nert-»- i.i;*- addi'.!.j:... nd_'i^tm'.-!r_-
.:; flow rA'.c TV bri;!i: kair.pl — : p^.i.*.!iti tl.f-
i \o'£f.lt- a '. ". : i r f: i .1 - l ra v erst p \j 1 1 . t »• : :^ ; ': c
t!p ptj!ni::ii: d'_ref tly into tj:c g:u fl;rcr\:-i
Iir.DK'd:a:i-'-. s'.ir: the pi:tnp u::d adjust t:ie
P.&w l,- i.-l i.. ..i.' v cot'.dLi:oi'.s bun:;-. i- 'or L:
. .1". iach ti^\t.p c p*..:.'. s.\n.-
. : ^c ;:•.( ^H)t ,Vr C5 \ p^;:.
irtc fnptd td.-Ui1. mei.: of T..,
. *;:!.L.:'. o' :.ir c. :r.p..;a' \ -
thr.c r.onu-E- : '- 'I irn o.T tlic pun-p at *,!:•:
eoiiClu;.1.-':! •' f.c': r«u «i.d rcc-. rd ; he :•.:•..»;
reaiii:;^^ HL:. ••. c :ne prjln- u::- :H.^L> Ir->;
the stack BI.^ hQ:,t:;e ir. a.-.crdanc^ wJilj ih-
sample recovery process dcfacr.urd in scct.o:.
4.2
FEDERAl OCGISTER. VOL. 36, NO 247—THURSDAr. DECEMBER 33, 1971
-------
IDLES AND REGULATIONS
iocJti(M_
O>UA:«_
WT|
13.(-
P. 14
tCrtt „..,... n..r-,|
Volume of water vapor.
eguation ;>-2
where:
V,.,.- Volume aS water vapor 1n tbe ff»*
sample (standard condltlonfi l .
CU. fL.
Vi,'* Total Tolume of liquid collected :n
l ai pi opera and silica gel (wo Fir.
uff 5-0). ml
4.3 Simple recovery. Exercl** care in mov-
ing the cullectlon tram Irom the 1*31 cite to
Uie fiimjj.i recovery area to minimize in*
low ot cui letted sample or the gam of
. ertraneoua particuJai* mau*r. Set aside a
porituu of iLe acctoi.c used In tbe aunplo
recovery as a bUnk fpr analysis. Measure tbo
volume or wui*r from th« nrst three Ira-
plngerb, then discard. Placfl the &lea lo
coii'.alnerc as follou^:
Conraint-r N'o. J. Remove the QJtcr from
ltd holder, p'.tcc In tbli cout&lner. and ceal.
Container A'o. 2. Place loose psrticujate.
inaiUr and bcetcno washluca d 001 all
•ample-eipos«d surTacw prior to the alter
in this container and seal. Dee a razor blade,
brusU or rubber policeman to lose adhering
pariiclcs.
Container Ko. 3. Tmusfer the glJlca gel
froiu the fourth Lmpinger to the orlfilcal con-
tainer and sea) Use a rubber policeman u
an aid in removing iilicft gel from tht
Implt.fcr
4.3 Ajia:yi»lB. Record Uie data required on
tbe eidDiple sheet shown la Figure 6-3.
HandJe each sample container a* follows:
Container NO. i. Tranaler the filter and
'any loo&c partlculate matter from the sample
container to » tared glasi weighing dUb.
desiccate, and dry to a constant weight. R«-
port results to the nearest 0.6 mg.
Container No. 2. Transfer the acetooa
wasuiugA 10 a tared beaker and evaporate to
dryucaa at ambient temperature and prea-
•ure Desiccate and dry to a constant weight.
Hepwrt reiuHi to Uic utarest 0.5 mg.
t aUlu gel
Container No. 3. Weigh tbe i
and report to the nearett i
6. Calibration.
UM methoda and equipment vhtch have
been approved by the Administrator u>
calibrate the onflc* meter, pilot tub*, dry
gu meter, and probe heater. "
after each test lerlei.
.
6.1 Average dry KM meter temperature
tnd avenge ortOcc preaure drop. See d«u
•heet (ngure 5-2).
«JJ Dry gu volume. Correct the uciple
volume meaaur«d bv tfae dry ga* meter to
atindarj condluona (70- T.. 28.83 Inches He)
by ujlng aquation 4-1.
Mii^.-Molt-u :_- »etght a: vmi«r. 18 lb./
ib • ii.-.:-
R^Ideal "B&O cojirtant. 21,0^ Inched
Hg — cu- ft. :i> -mole-'R.
T.^- A'jaulu'-e tcnip.--iiiii.-T a; alandarU
coud:iioQ* ojO' FL
PM-- Aba -:ut* prrs-ure at staudard con-
ditions. 20^2 '.'i •»!*» H^.
0.4 iloie'.ure content.
V.. .
i-qi:,,i:,.:i .'.
.,' v. ..i/; TJ^ r it,::. ^
17.71
in. BB
/p .4H\
I * fc«t + 7^-; 1
.( - LL")
'\ T. /
eqtutioD 5* 1
where:
V-.,.— Volume of fu umple through the
dry gm> meter (aundud conoj-
tlon*) . ca. fi.
'.— Volume at g*t aample through the
dry gat meter (meter oondj-
aone). cu. ft.
T.n~ Absolute tempermture at ttandard
coooitloni. MO' a
0.5 Total participate weight. ftttnnlne
the total partlculau: cAtch from the sum ot
the wc:guu on the an^TtU data iher*.
(Plgnre 5-3'
0.0 Concentration
fl.fl.l Concentrauon in gr 's c J.
wbcn:
equaiion 5-4
v- i\ •• .
ULaliJlL'd col.J.tt. : • . cu. IL
fEOEBAl UOJSTE*. VOL J6, NO. J47—IHU8SDAT. DKEMBIB 1J. to?I
29
-------
KULES AND REGULATIONS
PLANT.
DATE
RUN NO.
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT Of PARTICULATE COLLECTED.
1 . eng
FINAL WEIGHT
'.TARE WEIGHT
-
:x^:
WEIGHT GAIN
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGES
VOLUME.
ml
SILICA GEL
WEIGHT.
g
fl*| ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER. 41 g. ml):
INCREASE, g
(1 9/ml)
vircm of tsoktiirnr i&mptlrv.
oLJ ToluiEC ot lltiuid ooll«ci«l to
nii'l sUic* jrl law Ku'. 1-3} ml.
Jointly o( wtlw. l^./iul.
dni:)(;v cvrmttj.i. 3ij3 inchca H
j »eUhl of wftto. .
of gaflmniti!* through ibedry g« i
condlliuii3), cu. n.
l^ hiKjfr diy |U mttff
"
r prrsiure k
v.L-^f iweesLu* diuii »crofi the 0rtV (Mr
Kti- .V-.').tnctna ||:o.
teilti:i> »»era(r suck eu terapcraturt ts*
oUt sjiDpUnt; tlmf. mln.
t:i^k pw T»!ortly cklculiled by MtL'iod 7
- •'
i. ft.
6.8 'Acceptable results. The following
range sett me limit on acceptable laoklne-.tc
sampling rr^u!u:
If SOS < 1 < 1 10%. the- reaultaare *co«ptab>.
otheru-iic, reject tb« reeuJta and repeat
the Ubi.
7. Reference.
Addendum to 8p«clflc«tloiu for Incinerator
TeatiDB ftt PedanU PocLIlUeB. PHS, NCAPC.
Dec. 3. 1007.
Martin. Robert M.. Conaiructlon X>et&llf of
looklnetlc Source S&mpllng Equipment. En-
vironmental Protection Agency. APTD-0.*.?i.
Rom. Jerome J.. Maintenance. C&librnt'.M:.
and Operation of laokinetlc Source Sa:n-
plftug Equipment, Environmental I-iotcci:cn
Agency, APTD-0576.
Smith, w, 3.. R. T. anlgehajiv aod w. r
Todd. A Mrtriod of Interprc;iu6- SLACK :>.-jr.-
pling Data, Paper presented at tbe 63d An-
nual Meeting of Uie Air Polluoon Control
AasocJation. St. bouia. Mo.. June 14-10. li-'O
Smith. W 6.. *t al.. Stock Otu Samp:)",;
Improved and Simplified with Nrw E<;uip-
meut. APCA paper No. 67-119. 1967.
Spwlficatlona for lactneretor Testing ai
FederaJ Hacllltlae. PHS. NCAPC, 19S7.
VOLUME WATER, ml
Figure 5-3. Analytical data.
Concentration in Ibyou. ft.
1
e.-Concentration of puttciUolv mattv tu Tirfc
Hj..'3.c.f.. dry tMob.
equation 5-5
[.••Tot*} totomit of ptrttculaU nutter ooLwicd.
i^ -Volume of gu maple Uuwijh dry gts meter
IMADd&rd oondiuoni), cu. ft.
r JEquation 6-C
FIDERAL «CIJTH, VOL 36, NO. J47—THURSDAY, DECEMBER 33, 197]
3C
-------
APPENDIX B
STACK GAS AND SAMPLING DATA
31
-------
TABLE B-l. STACK GAS DATA - SECONDARY LEAD SMELTER
10
Run No .
1A
B
2A
B
3A
B
4A
B
5A
B
6A
B
7A
B
/Ap (avg)
cm H20 2
1.18
1.26
1.21
1.24
1.22
1.26
1.27
Ts (avg)
C
61
64
62
68
69
65
74
Ps
mm Hg
748.0
745.5
744.2
739.4
732.8
740.4
740.4
02,
18.5
18.5
18.5
18.5
18.5
18.5
18.5
co2
2.3
2.3
2.3
2.3
2.3
2.3
2.3
r
2.45
2.74
1.98
2.04
2.84
3.09
2.99
2.80
3.69
3.57
2.69
2.83
1.91
2.14
Md,
Ib/lb-mole
29.1
29.1
29.1
29.1
29.1
29.1
29.1
Vs (avg),
m/s
13.3
14.4
13.7
14.3
14.2
°
14.3
14.8
-------
TABLE B-2. SAMPLING DATA - SECONDARY LEAD PLANT
Run Ho
1A
B
2A
B
3A
B
4A
B
5A
B
6A
B
7A
B
Meter Volua*
' "
.30
.05
.49
.33
.39
.26
.50
.37
.47
.35
.37
.25
.94
.83
Percent
Ifoklnetlc
100
96
99
94
101.
97
103
99
105
101
102
98
105
101
Filter Box
142
149
94
97
92
149
94
149
148
96
92
151
123
118
Cat 9
Filter outlet
151
153
98
95
99
155
101
157
154
91
94
148
122
230
Caa «
probe outlet
148
148
95
93
94
148
94
148
148
99
92
148
122
120
Probe
Mid-point
128
149
94
96
104
164
95
138
148
84
108
153
128
139
CO
CO
-------
TECHNICAL REPORT DATA
iTlcaf:- read histnif lions en the n.'1'erse before coir:/:!i'ringj
1. REPORT NO.
EPA-600/2-79-116
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
EVALUATION OF STATIONARY SOURCE PARTICULATE MEASUREMENT
METHODS
Volume V. Secondary Lead Smelters
B REPORT DATE
June 1979
6. PERFORMING ORGANIZATION CODE
. AUTHOR(S)
8. PERFORMING ORGANIZATION REPORT NO.
J. E. Howes, Jr., R. N. Pesut, and W. M. Henry
. PERFORMING ORGANIZATION NAME AND ADDRESS
Jattelle, Columbus Laboratories
505 King Avenue
olumbus, Ohio 43201
10. PROGRAM ELEMENT NO.
1AD712 (FY-75)
11. CONTRACT/GRANT NO.
68-02-0609
12. SPONSORING AGENCY NAME AND ADDRESS
invironmental Sciences Research Laboratory - RTP, NC
Dffice of Research and Development
U.S. Environmental Protection Agency
Research Triangle Park, N.C. 27711
13. TYPE OF REPORT AND PERIOD COVERED
Interim 10/73 - 6/77
14. SPONSORING AGENCY CODE
EPA/600/09
15. SUPPLEMENTARY NOTES
Volume I was issued as EPA 650/2-75-051a, June .1975.
Volume II was issued as EPA 600/2-77-026, February 1977.
16. ABSTRACT
Operation of the Method 5 sampling system at secondary lead smelters with probe outlet
and filter box temperatures of 93°C (200°F) and 149°C (300°F), respectively, yielded
statistically equivalent mass loading results. Chemical analyses revealed no composi-
tional differences in the particulate matter collected at the two different sampling
temperatures. Sampling with MSA 1106 BH glass filters, as specified by Method 5, and
with ADL quartz-type filters yielded no statistically significant differences for
particulate mass loading or composition of the collected emissions. The Method 5 samp-
ling train system did not induce compositional changes in the particulate collections.
Samples taken from the probe and filter sections of the sampling train were composi-
tionally similar to grab samples and to samples taken from the stack emission control
baghouse collector.
The precision (repeatability) of particulate mass emission measurements by Method 5, on
the basis of paired sampling tests, was about 1.5 percent when the two systems were
operated simultaneously at a single fixed point in the stack. The collection efficiency
of the system for lead compounds was very good.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
* Air pollution
* Particles
* Flue gases
* Collection Methods
* Evaluation
* Temperature
* Lead inorganic compounds
* Smeltprs
b.IDENTIFIERS/OPEN ENDED TERMS
c. COSATl 1'icld/Group
13B
21B
14B
07 B
11F
18. DISTRIBUTION STATEMENT
RELEASE TO PUBLIC
19. SECURITY CLASS i This Report/
UNCLASSIFIED
20 SECURITY CLASS (This pagei
UNCLASSIFIED
21. NO. OF PAGES
40
22. PRICE
EPA For". 7220-1 (R.:v 1-7
34
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