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

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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

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                                                     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

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        APPENDIX B
STACK GAS AND SAMPLING DATA
             31

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                                  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


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                                                 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

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                                   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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