Series-1 -100-7/82
EVALUATION OF STATIONARY
SOURCE PERFORMANCE TESTS
 Emission Testing Concepts
 and Special Topics
 A
U S ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF AIR, NOISE AND RADIATION
STATIONARY SOURCE COMPLIANCE DIVISION
WASHINGTON DC 20460

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                                       DRAFT
   EVALUATION OF STATIONARY  SOURCE
          PERFORMANCE TESTS
    Emission Testing Concepts  and
          Special Problems
             Prepared by

      PEDCo Environmental,  Inc.
  505 South Duke Street, Suite  503
    Durham, North Carolina   27701
            Prepared for

U.S. ENVIRONMENTAL PROTECTION AGENCY
 OFFICE OF AIR, NOISE AND RADIATION
STATIONARY SOURCE COMPLIANCE DIVISION
       WASHINGTON, D.C.   20460
              July 1982

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                             INTENDED PURPOSE
     This is not an official policy and standards document.  The opinions,
findings, and conclusions are those of the authors and not necessarily those
of the Environmental Protection Agency.  Every attempt has been made to repre-
sent the present state of the art as well as subject areas still under eval-
uation.  Any mention of products or organizations does not constitute endorse-
ment by the United States Environmental Protection Agency.

     This document is issued by the Stationary Source Compliance Division,
Office of Air Quality Planning and Standards, USEPA.  It is for use in work-
shops presented by Agency staff and others receiving contractual or grant
support from the USEPA.  It is part of a series of instructional manuals
addressing compliance testing procedures.

     Governmental air pollution control agencies establishing training pro-
grams may receive single copies of this document, free of charge, from the
Stationary Source Compliance Division Workshop Coordinator, USEPA, MD-7,
Research Triangle Park, NC 27711.  Since the document is specially designed
to be used in conjunction with other training materials and will be updated
and revised as needed periodically, it is not issued as an EPA publication
nor copies maintained for public distribution.
                                   iii

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                            CONTENTS

                                                            Page

Section A.  Introduction to Source Sampling (Lecture 101)   A-l

     1.  Basic terminology and nomenclature                 A-3
     2.  Slides                                             A-25

Section B.  Method 1 (Lecture 102)                          B-l

     1.  Method 1—Sample and velocity traverses for sta-
         tionary sources                                    B-3
     2.  Slides                                             B-15

Section C.  Method 2 (Lecture 103)                          C-l

     1.  Method 2—Determination of stack gas velocity and
         volumetric flow rate                               C-3
     2.  Slides                                             C-35,

Section D.  Method 3 (Lecture 104)                          D-l

     1.  Method 3—Gas analysis for carbon dioxide, oxy-
         gen, excess air, and dry molecular weight          D-3
     2.  Slides                                             D-19

Section E.  Method 4 (Lecture 105)                          E-l

     1.  Method 4—Determination of moisture content in
         stack gases                                        E-3
     2.  Slides                                             E-21

Section F.  Method 5 (Lecture 106)          •                F-l

     1.  Method 5—Determination of particulate emissions
         from stationary sources                            F-3
     2.  Slides                                             F-43

Section G.  Method 6 (Lecture 107)                          G-l

     1.  Method 6—Determination of sulfur dioxide emis-
         sions from stationary sources                      G-3
     2.  Slides                                             G-19

Section H.  Method 7 (Lecture 108)                          H-l

     1.  Method 7—Determination of nitrogen oxide emis-
         sions from stationary sources                      H-3
     2.  Slides                                             H-19

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                      CONTENTS (continued)

                                                            Page
                                                            - •- jr

Section I.  Method 8 (Lecture  109)                           1-1

     1.  Method 8—Determination of sulfuric acid mist and
         sulfur dioxide emissions from stationary sources   1-3
     2.  Slides                                             1-21

Section J.  Highlights of EPA Methods 1-5 (Lecture 150)      j-l

Section K.  Summary of Equations (Lecture 151)               K-l

     1.  Source sampling calculations                       K-3
     2.  Slides                                             K-19

Section L.  Misalignment of Pitot Tube (Lecture 152)         L-!

     1.  Pitot tube errors due to misalignment and non-
         streamlined flow                                   L-3
     2.  Slides                                             L-7

Section M.  Isokinetic Sampling and Biases from Noniso-
  kinetic Sampling (Lecture 153)                             M-l

     1.  A method of interpreting stack sampling data       M-3
     2.  Slides                                             M-13

Section N.  Precision and Accuracy of Test Methods          N-l
  (Lecture 154)
     1.  Information to support data quality acceptance
         for performance audits and routine monitoring      N-3
     2.  Error analyses                                     N-8
     3.  Slides                                             N-13

Section 0.  Significance of Error for Source Test
  Observers (Lecture 155)                                    O-l

     1.  Use of significance of error for source test
         observer's decisions                               O-3
     2.  Slides                                             O-ll

Section P.  Stack Sampling Nomographs (Lecture 156)         P-l

     1.  Stack sampling nomographs for field validation     P-3
     2.  Slides                                             P-27
                              vi

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                 SECTION A.  INTRODUCTION TO SOURCE SAMPLING
Subject                                                                Page
1.  Basic terrm'nology and nomenclature  (taken  frofh the  APTI Course
    450 manual)                                                        A-3
2.  Slides                                                             A-25
                                     A-l

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                Basic Terminology and Nomenclature
There are three terms which are used to describe what exists in a stack:
1.   Concentration - The quantity of a pollutant per quantity of effluent
     gas.  An example of this is:
          grains (a weight unit)/cubic foot (a  volume unit)
2.   Stack gas flow rate - the quantity of effluent gas passing up the stack
     per length of time.  An example of this is:
          cubic feet (a volume unit)/hour  (a time  unit)
3.   Pollutant mass rate - The quantity of pollutant passing up the stack
     per length of time.  An example of this is:
          pounds (a weight unit)/hour (a time unit)
These three terms are related to each other by  the .equation:
          where pmr   =  average pollutant mass emissions  rate
                 c~    =  average stack concentration
                 Q_   =  average volumetric flow rate from the  stack
     The objective is to determine pmr ,  so the general  approach  is  to  determine
                                      *)
c". and Q_ (see Stack Sampling Flow Diagram).   c_ is determined  through  sampling
 o      o                                      o
train design.  Q"  is given by the equatipn

          Qs - Vs As ^
               where v"s =  average stack velocity
                     AS =  cross-section area of the stack

     The cross-section area Ag is easily determined.  The task  of determin.ing
the average stack velocity, V , is discussed in a following section.
                                    A-3

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                        Stack Sampling Fiow  Diagram
     The overall  objective of stack  sampling is the determination of the average


pollution mass emission rate (pmrs)  and can be summarized by the flow diagram


below.
              Q   =  A  v
               s      s  s
                                   prar  = c  0
                                   r  s    s x
                                          M
                                      Composition
                                                    Sampling Train Design
                                          A-4

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 i
01
                                           HEATED AREA   v F|LTER HOLDER
                 THERMOMETER
CHECK
VALVE
              .REVERSE-TYPE
                PITOT TUBE
                                PITOT MANOMETER  L
       ICE BATH



BY-PASS VALVE
                                                                                             VACUUM
                                                                                              GAUGE
                                                                                     MAIN VALVE
                                                                                                              VACUUM
                                                                                                               LINE
                                                          Paniculate sampling train.

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                       The Source  Test
A source sampling experiment provides data on source emissions parameters. The
isokinetic source test extracts a representative gas sample from a gas stream.
Although often used only to determine compliance with emissions regulations, the
test data can also provide information useful in evaluating control equipment effi-
ciency or design, process economics, or process control effectiveness. Valid source
sampling experiments,  therefore, yield valuable information to both the industrial
and environmental engineer.
  The source test is an original scientific experiment and should be organized and
executed with the same care taken in performing any analytical  experiment. This
requires that objectives be decided before starting the experiment and that the pro-
cedures  and equipment be designed to aid in reaching those objectives. The quan-
titative or qualitative analysis of the source sample should be incorporated as an in-
tegral part of the source test.  After all work is done, the results should be evaluated
to determine whether objectives have been accomplished. This section contains flow
charts and descriptions to assist in  the design, planning,  and performance of the
source test described.
Source Test Objectives
The essential first step in all experiments is the statement of objectives. The source
test measures a variety of stack gas variables which are used in evaluating several
characteristics of the emissions source. The source experiment should be developed
with techniques and equipment specifically designed to give complete, valid data
relating to these objectives. Approaching the experiment in this manner  increases
the possibilities of a representative sampling of the source parameters to  be
evaluated.
Experiment Design
A well designed experiment incorporates sampling equipment, techniques, and
analysis into an integrated procedure to meet test objectives. The source sampling
experiment must be based on a sampling technique that can collect the data re-
quired. The sampling equipment is then designed to facilitate the sampling pro-
cedure. The analysis of the sample taken must be an integral factor in the
sampling techniques and equipment design. This approach of achieving test objec-
tives provides the best possible source test program.
  Designing a source test experiment requires a knowledge of sampling procedures
and industrial processes, a thoroughly researched sampling experiment, and a good
basic understanding of the process operation to be tested.  This knowledge assists in
determining the types of pollutants emitted and  test procedures and analysis that
                             A-6

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will achieve valid, reliable test results. A literature search of the sampling problem
can yield information that may help improve test results or make testing much
easier.
Final Test Protocol
The final test protocol clearly defines all aspects of the test program, and incor-
porates the work done in research, experiment design, and the presurvey. All
aspects of this test, from objectives through analysis of the sample and results of the
sampling, should be organized into a unified program. This program is then ex-
plained to industrial or regulatory personnel involved. The protocol for the entire
test procedure should be understood and agreed upon prior to the start of the test.
A well organized test protocol saves time and prevents confusion as the work
progresses.
Test Equipment Preparations
The test equipment must be assembled and checked in advance; it should be
calibrated following procedures recommended in the Code of Federal Regulations
and this manual. The entire sampling system should be assembled as intended for
use during the sampling experiment. This assures proper operation of all the com-
ponents and points out possible problems that may need special attention during
the test. This procedure will assist in making preparations and  planning for spare
parts.  The equipment should then be carefully packed for shipment to the
sampling site.
   The proper preparation of sampling train reagents is an important part of get-
ting ready for the sampling experiment. The Method 5 sampling train requires well
identified, precut, glass mat filters that have been desiccated to a constant weight.
These tare weights must be recorded to ensure against errors. Each filter should be
inspected for pinholes that could allow particles to  pass through. The acetone (or
other reagent) used to clean sampling equipment must be a low residue, high
purity solvent stored in glass containers. Silica gel desiccant should be dried at 250 °
to 300°F for 2 hours, then stored in air-tight containers; be sure the indicator has
not decomposed (turned black). It is a good procedure, and relatively inexpensive,
to use glass-distilled, dionized water in the impingers. Any other needed reagents
should be carefully prepared. All pertinent data on the reagents, tare weights, and
volumes should be recorded and filed in the laboratory with duplicates  for the
sampling team leader.
 Testing at the Source
 The first step in performing the source test is establishing communication among
 all parties involved in the test program. The source sampling test team should
 notify the plant and  regulatory agency of their arrival. All aspects of the plant
 operation and sampling experiment should be reviewed and understood by those

                                  A-7

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                              Figure 5-1. Planning  and performing a  stack test.
EACH STACK TEST
SHOULD BE CONSIDERED
AN ORIGINAL SCIENTIFIC
EXPERIMENT
CALIBRATE EQUIPMENT
  •DGM
  •Determine console AH®
  •Noii la
  •Thermometers and
   thermocouples
  •Pressure gages
  •Orsat
  •Pitoc tube and probe
  •Nomographs
                                    DETERMINE NECESSITY OF A SOURCE TEST
                                      •Decide on data required
                                      •Determine that source text will give this data
                                      •Analyze cost
ARRIVAL AT SITE
  •Notify plant and
   regulatory agency
   personnel
  •Review test  plan with all
   concerned
  •Check weather forecasts
  •Confirm process ope.-ation
   parameters in  control room
                                                           ±
                                    STATE SOURCE TEST OBJECTIVES
                                      •Process evaluation
                                      •Process design data
                                      •Regulatory compliance
DESIGN EXPERIMENT
  •Develop sampling approach
  •Select equipment to meet test objectives
  •Select analytical method
  •Evaluate possible errors or biases and correct
   sampling approach
  •Determine manpower needed for test
  •Determine time required for test with margin for
   breakdowns
  •Thoroughly evaluate entire experiment
   with regard to applicable State and Federal
   guidelines
                                    PRE-SURVEY SAMPLING SITE
                                      •Locate hotels and restaurants in area
                                      •Contact plant personnel
                                      •Inform plant personnel of testing objectives and
                                       requirements tor completion
                                      •Note shift changes
                                      •Determine accessibility of sampling site
                                      •Evaluate safety
                                      •Determine pan locations and application to
                                       Method! 1 and 2 (12/23/71  Federal Register)
                                      •Locate electrical power supply to site
                                      •Locale rcstiooms and food at plane
                                      •Drawings, photographs, or  blueprints of sampling site
                                      •Evaluate applicability of sampling approach from
                                       experiment design
                                      •Note any special equipment needed
                                    FINALIZE TEST PLANS
                                                           _L
                                      •Incorporate prcrarrey into experiment design
                                      •Submit experiment design for ap-
                                       proval by Industry and Regulatory Agency
                                      •Set test dates and duration
PREPARE EQUIPMENT FOR TEST
  •Assemble and confirm operation
  •Prepare for shipping
  •Include spare parts and reserve equipment
                       JL
CONFIRM TRAVEL AND SAMPLE TEAM ACCOM-
MODATIONS AT SITE
                                   CONFIRM TEST DATE AND PROCESS OPERATION
                                      •Final step before travel arriving at site
SAMPLING FOR PARTICULATE EMISSIONS
  •Carry equipment to sampling site
  •Locate electrical connections
  •Assemble equipment
PRELIMINARY CAS VELOCITY TRAVERSE
  •Attach thermocouple or thermometer to pilot
   probe assembly
  •Calculate sample points from guidelines outlined in
   Method 1 and 2 of Federal Register
  •Mark pilot probe
  •Traverse duct for velocity profile
  •Record -Ip's and temperature
  •Record duct static pressure
                                                          T
RESEARCH LITERATURE •
  •Basic process operation
  •Type of pollutant emitted
   from process
  •Physical state at source
   conditions
  •Probable points of emission
   from process
  •Read sampling reports
   from other processes
   sampled:
    1. Problems to expect
    2. Estimates of variables
       a. H;>O vapor
       b. Temperature at
         source
  •Study analytical pro-
   cedures used for
   processing test samples
PREPARE FILTERS AND
REAGENTS
  •Mark filters with insoluble
   ink
  •Desiccate tu const-nt
   weight
  •Record weights in per-
   manent laboratory file
  •Copy file for on site record
  •Measure deionized distilled
   HgO for impingers
  •Weigh silica gel
  •Clean sample storage
   containers
DETERMINE APPROX-
IMATE MOLECULAR
WEIGHT OF STACK CAS
USING FYRITE AND
NOMOGRAPHS
APPROXIMATE HoO
VAPOR CONTENTOF
STACK GAS
                                                  A-8

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involved. The proper plant operating parameters and sampling experiment pro-
cedures should be recorded in a test log for future reference. The sampling team is
then ready to proceed to the sampling site.
  The flow diagram outlines the procedures for performing the stack test. The
items given are for a basic Method 5 paniculate sample. Each item is explained in
various sections of this manual. The laboratory training sessions given in Course
450 help to organize the Method 5 test system.
  The flow diagram should be of assistance to those having completed the 450
course curriculum and can also serve as a useful guide to anyone performing a
stack test.
METHODS FOR SETTING THE ISOKINETIC FLOW RATE
IN THE METHOD 5 SAMPLING TRAIN
The commercially available nomograph is often used for the solution of the
isokinetic rate equation. These nomographs have based the solution of the
isokinetic equation upon the assumptions that the pitot tube coefficient will be
0.85, the stack gas dry molecular weight will  be 29.0 Ib/lb-mole and will  only vary
with a change in stack gas moisture content in addition  to relying on the  use of a
drying tube in the train. The nomograph  also assumes that changes in other equa-
tion variables will be insignificant. Many purchasers are unaware of these assump-
tions or manufacturer construction errors  and use the device without calibrating it
or verifying its accuracy. Procedures are presented here  to ascertain the precision of
nomograph construction and its accuracy. The basic equations employed  in con-
structing a nomograph are given and a calibration form is provided.
    The equation for derivation of  the  isokinetic rate is given
below:

                 f         s         n        *  Md Tm Pr~\
(Eq.5-1)    AH- 846.72 Dn4 AH@ Cp2(\~Bws)2   M  -  p     A/»
                 L                                Ms 1s ^m  J
where                      Cp = pitot tube coefficient
                           Dn = nozzle diameter (in.)
                           A//=pressure difference of orifice meter (in. fyO)
                           AH@ = orifice meter coefficient,  AH for 0. 75 cfm at
                                   STP=0.9244/Km2  (in. H2O)
                           Ms = apparent stack gas molecular weight
                              ^Mdfl-BaJ + lSBu, (lb/lb.moie)
                           Md = dry gas  molecular weight (29) for dry air
                            .    (Ib/lb-mole)
                           Ps = absolute stack pressure  (in. Hg)
                           pm = meter absolute pressure (in. Hg)
                           Ap = pressure difference of pitot tube (in. H.2O)
                           Tm = absolute meter temperature = °R= °F+ 460°

                              isokinetic AH = KAp

                  K = Reduced terms in the  isokinetic equation.

                                   A-9

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RECORD ALL INFORMA-
TION ON DATA SHEETS
  •Sample case number
  •Meter console number
  •Probe length
  •Barometric pressure
  •Nozzle diameter
  •C factor-
  •Assumed H2O
  •Team supervisor
  •Observers present
  •Train leak test rate
  •General comments
  •Initial DGM dial readings
TAKE INTEGRATED
SAMPLE OF STACK GAS
FOR ORSAT ANALYSIS (OR
PERFORM MULTIPLE
FYRJTE READINGS
ACROSS DUCT)
           _L
 ANALYZE STACK GAS FOR
 CONSTITUENT GASES
   •Determine molecular
    weight
   •CO, and O»
    concentration for F-factor
    calculations	
            L
 PREPARE OTHER TRAIN;
 FOR REMAINING
 SAMPLING     	
 REPACK EQUIPMENT
 AFTER SAMPLING IS
 COMPLETED
                                                       i
 USE NOMOGRAPH OR CALCULATOR TO SIZE
 NOZZLE AND DETERMINE C FACTOR
   •Adjust for molecular weight and pilot tube C
   •Set K pivot point on nomograph	
 LEAK TEST COMPLETELY ASSEMBLED
 SAMPLING TRAIN @15" Hs VACUUM AND
 MAXIMUM LEAK RATE OF 0.02 CFM	
I NOTIFY ALL CONCERNED THAT TEST IS ABOUT
 TO START	
I CONFIRM PROCESS OPERATING PARAMETERS   I

                       •                         ^
START SOURCE TEST
  •Record start time - military base
  •Record gat velocity
  •Determine AH desired from nomograph
  •Stan pump and set orifice meter
   differential manometer to desired AH
  •Record
      1. Sample point
      2. Time from zero
      3. DGM dial reading
      4. Desired AH
      5. Actual AH
      6. All temperatures DGM, stack, sample case
  •Maintain isokinetic AH at all times
  •Repeat for all points on traverse	
                                                         \ MONITOR PROCESS RATE |
                                                                       '
                                                                                           TAKE MATERIAL
                                                                                           SAMPLES IF NECESSARY
                                                          TAKE CONTROL ROOM
                                                          DATA
 AT CONCLUSION OF TEST RECORD
   •Stop time - 24 hour clock
   •Final DGM
   •Any pertinent observations on sample
  LEAK TEST SAMPLE TRAIN
    •Test at highest vacuum (in. Hg) achieved during test
    •Leak rate should not exceed 0.02 CFM
    •Note location of any  leak if possible	
                                   REPEAT PRECEDING STEPS FOR THREE
                                   PARTICULATE SAMPLES      	
  SAMPLE CLEAN-UP AND RECOVERY

    •dean samples in laboratory or other clean area
     removed from site and protected from the outdoors
    •Note sample condition
    •Store samples in quality assurance containers
    •Mark am1 label .ill samples
    •Pack carefully for shipping if analysis is not done on
     site       	
                                   ANALYZE SAMPLES
                                     •Follow Federal Register or State guidelines
                                     •Document procedures and any variations employed
                                     •Prepare analytical Report Data	
                                    CALCULATE
                                      •Moisture content of stack gas
                                      •Molecular weight of gas
                                      •Volumes sampled at standard conditions
                                      •Concentration/standard volume
                                      •Control device efficiency
                                      •Volumetric flow rate of stack gas
                                      •Calculate pollutant mass rate
                                    WRITE REPORT

                                      •Prepare as possible legal document
                                      •Summarize results
                                      •Illustrate calculations
                                      •Give calculated results
                                      •Include all raw data (proce* dr test)
                                      •Attach descriptions of testing and analytical methods
                                      •Signatures of analytical and lest personnel
                                    SEND REPORT WITHIN MAXIMUM TIME
                                    TO INTERESTED PARTIES	
                                                    A-10

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          _L
CALIBRATE EQUIPMENT
  •Noules
  •DGM
  •Orifice meter
  •Mncr console
  •Pilot tubes
  •Nomograph
                                      Figure 5-2. Source cest outline.
[ASSEMBLE SAMPLING TRAIN
                      X
  LEAK TEST
    •Pilot lino
    •Meter console
    •Sampling train @ 15" Hg.
                                 SET UP NOMOGRAPH OR CALCULATOR
                                                                                                 JL
•Mark dry and desiccate
 filters to constant weight
•Assemble in filter* and ical
 until ready to use
ESTIMATE COz
CONCENTRATION USING
FYRITE



CALCULATE SAMPLE POINT USING
1
DO PRELIMINARY TEMPERATURE
VELOCITY TRAVERSE
METHOD 1

AND
I . -

1
ESTIMATE H?
USING WET B
BULB
1
 PREPARE TO TAKE
 INTEGRATED SAMPLE OF
 FLUE GAS DURING EN-
 TIRE DURATION OF TEST
I ANALYZE USING ORSAT
  FILL OUT DATA SHEET
    •Date    *DGM Reading
    •Time   'Test time at each point
  MONITOR AT EACH TEST POINT
    •DGM—On time
    •Ap
    •Appropriate AH
    •Slack temperature
    •Sample case temperature
    •Impinger temperature
                                 STOP TEST AND RECORD
                                   •Final DGM
                                   •Slop time
                                   •Note* on sampling and appearance of sample
MONITOR BOILER
OPERATION
                                                                                      RECORD FUEL FEED
                                                                                      RATE AND PRODUCTION
                                                                                      RATE
                                 LEAK TEST AT HIGHEST VACUUM REACHED
                                 DURING TEST
SAMPLE CLEAN-UP
•Probe & nozzle
•Filter
•H2O
•Silica Gel
                                 CALCULATE
                                   •Moisture content of gas
                                   •Molecular weight of gas (dry Ic wet)
                                   •Average gas velocity
                                   •% isokinelic
                                   •Pollutant mass rate
                                    (concentration and ratio of areas)
                                                 WRITE REPORT
                                                      A-ll

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  The Method 5 sampling train is intended to operate at a sampling rate of
0.75 cfm of dry air at 68°F and 29.92 in. Hg. The orifice meter pressure differen-
tial that would produce such a sampling rate through the orifice is designated
  An additional equation is necessary in order to estimate the nozzle diameter that
will give a flow rate of 0.75 cfm at a reasonable pressure drop across the orifice
meter.                         /;
                                .0358
(Eq.5-2)
                              /
                        n   1 /°-
                       Dn=\/
                            j/
                                Tm Cp(l-Bws)

where                      Dn = nozzle diameter (in.)
                            Qjn~ volumetric flow rate through meter (ft*)
                            Pm = absolute pressure at meter (in. Hg)
                            Ps = absolute pressure at stack (in. Hg)
                            Tm = absolute temperature at meter (°R)
                            Ts = absolute temperature at  stack (°R)
                            Cp — pitot tube calibration coefficient
                            Bws = water vapor in stack gas, volume fraction
                            Ms = molecular weight of stack gas, wet basis
                                 (Ib/lb-mole)
                              i = average velocity head of stack gas (in. H2O)
  Once Dn is calculated, the source tester should select the nozzle in his tool box
which has a value closest to that calculated. The actual nozzle used should be
checked with calipers, and that value of Dn is then substituted in Equation 5-1.
  Most of the variables in this equation  and the isokinetic AH equation are known
prior to sampling or can be closely estimated. Often the solution to the equation
can be partially calculated before the sampling with the few remaining variables
inserted and the equation quickly solved on site. The calculation of isokinetic AH
using the derived equations allows the sampler to more quickly and easily adjust
the sampling rate for changes in the stack gas variables.

SAMPLING METER CONSOLE OPERATION
The sampling meter console must be calibrated and thoroughly leak tested Meter console
operating  procedures will differ somewhat according to manufacturer. The pro-
cedures discussed here will  aid in operating most types of consoles. The objective is
to understand console operating procedures for isokinetic source sampling.
 Sampling Train Leak Tests
 Completely assemble the sampling train as intended for use during the test. Turn
 on probe and filter heating systems and allow them to reach operating
 temperatures. Disconnect the umbilical cord vacuum  line and turn on the meter

                                      A-12

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console pump. This allows the pump to lubricate itself and to warm up (this is
especially important in cold weather). Leak test the pitot tubes and lines during
this warm up.

  The pitot tube impact pressure leg is leak tested by applying a positive pressure.
Blow into the impact opening until  > 7.6 cm (3 inches) 1^0 is indicated by the
differential pressure gage.  Seal the impact opening. The pressure should be stable
for at least 15 seconds. The static pressure leg of the pitot tube is leak tested in a
similar way by drawing a negative pressure > 7.6 cm H<>0. Correct any leaks.
  The sampling train is leak tested when it has reached operating temperature.
Turn off the console pump; connect the umbilical vacuum line.  With the coarse
control value completely off, turn the fine adjustment (bypass) valve completely
counterclockwise.  Plug the nozzle inlet and turn on the  console pump. Slowly turn
the coarse adjustment valve fully open. Gradually turn the fine adjustment valve
clockwise until 380 mm  (15 inches) Hg vacuum appears on the vacuum gage. If
this vacuum  is exceeded, do not  turn the fine adjustment valve back
counterclockwise;  proceed with the leak test at the vacuum indicated or slowly
release the nozzle  plug and restart the leak test. At the desired vacuum observe the
dry gas meter pointer. Using  a stopwatch, time the leak rate for at least 60
seconds. The maximum allowable leak is 0.00057 m^/min. (0.02 cfm). Having
determined the leak rate,  slowly release  the nozzle plug  to bleed air into the train;
when the vacuum falls below  130 mm(5 inches) Hg, turn the coarse adjustment
valve completely off. If the leak test  is unacceptable, trace all sections of the
sampling train from the filter holder inlet back, (i.e., leak test from the filter inlet,
then the first impinger,  etc.)  until the leak is found.  Correct the leak and retest.
Leak test at  the highest  vacuum reached during the test after the completing the
sampling procedure. Testing  for leaks should also be done any time  the train is
serviced (i.e., filter holder change).  Record all dry gas meter readings and leak
rates for each leak test.
 Train Operation
 When the leak tests are completed, the sampling console should be prepared for
 sampling. The sampling console differential pressure gages for the pitot tubes and
 orifice meter should be checked. Zero and level the gages as required. If the con-
 sole does not use oil manometers, the gages must agree with an oil manometer
 within 5 percent for at least 3 Ap readings taken in the stack. This check should be
 done before testing. Oil manometers should be periodically leveled and re-zeroed
 during the test if they are used in the console.
   The consoli. operator should then determine the source variables used in solving
 the isokinetic rate equation. The isokinetic AH may be determined by using a
 nomograph, an electronic calculator,  or a source sampling slide rule. The variables
 that need to be determined  are: stack gas moisture content, average gas velocity
 pressure (Ap),  stack gas temperature,  and estimated average console dry gas mecer
 temperature. The stack gas  moisture can  be determined  by Reference Method 4

                                        A-13

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sampling or estimated with a wet bulb-dry bulb thermometer technique. The
average Ap and stack gas temperature are determined by a preliminary stack
traverse. The dry gas meter average temperature can be estimated to be 10°C
(25°— 30°F) greater than the ambient temperature at the site. These values are
then used in the nomograph or calculator to find the isokinetic AH.
  The operator can now set up the sampling data  sheet.  Record the dry gas meter
initial reading. Position sampling train at the first  sampling point; read the pitot
tube Ap  and calculate the corresponding AH. Record starting time of the test.
Turn on the console pump and open the coarse sampling valve while
simultaneously starting a stopwatch. Adjust AH to the proper value using the fine
adjustment valve. Check temperatures and record all data on the data sheet.
  The sampling train should be moved to the next sampling point about
15 seconds before the time at point one is over. This allows the pitot tube reading
to stabilize. The dry gas meter volume at the point sampled is read when the stop-
watch shows the point sample time is over. The operator should quickly read the
Ap  and calculate AH for the next point,  then set the proper sampling rate. Record
all data and proceed as described for  all points on the traverse. At the end of the
test, close the coarse valve, stop  the pump, and record the stop time. Record the
final dry gas meter reading. Remove the  sampling train from the stack and test the
system for leaks. Record the leak rate. After the train has cooled off, proceed to
the cleanup area.

SAMPLING CASE PREPARATION
Inspect and clean the source  sampling glassware case before a sampling experi-
ment; remove and clean the sample case  glassware. Check the case for needed
repairs and calibrate the filter heater. Store the case completely assembled.
Glassware
All glassware including the filter holder and frit should be disassembled and
cleaned. Separate the individual glass pieces and check for breaks or cracks. Pieces
needing repair are cleaned after repairs have been made.  A thorough glass clean-
ing for simple particulate testing is done with soap and water followed by a
distilled water rinse. If analytical work is to be performed on the sample water
condensed, clean the glassware by soaking in a methanol-basic hydroxide (NaOH or
KOH) solution with pH>9. Glass should be left in the base solution until any stains
can be easily washed away, but not any longer than 48 hours as the solution can
etch the glass. The base should be rinsed away with several portions of distilled
water. If ball-joint glassware is used, remove  vacuum grease before cleaning with
heptane, hexane, or other suitable solvent. Clean the glass frit by pulling several
aliquots of HNC>3 through the glass frit with a vacuum pump. It should be rinsed
at least three times with double volumes of distilled water and dried before using.
                                   A-14

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The rubber gasket surrounding the frit should be cleaned, removing any particles
imbedded in the rubber, which could prevent proper sealing. The frit and gasket
must be constructed such that the glass filter mat does not become compressed in
the sealing area. If this is not the case, or the rubber is in poor condition,  discard
the frit.
The Sample Case
The sample case should be checked thoroughly for needed repairs. All handles,
brackets, clamps, and electrical connections must  be inspected. Insulation in both
the hot and cold areas must be in good condition. The sample case should not leak
water from the melting ice into the filter heating compartment. The impinger sec-
tion should have protective foam padding on the bottom and a good drainage
system. The drain plug should be clean.
   Calibrate the heater in the filter compartment to maintain a temperature around
the filter of 120°± 14°C (248°±25°F)or at other temperatures as specified in the
subparts of Title 40 of the Code of Federal Regulations. This calibration should be
performed at several conditions (to account for seasonal weather changes) so that
the filter compartment temperature can be maintained at  the proper level at all
times. Often during sampling the filter section is not easy to see, consequently, the
filter temperature is difficult to monitor accurately. If the  case is calibrated for
several conditions, operators can maintain proper temperature control more closely.

Sampling Preparations
The sample case is readied for sampling by filling the impingers with water and
silica gel. Impingers 1 and 2 are each filled with 100 ml of water by inserting a
funnel in the side arm and slowly pouring in the water. This makes it easy to
displace in the impinger and keeps the water from filling the bubbler tube. The
third impinger is left dry. The fourth impinger is filled with 200-300 gm of pre-
weighed silica gel. The silica gel must be added through the side arm. This
prevents dust from collecting on greased ball joints or silica gel from being pulled
up the center tube and out of the impinger. After loading the impingers, securely
fasten the U-joints. Attach the probe to the sampling case and secure the filter
holder in position. Allow the filter compartment and probe to reach operating
 temperature. Leak test the assembled train from the probe nozzle by pulling
 380 mm Hg (15 in. Hg) vacuum on the system. The maximum allowable leak rate
 is 0.00057 m3/min (0.02 cfm). After the  leak test, fill the impinger section with
 ice and allow time for all temperatures to stabilize.

 SAMPLING PROBE PREPARATION
 The sampling probe should be thoroughly inspected before field use. Remove the
 glass probe  liner  by loosening the union at the end of the  probe. Completely
 disassemble the probe union and seal gasket, and inspect all the individual  com-
 ponents

                                          A-15

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Probe Sheath and Pitot Tubes
The stainless steel probe sheath should have a small hole drilled near the end of
the probe. This .prevents a pressure differential inside the sheath from possibly
diluting the sample with air drawn down the probe. If the hole is not there, the
probe end (fitted into the sample case) should be sealed air tight. Check the weld
at the swage fittings for cracks and repair if necessary. Inspect the pitot tubes for
damage and proper construction details  (see pitot tube calibration section). Pitot
tubes should be cleaned, checked for cracks or breaks, and securely fastened to the
probe sheath to prevent accidental misalignment in the stack. All pitot tubes and
components must be leak tested.
  Examine the union and seal gasket for wear. A stainless steel ring should be in-
cluded in the union-gasket configuration for good compression and an air tight
seal. If a rubber o-ring gasket is used (stack temperatures < 350 °F) it should be
inspected for wear and replaced if necessary. Asbestos string gaskets must be
replaced each time the union-gasket is disassembled. After inspecting  the glass
liner-heating element, reassemble the probe in the following manner to prevent
leaks:
       1.   Insert glass liner through probe  and swage nut;
       2.   Place stainless steel ring over glass with flat side facing out;
       3.   Fit gasket over glass liner and push onto steel ring;
       4.   Align glass liner end with edge of swage nut  closest to pitot tube orifice
           openings;
       5.   Screw the union on finger tight;
       6.   Use probe wrenches to tighten the union. If too much tightening is done
           here,  the end of the glass liner will break.

Glass Liner-Heating Element
The glass liner should be thoroughly cleaned with a probe brush, acetone,  and
distilled t^O.  If it will not come clean in this manner, it should be cleaned with
dilute HC1 or replaced.  The  glass liner-heating element in many sampling probes
can not be separated, making thorough cleaning difficult. An easily separated
liner-heater is a great advantage.
   The heating element should be checked for good electrical insulation; the insula-
tion on a frequently used probe liner heating element will eventually be worn or
burned away. This can expose frayed  wires, which may short against the probe
sheath. These hazards can be avoided with careful inspections and repair. After
thorough inspection, check the heating element in the reassembled probe. This
procedure is helpful in finding problems before arrival at the sampling site. Atten-
tion should be given to the function of the  electrical system and wrappings around
the glass liner; these wraps help prevent electrical shorts against the probe sheath
while minimizing glass liner flexing that can cause a liner break or electrical short.
                                       A-16

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Summary

A thorough probe check before a sampling experiment helps prevent field
problems. Disassemble the probe and inspect all components. Make certain con-'
struction details and integrity are correct. Clean the glass liner thoroughly. Check
the heating element electrical connections. Test the reassembled probe for leaks
and proper heating.

CLEANING AND ANALYTICAL PROCEDURES
FOR THE METHOD 5 SAMPLING TRAIN
The clean-up and analysis of the sample taken with the Method 5 Sampling Train
is an integral part of the entire experiment. The precise operation of Method 5
Sampling equipment must be complemented by a careful clean-up of the train
components. Analysis of the sample using approved procedures and good
laboratory technique provides accurate laboratory data.  Good testing at  the stack
must be followed by accurate analysis in the laboratory so that valid data may be
presented.
Cleaning the Sampling Train
The sequence of procedures in cleaning the sampling train is best presented in an
outline-flowchart form. Each step is presented with appropriate comments.


Additional Comments
The flowchart (Figure 5-3) gives the general procedure for sample clean-up. Many
factors can affect the accuracy of the final sample obtained. Care and experience
are very important when cleaning the sample train.  A number of helpful tips are
given below;
       1.   Always perform clean-up procedures in a clean,  quiet area. The best
           area is a laboratory.
       2.   Make a probe holder for the probe cleaning procedure or be sure two
           people perform the procedure; this prevents spills and accidents.
       3.   Clean all equipment in an area where an accidental spill may be
           recovered without contaminating the  original sample.
           a.  Open and clean the filter holder  over clean glassine or waxed
               paper so  that a spill can be recovered.
           b.  Clean probe into a container sitting  on the same type of glassine
               paper.
       4.   Clean the probe equipment thoroughly:
           a.  Brush probe a minimum of three times.
           b.  Visually inspect the probe interior.
           c.  Record appearance and confidence of cleanliness.
           d.  Repeat brushing until cleaning is complete.
           e.  Confidence ^  99%. Check with  tared cotton swab brushed  through
               probe.
                             A-17

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                                  Figure 5-3. Cleaning the sample train.
                                                                           Testing completed
                                                               Perform final leak check on sampling train
                                                               with vacuum 2:  test vacuum. Leak rate must
                                                               be •£ 0.02 cfm.
                                              Inspect sample and record observations
Impinger water color
and turbidity
Filter appearance
Appearance of probe
and all other glassware
Allow hot probe
to cool sufficiently
                                    Disassemble sampling train (log all information in test log)
                                                                                T
Z. Be sure cap wiu not
melt to nozzle.
3. Be rare paniculate
will not stick to cap


| Clean probe exterior

Blow out
pilot tubes




Wash exeat
dust off probe
sheath and
nozzle

Carefully remove nozzle
and probe end cap*


Do not allow pani-
culate to be lost




Cap
probe
end


Disassemble
filter

Cap filter
inlet and
outlet


Filter mat placed in
clean, tared
weighing dish





1
Additional am
optional
1
Organic -Inori
extraction

Glass components are
scrubbed thoroughly with
acetone washings added
to tared probe wash beaker

Desiccate 24 hrs. over
16 mesh calcium
sulfate or other
anhydrous desiccant


Clean probe with nozzle
in place using acetone
and brush attached to
stainless steel or teflon
handle
 Brush entire length of
 probe with acetone 2 S
 times into marked
 container or clean,
 tared beaker
 Remove nozzle and inspect it
 and probe liner
                                                Weigh and record
              Desiccate 6 hrs.
      J
              Weigh, and record.
              Continue to constant weight—
              weights differ £ 0.5 mg
              dean probe liner again until no
              sign of particuUta can be seen in the
              acetone or on the glass
                      Clean nozzle by rinsing with acetone
                      1. Brush interior from blunt back side only.
                      2. Never force brush into sharp nozzle end;
                         bristles will be cut contaminating sample.
                                    All washings (filter glassware included)
                                    added to clean, marked, tared beaker
                                    Evaporate acetone at room temperature
                                    and pressure
                                    Desiccate and weigh to constant weight
                                    as with filler
                                                          A-18

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 5.   Clean filter equipment thoroughly.
     a.   Brush all glassware until clean.
     b.   Check with tared cotton swab.
     c.   Remove all filter mats adhering to rubber seal ring. This is
         extremely important for accurate particulate weighing.
     d.   Do not scrape glass frit into sample.
 6.   The laboratory scale accuracy and sensitivity should be checked before
     each analysis using standard weights. Actual weight and scale reading
     should agree to ± 0.5 mg.
 7.   Careful labeling of all train  components, tared beakers, and sample
     containers  avoids problems  and confusion.
 8.   Permanently marked weighing glassware with permanent record of their
     new, clean,  reference tare weight allows a check of cleanliness when
     tared just prior to use. This  can also be helpful in checking any
     weighing discrepancies in the analysis (re-tare reference periodically).
 9.   Acetone is the solvent recommended for cleaning;  however, water
     washing may be suggested by the type of pollutant sampled and should
     be added to the procedure if indicated.
10.   Adding heat to the evaporation of solvent could evaporate volatile
     materials and give erroneous data.
11.   The laboratory must have:
     a.   An analytical balance with minimum precision to 0.5 mg,
     b.   Large desiccating container that is air tight.
12.   Use only American Chemical Society Reagent grade organic solvent.
13.   Use deionized, glass-distilled H2O.
14.   Evaporate a control blank of 100 ml of each solvent used  in any part of
     the analysis in tared beaker  at room termperature and pressure.
15.   Use only glass wash bottles and glass containers  for all procedures that
     involve analytical workup. Only silica gel may be stored in plastic
     containers.
16.   Organic-inorganic extraction of the impinger may be useful in deter-
     mining emissions from some sources. Use the flowchart as a guide to
     this procedure.
                                 A-19

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                                Impinger H2O
                              Record total volume
                        Add to 500 ml separatory funnel
                    Add 50 ml anhydrous diethyl ether
                Shake 3 minutes venting ether fumes periodically
                        Let stand for separation of layers

H2<3 bottom layer separated                                 Et2O to tared beaker
Extract H2O twice again for a total
of three Et2O extractions.
Combine extracts.
H2O is then extracted three times with
50 ml chloroform (CHC13)	
                I
H2O to tared beaker                                      CHCIs + Et2O extracts
Evaporate H2O at room temperature and            Evaporate at room temperature
pressure                                                            and pressure

      17.   Procedures given here are only for cleaning Method 5 Train,
           although,  they are good general starting point procedures for cleaning
           any sampling train.
  The most important aspect of cleaning and analyzing the Method 5 Sampling
Train is the practice of good laboratory technique. The sampling team may not in-
clude an experienced chemist; therefore, good technique may have to be learned
by all team members. If an experienced analytical chemist is a member of the
sampling team it would probably be best to allow him to assist in cleaning the
equipment. This would help  to assure good  techniques and perhaps save time in
preparing samples for more extensive qualitative or quantitative analysis.


SAFETY ON SITE
Source sampling is performed at a variety of industrial sites and under many dif-
ferent conditions. Adequate safety procedures may be different for  any given situa-
tion;  however, generally accepted industrial safety procedures should be helpful to
source samplers. The test team must be aware of safe operating methods so that
alert discretion may be used for team safety at a particular sampling site. Safety is
an attitude that must be instilled in all sample team members. Well thought out
and followed procedures will  ensure the safety of all  team members. The team con-
cept essential to successful testing is vital for safe testing. It ,rust be stressed that
safety is everyone's responsibility for themselves as well as for other  team  members.
                                       A-20

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Key Factors to Good Safety
Knowledge and experience are the major factors in formulating sound safety prac
tice. An individual must draw upon these factors in determining safe methods. A
knowledge of standard safety and operating procedures will permit their applica-
tion in any situation. This basic knowledge in conjunction with understanding of
the job  tasks and possible dangers assists in planning preventive safety measures.
Plans for operating at the job site may be developed around these procedures. If an
accident does occur, the people  involved must be informed of proper emergency
practices and use of first aid. Job experience and analysis of past accidents should
be used in developing preventive safety programs.
Accident Analysis
The basic philosophy of a safety program should be that accidents are caused and,
therefore, can be avoided or prevented. Accident analysis is a productive tool of
this philosophy when it is used as a preventive step. This implies advance examina-
tion of a potentially hazardous situation to predict possible accidents and eliminate
their causes. Accident analysis is most effective when employed after an accident
has taken place.  The analysis procedure involves listing the major and con-
tributing causes of the accident. If the real causes of the accident  are analyzed in
this manner, corrective action will suggest itself.  Accident analysis should include
preventive suggestions from people involved at  the job site or those who have been
previously injured.
Common Causes of Accidents
There are a number of items that may be considered common causes of accidents:
       1.   Failure of supervisory personnel to give adequate instructions or inspec-
           tions. This includes instructions for performing the job and safety re-
           quirements. Inspection of the job site is advisable for all applicable con-
           cerns and safety before, during, and after the job.
       2.   Failure of person in charge to properly plan or conduct the activity. Ex-
           periment design and performance are  important  factors in success and
           safety of a stack test. This includes providing adequate manpower for
           the task.
       3.   Improper design, construction, or layout. Design aspects relate to equip-
           ment used and plan of operation.
       4.   Protective devices or proper tools and  equipment not provided. "Jerry
           rigging" and "making do" should only occur under unusual cir-
           cumstances, not as standard practice.
       5.   Failure on the part of any personnel to follow rules or instructions.
           Safety is the responsiblity of each individual for himself and others
           around him. Personal disregard for safety rules jeopardizes the safety of
           all.

                              A-21

-------
       6.   Neglect or improper use of protective devices, job equipment, or
           materials.
       7.   Faulty, improperly maintained devices. Poorly maintained job equip-
           ment is inexcusable.
       8.   Personnel without adequate knowledge or training for performing job.
           tasks. All present should be capable of performing the job tasks
           assigned. Trainees should be closely supervised.
       9   Personnel in poor physical condition or with a poor mental attitude for
           task. This can have implications for the attitude of personnel toward
           each other, the supervisor, the task itself, or working conditions.
      10.   Unpredictable agents outside the organization. This may mean contract
           personnel who do not abide by standard rules or something as unpredic-
           table as a biting  insect or bad weather.

Accident Prevention
Preventing accidents during a  stack test begins  with advance planning.
Knowledge of process operations and important considerations of the site
environment will give insight into chemical, mechanical, or electrical hazards
that may be present. This knowledge will be useful in deciding on equipment to
be used at  the site. Knowledge of the weather conditions and logistical con-
straints further aid in establishing a safe test program. These items in conjunc-
tion with evaluation of site safety and first aid facilities will allow preparation of
a source sampling experiment.
  The source  test  program will operate at peak efficiency and safety if plans are
properly followed. Thorough planning, including contingency actions, eliminates
the confusion  that often contributes to accidents. This planning must include
allotment of sufficient time  for completion of the task, taking into account
possible delays. Test personnel should be well informed of the program pro-
cedures; their input for test  performance and safety suggestions will be useful.
Having once established an  operating plan, all involved should adhere to it closely.
  After thorough  planning of the test program, attention focuses upon testing and
safety equipment and on site operating practices. General comments on equipment
preparation apply to both the sampling and safety apparatus. Experimental design
and personnel suggestions should indicate what  equipment will be needed on the
site for all  functions. Equipment should be prepared and assembled in advance; it
should be checked for suitable operation or potential problems.  Equipment that
could handle unexpected situations should also be included. Carry  only necessary
equipment to the site and use it properly.
  Work at the site must be  organized following standard rules and work the plan
carefully followed. Safety equipment should be used and personnel must remain
alert to any changes on the  site that could effect safe operation. All present should
be made aware of any suspected problems.
                                  A-22

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Summary

The most important factor in any safety program is common sense. Common sense
can, however, be an elusive element. Several steps presented in this section can
help in developing sensible safety practices. Thorough advance planning and
preparation for the jobs at hand begin the process of good safety practice.
Informing involved personnel of all plans and using their suggestions about work
safety increases the effectiveness of the planning. Analyzing a work situation for
hazards, including past problems, into a coherent, organized safety program,
usually results in common sense corrective procedures.
                                     A-23

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SLIDE 101-0                                       NOTES
INTRODUCTION TO
SOURCE SAMPLING
 SLIDE  101-1
    PURPOSE OF SOURCE SAMPLING
               THE AGENCY
 1. Provide data to formulate control strategy.
 2. Provide data to evaluate compliance.
 3. Provide data upon which regulations can be based.
  SLIDE 101-2

      PURPOSE OF SOURCE SAMPLING
                  INDUSTRY
  1. Provide information on process operations.
  2. Provide information on control device efficiency.
  3. Provide information for design of new process and
   control equipment.
                                    A-25

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SLIDE  101-3
NOTES
      BASIC TERMINOLOGY

         CONCENTRATION
Quantity of pollutant per quantity of effluent gas.
           grams/cubic foot
      STACK GAS FLOW RATE
  Quantity of effluent gas per length of time.
           cubic feet/hour
      POLLUTANT MASS RATE
   Quantity of pollutant per length of time.
            pounds/hour
 SLIDE 101-4
POLLUTANT MASS RATE EQUATION
       Pmrs  - Cs Qs
 SLIDE 101-5
    STACK SAMPLING FLOW DIAGRAM
0,
= A.v.
     C.   T   P
pmr.
= c.Q.
                   M
                COMPOSITION
                                   A-27

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                            SECTION B.  METHOD 1

Subject                                                                Page

1.  Method 1—sample and velocity traverses for stationary sources
    (taken from the Environmental Protection Agency Performance
    Test Methods manual)                                               B-3

2.  Slides                                                             B-15
                                      B-l

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         METHOD 1—SAMPLE AND VELOCITY TRAVERSES
                 FOR STATIONARY SOURCES
1.  Principle and Applicability
     1.1  Principle.  To aid in the representative measurement of
pollutant emissions and/or total volumetric flow rate from a
stationary source, a measurement site where the effluent stream
is flowing in a known direction is selected, and the cross-section
of the stack is divided into a number of equal areas.  A traverse
point is then located within each of these equal areas.
     1.2  Applicability.  This method is applicable to flowing gas
streams in ducts, stacks, and flues.  The method cannot be used when:
(1) flow is cyclonic or swirling (see Section 2.4), (2) a stack is
                                                              p
smaller than about 0.30 meter (12 in.) in diameter, or 0.071 m
        2
(113 in. ) in cross-sectional area, or (3) the measurement site is less
than two stack or duct diameters downstream or less than a half
diameter upstream from a flow disturbance.
     The requirements of this method must be considered before con-
struction of a new facility from which emissions will be measured;
failure to do so may require subsequent alterations to the stack or
deviation from the standard procedure.  Cases involving variants are
subject to approval by the Administrator, U.S. Environmental Protection
Agency.
2.  Procedure
     2.1  Selection of Measurement Site.   Sampling or velocity measure-
ment is performed at a site located at least eight stack or duct
                              B-3

-------
diameters downstream and two diameters upstream from any flow
disturbance such as a bend, expansion, or contraction in the stack,
or from a visible flame.  If necessary, an alternative location may
be selected, at a position at least two stack or duct diameters
downstream and a half diameter upstream from any flow disturbance.
For a rectangular cross section, an equivalent diameter (De) shall
be calculated from the following equation, to determine the upstream
and downstream distances:
          n   -   2LM
          De  "  "HTw
where L  = length and W = width.
     2.2 Determining the Number of Traverse Points.
     2.2.1  Particulate Traverses.  When the eight- and two-diameter
 criterion can be met, the minimum number of traverse points shall be:
 (1)  twelve, for circular or  rectangular stacks with diameters (or
 equivalent diameters) greater than 0.61 meter  (24 in.); (2) eight,
 for  circular stacks with diameters between 0.30 and 0.61 meter
 (12-24  in.); and  (3)  nine,  for  rectangular stacks with equivalent
 diameters  between  0.30  and  0.61 meter (12-24 in.).
     When  the  eight-  and  two-diameter criterion cannot be met, the
 minimum number of  traverse  points  is  determined from Figure 1-1.
 Before  referring  to the figure, however,  determine  the distances  from
 the  chosen measurement site to  the nearest upstream and downstream
 disturbances,  and  divide  each distance by the  stack diameter or
 equivalent diameter, to determine  the distance in terms of  the number
 of duct diameters.  Then, determine  from Figure 1-1 the minimum  number
                          B-4

-------
en

en
             0.5
            50
         V)
            40
o
a.

UJ

cc
UJ

>  30
         O

         oc
            20
         S  10
            DUCT DIAMETERS UPSTREAM FROM FLOW DISTURBANCE (DISTANCE A}



                       1.0                 1.5                 2.0
                  * FROM POINT OF ANY TYPE OF

                    DISTURBANCE (BEND, EXPANSION. CONTRACTION. ETC.
                                           I
25
                                                                                 I
Y
T
A

-
*
\

-

5
1
—




1
1
4
'DISTURBANCE

MEASUREMENT
:- SITE


DISTURBANCE
                                                                                I
                       3456789


                   DUCT DIAMETERS DOWNSTREAM FROM FLOW DISTURBANCE (DISTANCE B)



                    Figure 1-1. Minimum number of traverse points for particulate traverses.
                                                                                10

-------
of traverse points that corresponds:  (1) to the number of duct
diameters upstream; and (2) to the number of diameters downstream.
Select the higher of the two minimum numbers of traverse points, or
a greater value, so that for circular stacks the number is a
multiple of 4, and for rectangular stacks, the number is one of those
shown  in Table 1-1.
   Table 1-1.  CROSS-SECTIONAL LAYOUT FOR RECTANGULAR STACKS
               No. of traverse          Matrix
                   points               layout
                     9                   3x3
                     12                   4x3
                     16                   4x4
                     20                   5x4
                     25                   5x5
                     30                   6x5
                     36                   6x6
                     42                   7x6
                     49                   7x7
      2.2.2  Velocity (Non-Particulate)  Traverses.   When  velocity  or
 volumetric flow rate is to be determined (but not  particulate  matter),
 the same procedure as that for particulate traverses  (Section  2.2.1)
 is followed, except that Figure 1-2 may be used instead  of Figure 1-1.
      2.3  Cross-Sectional  Layout and Location of Traverse Points.
      2.3.1  Circular Stacks.  Locate the traverse  points on two perpendi
 cular diameters according to Table 1-2 and the  example shown in
 Figure 1-3.  Any equation (for examples, see Citations 2 and 3 in the
                              B-6

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D3
 I
             05
DUCT DIAMETERS UPSTREAM FROM FLOW DISTURBANCE (DISTANCE A)


             1.0                 1.5                 2.0
           50
           40
         O
         a.

         LLJ
         V)
         oc
         UJ
         O
         oc
         D


         S
         D
         5
           30
            20
         ?  10
                       T
                                           I
                       _L
25
\
J
A

"•
f


3
i
i
i
—



|
1


fc
'DISTURBANCE

MEASUREMENT
"-- SITE



DISTURBANCE
              2         3         4         5         6         78         9

                  DUCT DIAMETERS DOWNSTREAM FROM FLOW DISTURBANCE (DISTANCE B)
                                                                       10
               Figure 1-2. Minimum number of traverse points for velocity (nonparticulate) traverses.

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TRAVERSE
  POINT

    1
    2
    3
    4
    5
    6
 DISTANCE.
% of diameter

     4.4
    14.7
    29.5
    70.5
    85.3
    95.6
             Figure 1-3.  Example showing circular stack cross section divided into
             12 equal areas, with location of traverse points indicated.
                                  B-8

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Table 1-2. LOCATION OF TRAVERSE POINTS IN CIRCULAR STACKS
      (Percent of stack diameter from inside wall to traverse point)
Traverse
point
number
on a
diameter
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
Number of traverse points on a diameter
2
14.6
85.4






















4
6.7
25.0
75.0
93.3




















6
4.4
14.6
29.6
70.4
85.4
95.6


















8
3.2
10.5
19.4
32.3
67.7
80.6
89.5
96.8
















10
2.6
8.2
14.6
22.6
34.2
65.8
77.4
85.4
91.8
97.4














12
2.1
6.7
11.8
17.7
25.0
35.6
64.4
75.0
82.3
88.2
93.3
97.9












14
1.8
5.7
9.9
14.6
20.1
26.9
36.6
63.4
73.1
79.9
85.4
90.1
94.3
98.2










16
1.6
4.9
8.5
12.5
16.9
22.0
28.3
37.5
62.5
71.7
78.0
83.1
87.5
91.5
95'. 1
98.4








18
1.4
4.4
7.5
10.9
14.6
18.8
23.6
29.6
38.2
61.8
70.4
76.4
31.2
85.4
89.1
92.5
95.6
98.6






20
1.3
3.9
6.7
9.7
12.9
16.5
20.4
25.0
30.6
38.8
61.2
69.4
75.0
79.6
83.5
87.1
90.3
93.3
96.1
98.7




22
1.1
3.5
6.0
8.7
11.6
14.6
18.0
21.8
26.2
31.5
39.3
60.7
68.5
73.8
78.2
82.0
85.4
88.4
91.3
94.0
96.5
98.9


24
1.1
3.2
5.5
7.9
10.5
13.2
16.1
19.4
23.0
27.2
32.3
39.8
60.2
67.7
72.8
77.0
80.6
83.9
86.8
89.5
92.1
94.5
96.8
98.9
                           B-9

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Bibliography) that gives the same values as those in Table 1-2 may
be used in lieu of Table 1-2.
     For particulate traverses, one of the diameters must be in a plane
containing the greatest expected concentration variation, e.g., after
bends, one diameter shall be in the plane of the bend.  This requirement
becomes less critical as the distance from the disturbance increases;
therefore, other diameter locations may be used, subject to approval of
the Administrator.
     In addition, for stacks having diameters greater than 0.61 m
(24 in.) no  traverse points shall be located within 2.5 centimeters
(1.00  in.) of the stack walls; and for stack diameters equal to or less
than 0.61 m  (24 in.), no traverse points shall be located within 1.3 cm
(0.50  in.) of the stack walls.  To meet these criteria, observe the
procedures given below.
     2.3.1.1  Stacks With Diameters Greater Than 0.61 m (24 in.).  When
any of the traverse points as  located  in Section 2.3.1 fall within
2.5 cm (1.00 in.) of the stack walls,  relocate them away from the
stack  walls  to:  (1) a distance of 2.5 cm  (1.00 in.); or (2) a distance
equal  to the nozzle inside diameter, whichever is larger.  These
relocated traverse points  (on  each end of  a diameter) shall be the
"adjusted" traverse points.
     Whenever two successive traverse  points are combined to form a
single adjusted traverse point, treat  the  adjusted point as two
separate traverse points,  both in the  sampling (or velocity measure-
ment)  procedure, and  in  recording the  data.
                           B-10

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     2.3.1.2  Stacks With Diameters Equal to or Less Than 0.61 m (24
in.).  Follow the procedure in Section 2.3.1.1, noting only that any
"adjusted" points should be relocated away from the stack walls to:
(1) a distance of 1.3 cm (0.50 in.); or (2) a distance equal to the
nozzle inside diameter, whichever is larger.
     2.3.2  Rectangular Stacks.  Determine the number of traverse points
as explained in Sections 2.1 and 2.2 of this method.  From Table 1-1,
determine the grid configuration.  Divide the stack cross-section into as
many equal rectangular elemental areas as traverse points, and then
locate a traverse point at the centroid of each equal area according to
the example in Figure 1-4.
     If the tester desires to use more than the minimum number of
traverse points, expand the "minimum number of traverse points" matrix
(see Table 1-1) by adding the extra traverse points along one or the
other or both legs of the  matrix; the final matrix need not be balanced.
For example, if a 4 x 3 "minimum number of points" matrix were expanded
to 36 points, the final matrix could be9x4or!2x3, and would not
necessarily have to be 6 x 6.  After constructing the final matrix,
divide the stack cross-section into as many equal rectangular, elemental
areas as traverse points, and locate a traverse point at the centroid of
each equal area.
     The situation of traverse points being too close to the stack walls
is not expected to arise with rectangular stacks.  If this problem
should ever arise, the Administrator must be contacted for resolution of
the matter.
                             B-ll

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               	I	[__
                  o    '   o        o
                       I
                               I
Figure 1 -4.  Example showing rectangular stack cross
section divided into 12 equal areas, with a traverse
point at centroid of each area.
                 B-12

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     2.4  Verification of Absence of Cyclohic Flow.  In most stationary
sources, the direction of stack gas flow is essentially parallel to the
stack walls.  However, cyclonic flow may exist (1) after such devices as
cyclones and inertial demisters fbllowing venturi scrubbers, or (2) in
stacks having tangential inlets or other duct configurations which tend
to induce swirling; in these instances, the presence or absence of
cyclonic flow at the sampling location must be determined. The following
techniques are acceptable for this determination.
     Level and zero the manometer.  Connect a Type S pi tot tube to the
manometer.  Position the Type S pi.tot tube at each traverse point, in
succession, so that the planes of the face openings of the pi tot tube
are perpendicular to the stack cross-sectional plane: when the Type S
pitot tube is in this position, it is at "0° reference."  Note the
differential pressure (Ap) reading at each traverse point.  If a null
(zero) pitot reading is obtained at 0° reference at a given traverse
point, an acceptable flow condition exists at that point.  If the pitot
reading is not zero at 0° reference, rotate the pitot tube (up to +90°
yaw angle), until a null reading is obtained.  Carefully determine and
record the value of the rotation angle (a) to the nearest degree.  After
the null technique has been applied at each traverse point, calculate
the average of the absolute values of o; assign a values of 0° to those
points for which no rotation was required, and include these in the
overall average.  If the average value of a is greater than 10°, the
overall flow condition in the stack is unacceptable and alternative
methodology, subject to the approval of the Administrator, must be used
to perform accurate sample and velocity traverses.
                            B-13

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3.  Bibliography
     1.  Determining  Dust Concentration in a Gas Stream.  ASME.  Per-
formance Test Code  No.  27.  New York.  1957.
     2.  Devorkin,  Howard, et al.  Air Pollution Source Testing  Manual.
Air Pollution Control District.  Los Angeles, CA.  .November 1963.
     3.  Methods  for  Determination of Velocity, Volume, Dust and Mist
Content of Gases.   Western Precipitation Division of Joy Manufacturing
Co.  Los Angeles, CA.   Bulletin WP-50.  1968.
     4.  Standard Method for Sampling Stacks for Particulate Matter.  In:
1971 Book of ASTM Standards, Part 23.  ASTM Designation D-2928-71.
Philadelphia, PA.   1971.
     5.  Hanson, H. A., et al.  Participate Sampling Strategies  for
Large Power Plants  Including Nonuniform Flow.  USEPA, ORD, ESRL, Research
Triangle Park, N.C.   EPA-600/2-76-170.  June 1976.
     6.  Entropy Environmentalists, Inc.  Determination of the Optimum
Number of Sampling  Points:  An.Analysis of Method 1 Criteria. Environmental
Protection Agency.  Reserch Triangle Park, N. C. EPA Contract No. 68-01-317
Task 7.
                          B-14

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SLIDE 102-0
NOTES
      METHOD — 1
Sample and Velocity Traverses
   for Stationary Sources
 SLIDE  102-1


        CRITERIA FOR SELECTION OF
             MEASUREMENT SITE
 • Effluent stream must be flowing in a known direction.
 • Ideally, site should be at least eight stack  diameters
   downstream and two diameters  upstream from any
   flow disturbance.
 • Alternatively, site must be located at a minimum of two
   stack diameters downstream and one-half diameter
   upstream from any flow disturbance.


 SLIDE 102-2

 UPSTREAM AND DOWNSTREAM FLOW DISTURBANCES
                         DISTURBANCE
          UPSTREAM
          DISTANCE
         DOWNSTREAM
          DISTANCE
                                       B-15

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SLIDE  102-3
                                                               NOTES
       EXAMPLE FOR CIRCULAR STACKS
Inside of far wall to outside of nipple (distance 1)
Inside of near wall to outside of nipple (distance 2)  =
Stack ID (distance 1 - distance 2)
Nearest upstream disturbance (distance A)
Nearest downstream disturbance (distance B)
                   CALCULATION
            74" (distance A) -f- 36" (stack ID) = 2
           288" (distance B) -~ 36" (stack ID) = 8
 39"
  3"
 36"
 74"
288"
SLIDE  102-4

              MINIMUM NUMBER OF TRAVERSE POINTS
  0.5
  501—
              DUCT DIAMETERS UPSTREAM FROM FlOW DISTURBANCE (DISTANCE Al
                 10             1.5             2.0
                                                            2.5
                      -USE FOR PARTICULATE

                      • USE FOR NONPARTICULATE
\ 7 DISTURBANCE
II
1
,
I


i
1


J
*

^

	 	 SAMPLING
SITE

DISTURBANCE
&
          3      4       5       6       7       B       9
             DUCT DIAMETERS DOWNSTREAM FROM FLOW DISTURBANCE (DISTANCE Bl
                                           B-17

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SLIDE 102-5
                                             NOTES
        LOCATION OF TRAVERSE POINTS
    AS A PERCENTAGE OF STACK DIAMETER
Traverse
point
number
on a
diameter 2
1 14.6
2 85.4
3
4
5
6
7
8
9
10
11
12
Number of traverse points
on a diameter

4
6.7
25.0
75.0
93.3









6
4.4
14.6
29.6
70.4
85.4
95.6







8
3.2
10.5
19.4
32.3
67.7
80.6
89.5
96.8





10
2.6
8.2
14.6
22.6
34.2
65.8
77.4
85.4
91.8
97.4



12
2.1
6.7
11.8
17.7
25.0
35.6
64.4
75.0
82.3
88.2
93.3
97.9
 SLIDE  102-6
  MEASURED LOCATIONS OF TRAVERSE POINTS
             (CIRCULAR STACK)
TRAVERSE
 POINT
   1
   2
   3
   4
   5
   6
          DISTANCE
DIAMETER
  4.4
  14.7
  29.5
  70.5
  85.3
  95.6
                                B-19

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 SLIDE 102-7                                          NOTES


CRITERIA FOR LOCATING SAMPLE POINTS IN
              CIRCULAR STACKS
 • One diameter must be in a plane containing greatest
   expected concentration variation, for particulate
   traverses.
 • No traverse point shall be located within 2.5 cm (1.0 in.)
   of stack wall for stacks greater than 0.61 m (24 in.) in
   diameter.
 • No traverse point shall be located within 1.3 cm
   (0.50 in.) of stack wall for stacks with diameters < 0.61 m
   (24 in.).
 SLIDE 102-8


(cont.)

       • Relocated traverse points shall be defined as
        "adjusted" traverse points.
       • When two traverse points are combined to form
        a single adjusted traverse point, treat adjusted
        point as two points.
 SLIDE 102-9
         BALANCED MATRIX SCHEME FOR
               RECTANGULAR STACKS
                 Number of      Matrix
               Traverse Points    Layout
9
12
16
20
25
30
36
42
49
3x3
4x3
4x4
5x4
5x5
6x5
6x6
7x6
7x7
                                      B-21

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SLIDE  102-10
                                NOTES
 EXAMPLE FOR RECTANGULAR STACKS
 Dimensions:
 Length of stack (L) (- wall thickness)         =  36"
 Width of stack (W) (- wall thickness)         -  36"
 Equivalent Diameter (De)
        De  -
               2LW
36x36
        = 36"
               L + W      36 + 36
 Nipple Length
 Nearest upstream disturbance (distance A)
 Nearest downstream disturbance (distance B)
 74" (distance A) -^ 36" {stack De)
 288" (distance B) -^ 36" (stack De)
              =   0
              =  74"
              = 288"
              =   2
              =   8
 SLIDE 102-11
TRAVERSE POINT LOCATIONS (RECTANGULAR STACK)
                                        B-23

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SLIDE 102-12                                      NOTES


       MEASURED LOCATIONS OF
           TRAVERSE POINTS
        (RECTANGULAR STACK)


 Point  Length of nipple   Distance X   Distance Y
  1-1         0            4.5"          6"
  1-2         0            4.5"         18"
  1-3         0            4.5"         30"
  2-1         0           13.5"          6"
  2-2         0           13.5"         18"
  2-3         0           13.5"         30"
  3-1         0           22.5"          6"
  3-2         0           22.5"         18"
  3-3         0           22.5"         30"
  4-1         0           31.5"          6"
  4-2         0           31.5"         18"
  4-3         0           31.5"         30"
SLIDE 102-13


          NON PARALLEL FLOW
  Presence or absence of non parallel flow must
  be determined after:
       •  Cyclones
       •  Inertial Demisters
       •  Stacks Having Tangential Inlets
SLIDE 102-14

     VERIFY SUITABILITY OF SITE

1. Calculate absolute value of«.
2. If average value of <* is > 10°, flow condi-
  tions are unacceptable.
                                   B-25

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                            SECTION C.  METHOD 2

Subject                                                               Page

1.   Method 2--determination of stack gas velocity and volumetric
    flow rate (Type S pi tot tube) (taken from the Environmental
    Protection Agency Performance Test Methods manual)                C-3

2.   Slides                                                            C-35
                                     C-l

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    METHOD 2—DETERMINATION OF STACK GAS VELOCITY AND
         VOLUMETRIC FLOW RATE (TYPE S PITOT TUBE)

1.  Principle and Applicability
     1.1  Principle.  The average gas velocity in a stack is
determined from the gas density and from measurement of the average
velocity head with a Type S (Stausscheibe or reverse type) pi tot tube.
     1.2  Applicability.  This method is applicable for measurement
of the average velocity of a gas stream and for quantifying gas flow.
     This procedure is not applicable at measurement sites which fail
to meet the criteria of Method 1, Section 2.1.  Also, the method cannot
be used for direct measurement in cyclonic or swirling gas streams;
Section 2.4 of Method 1 shows how to determine cyclonic or swirling
flow conditions.  When unacceptable conditions exist, alternative
procedures, subject to the approval of the Administrator, U. S.
Environmental Protection Agency, must be employed to make accurate
flow rate determinations; examples of such alternative procedures are:
(1) to  install straightening vanes;  (2) to calculate the total volumetric
flow rate stoichiometrically, or (3) to move to  another measurement
site at which the flow is acceptable.
2.  Apparatus
     Specifications for the apparatus are  given  below.  Any other
apparatus that has  been demonstrated  (subject to approval of the
Administrator) to be capable of meeting the specifications will be
considered acceptable.
     2.1  Type S Pitot Tube.  The Type  S pitot tube  (Figure 2-1) shall
be made of metal tubing  (e.g., stainless steel).   It is recommended
that the  external tubing diameter  (dimension D., Figure 2-2b)  be
                                              t
                            C-3

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1.90 2.54cm*
(0 75 1.0 in.)
                         ^A'^-.-j. . ..b —I
           	
           rmfm*.~A:,wj--,lTLr

             7.62 cm (3 in.)*
                             TEMPERATURE SENSOR
                              TYPE SPITOTTUBE
            'SUGGESTED (INTERFERENCE FREE)
             PITOT TUBE  THERMOCOUPLE SPACING
                                                              LEAK-FREE
                                                             CONNECTIONS
                                              MANOMETER
                        Figure 2-1.  Type S pitot tube manometer assembly.
                                       C-4

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between 0.48 and 0.95 centimeters (3/16 and 3/8 inch).  There shall
be an equal distance from the base of each leg of the pitot tube to
its face-opening plane (dimensions P. and PB, Figure 2-2b); it is
recommended that this distance be between 1.05 and 1.50 times the
external tubing diameter.  The face openings of the pi tot tube shall,
preferably, be aligned as shown in Figure 2-2; however, slight mis-
alignments of the openings are permissible (see Figure 2-3).
     The Type S pi tot tube shall have a known coefficient, determined
as outlined in Section 4.  An identification number shall be assigned
to the pitot tube; this  number shall be permanently marked or
engraved on the body of  the  tube.
     A standard pitot tube may be used instead of a Type S, provided
that it meets the specifications of Sections 2.7 and  4.2; note, however,
that the static and  impact pressure holes of standard pitot tubes are
susceptible to plugging  in particulate-laden gas streams.  Therefore,
whenever a standard  pitot tube is used to perform a traverse, adequate
proof must be furnished  that the openings of the pitot  tube have not
plugged up during the traverse period; this can be done by  taking a
velocity head  (AP)  reading at the final  traverse point, cleaning out
the  impact and static holes  of the  standard pitot tube  by  "back-
purging" with pressurized air, and  then  taking another  AP  reading.
If the  Ap  readings  made  before and  after  the air purge  are  the  same
(+5  percent), the traverse  is acceptable.  Otherwise, reject  the run.
Note that  if Ap  at  the  final traverse  point is unsuitably  low,
another point may be selected.   If  "back-purging" at  regular  intervals
                              C-5

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   TRANSVERSE
    TUBE AXIS
             \
                         FACE
                       OPENING
                        PLANES

                          (a)
                         A SIDE PLANE
LONGITUDINAL '
TUBE AXIS
7 Dt A
S * B
                                         PA

                                         PB
NOTE:

1.05 Dt < P<1.50Dt
                         B SIDE PLANE

                           (b)
                        A ORB
                           (c)
Figure 2-2.  Properly constructed Type S pilot tube, shown
in:  (a) end view; face opening planes perpendicular to trans-
verse axis; (b) top view; face opening planes parallel to lon-
gitudinal axis; (c) side view; both legs of equal length and
center lines coincident, when viewed from both sides. Base-
line coefficient values of 0.84 may be assigned to pitot tubes
constructed this way.
                      C-6

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       TRANSVERSE
        TUBE AXIS
                                  (a)
LONGITUDINAL
 TUBE AXIS —
                        (c)
                                                   9
                                                                FLOW
(d)
                                                                          01W
                          •-4E
                                             (e)
                                             (f)
                                             (g)

           Figure 2-3. Types of face-opening misalignment that can result from field use or im-
           proper construction of Type S pitot tubes. These will not affect the baseline value
           of Cp(s) so long as ai anda2< 10°, 01 and 02 < 5°, z< 0.32 cm (1/8 in.) and w <
           0.08 cm (1/32 in.) (citation 11 in Section 6).
                                   C-7

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is part of the procedure, then comparative Ap readings shall be taken,
as above, for the last two back purges at which suitably high Ap
readings are observed.
     2.2  Differential Pressure Gauge.  An inclined manometer or
equivalent device is used.  Most sampling trains are equipped with
a 10-in. (water  column) inclined-vertical manometer,-having 0.01-in.
HgO divisions on the 0- to 1-in. inclined scale, and 0.1-in. HgO
divisions on the 1- to 10-in. vertical scale.  This type of manometer
(or other gauge  of equivalent sensitivity) is satisfactory for the
measurement of Ap values  as low as  1.3 mm (0.05 in.) H^O.  However, a
differential pressure gauge of greater sensitivity shall be used
(subject to the  approval  of the Administrator), if any of the following is
found to be true:   (1) the arithmetic average of all Ap readings at
the traverse points in the stack is  less than 1.3 mm (0.05 in.) hLO;
(2) for traverses of 12 or more points, more than 10 percent of the
individual Ap readings are below 1.3 mm (0.05 in.) hLO; (3) for traverses
of fewer than 12 points,  more than  one Ap reading is below 1.3 mm
(0.05 in.) H20.  Citation 18 in Section 6 describes commercially
available instrumentation for the measurement of low-range gas velocities.
     As an alternative to criteria  (1) through  (3) above, the following
calculation may  be performed to determine the necessity of using a more
sensitive differential pressure gauge:
                  n
          T  m
                   Z     /Ap~
                 1  =  1      1
where:
     Ap. =  Individual  velocity head  reading  at a  traverse point,
           mm H2°  (in-  H2°)     C-8

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     n   = Total number of traverse points
     K   = 0.13 mm H20 when metric units are used and 0.005 in.  H^O
           when English units are used
If T is greater than 1.05, the velocity head data are unacceptable
and a more sensitive differential pressure gauge must be used.
     Note:  If differential pressure gauges other than inclined
manometers are used (e.g., magnehelic gauges), their calibration
must be checked after each test series.  To check the calibration
of a differential pressure gauge, compare Ap readings of the gauge
with those of a gauge-oil manometer at a minimum of three points,
approximately representing the range of Ap values in the stack.   If,
at each point, the values of Ap as read by the differential pressure
gauge and gauge-oil manometer agree to within 5 percent, the differential
pressure gauge shall be considered to be in proper calibration.   Other-
wise, the test series shall either be voided, or procedures to adjust
the measured Ap values and final results shall be used, subject  to the
approval of the Administrator.
     2.3  Temperature Gauge.  A thermocouple, liquid-filled bulb
thermometer, bimetallic thermometer, mercury-in-glass thermometer, or
other gauge capable of measuring temperature to within 1.5 percent of
the minimum absolute stack temperature shall be used.  The temperature
gauge shall be attached to the pi tot tube such that the sensor tip does not
touch any metal; the gauge shall be in an interference-free arrangement
with respect to the pitot tube face openings (see Figure 2-1 and also
Figure 2-7 in Section 4).  Alternate positions may be used if the pitot
tube-temperature gauge system is calibrated according to the procedure
                              C-9

-------
of Section 4.  Provided that a difference of not more than 1 percent
in the average velocity measurement is introduced, the temperature
gauge need not.be attached to the pitot tube; this alternative is
subject to the approval of the Administrator.
     2.4  Pressure  Probe  and Gauge.  A piezometer tube and mercury-
or water-filled U-tube manometer capable of measuring stack pressure
to within 2.5 mm  (0.1 in.) Hg is used.  The static tap of a standard
type pitot tube or  one leg of a Type S pitot tube with the face opening
planes positioned parallel to the gas flow may  also  be used as the
pressure  probe.
     2.5  Barometer.  A  mercury, aneroid, or other barometer capable
of measuring atmospheric pressure to within 2.5 mm Hg  (0.1 in. Hg) may
be used.   In many cases, the barometric reading may  be obtained from
a nearby  national weather service station,  in which  case the station
value  (which is  the absolute barometric pressure) shall be requested
and  an adjustment for elevation  differences between  the weather station
and  the sampling point shall be  applied at  a  rate of minus 2.5 mm
 (0.1  in.) Hg per 30 meter (100 foot)  elevation  increase, or vice-versa
for  elevation decrease.
      2.6  Gas Density Determination Equipment.   Method  3 equipment, if
needed (see Section 3.6), to determine the  stack gas dry molecular
weight, and Reference Method 4 or Method  5  equipment for moisture content
determination; other methods may be used  subject to  approval of the
Administrator.
      2.7  Calibration Pitot Tube.   When calibration  of the Type S pitot
tube is necessary  (see Section 4), a standard pitot  tube is used as a
reference.  The standard pitot tube shall,  preferably,  have a known
                                  C-lo

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coefficient, obtained either (1) directly from the National Bureau
of Standards, Route  270,  Quince Orchard Road, Gaithersburg,
Maryland, or (2)-by calibration against another standard pitot tube
with an NBS-traceable coefficient.  Alternatively, a standard pitot
tube designed according to the criteria given in 2.7.1 through 2.7.5
below and illustrated in Figure 2-4 (see also Citations 7, 8, and 17
in Section 6) may be used.  Pitot tubes designed according to these
specifications will have baseline coefficients of about 0/99 j^O.Ol.
     2.7.1  Hemispherical (shown in Figure 2-4), ellipsoidal, or
conical tip.
     2.7.2  A minimum of six diameters straight run (based upon D, the
external diameter of the tube) between the tip and the static pressure
holes.
     2.7.3  A minimum of eight diameters straight run between the static
pressure holes and the centerline of the external tubei following the
90 degree bend.
     2.7.4  Static pressure holes of equal size (approximately 0.1 D),
equally spaced in a piezometer ring configuration.
     2.7.5  Ninety degree bend, with curved or mitered junction.
     2.8  Differential Pressure Gauge for Type S Pitot Tube Calibration.
An inclined manometer or equivalent is used.  If the single-velocity
calibration technique is employed (see Section 4.1.2.3), the calibration
differential pressure gauge shall be readable to the nearest 0.13 mm
HpO (0.005 in. HpO).  For multivelocity calibrations, the gauge shall  be
readable to the nearest 0.13 mm H20 (0.005 in H20) for Ap values between 1.3
and 25 mm H20 (0.05 and 1.0 in. H20), and to the nearest 1.3 mm H20
(0.05 in. H20) for Ap values above 25 mm H20 (1.0 in.  H20).  A special,  more
sensitive gauge will be required to read Ap values below 1.3 mm H20' [0.05
in. H20](see Citation 18 in Section 6).
                                       C-ll

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                     c=Q
o
i—•
ro
T
                                                          CURVED OR
                                                        MITERED JUNCTION
                                                           HEMISPHERICAL
                                                                TIP
                            Figure 2-4. Standard pitot tube design specifications.

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3.  Procedure
     3.1  Set up the apparatus as shown in Figure 2-1.  Capillary
tubing or surge tanks installed between the manometer and pitot tube
may be used to dampen Ap fluctuations.  It is recommended, but not
required, that a pretest leak-check be conducted, as follows:   (1) blow
through the pi tot impact opening until at least 7:6 cm (3 in.)
H20 velocity pressure registers on the manometer; then, close off the
impact opening.  The pressure shall remain stable for at least 15
seconds; (2) do the same for the static .pressure side, except using
suction to obtain the minimum of 7.6 cm (3 in.) H20.  Other leak-check
procedures, subject to the approval of the Administrator, may be used.
     3.2  Level and zero the manometer.  Because the manometer level
and zero may drift due to vibrations and temperature changes, make
periodic checks during the traverse.  Record all necessary data as
shown in the example data sheet  (Figure 2-5).
     3.3  Measure the velocity head and temperature at the traverse
points  specified by Method 1.  Ensure that the proper differential
pressure gauge is being used for the range of Ap values encountered
(see Section 2.2).  If it is necessary to change to a more sensitive
gauge,  do so, and remeasure the Ap and temperature readings at each
traverse point.  Conduct a post-test leak-check  (mandatory), as
described in Section 3.1 above,  to validate the  traverse  run.
     3.4  Measure the static pressure in the stack.  One  reading  is
usually adequate.
     3.5  Determine the atmospheric pressure.
     3.6  Determine the stack gas dry molecular weight.   For combustion
processes or processes that emit essentially C02> 02, CO, and N2> use
                              C-13

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PLANT
DATE .
RUN NO.
STACK DIAMETER OR DIMENSIONS, m(in.)
BAROMETRIC PRESSURE, mm Hg (in. Hg)_
CROSS SECTIONAL AREA. m2(ft2)	
OPERATORS 	
PITOTTUBEI.D.NO.
  AVG. COEFFICIENT, Cp =
  LAST DATE CALIBRATED.
                             SCHEMATIC OF STACK
                                CROSS SECTION
   Traverse
    Pt.No.
mm (in.) H20
                                  Stack Temperature
      ts. °C
T. °K
mm Hg (in.Hg)
                                  Avenge
                      Figure 2-5. Velocity traverse data.
                                     C-14

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Method 3.  For processes emitting essentially air, an analysis need
not be conducted; use a dry molecular weight of 29.0.  For other processes,
other methods,-subject to the approval of the Administrator, must be used.
     3.7  Obtain the moisture content from Reference Method 4 (or
equivalent.) or from Method 5.
     3.8  Determine the cross-sectional area of the stack or duct at
the sampling location.  Whenever possible, physically measure the stack
dimensions rather than using blueprints.
4.  Calibration
     4.1  Type S  Pitot Tube.  Before its initial use, carefully examine
the Type S pitot tube in top, side, and end views to verify that the face
openings of the tube are aligned within the specifications illustrated in
Figure 2-2 or 2-3.  The pitot tube shall not be used if  it fails to meet
these alignment specifications.
     After verifying the face opening alignment, measure and record the
following dimensions of the pitot tube:  (a) the external tubing diameter
(dimension D., Figure 2-2b); and (b) the base-to-opening plane distances
(dimensions P. and Pg, Figure 2-2b).  If D. is between 0.48 and 0.95 cm
(3/16 and 3/8 in.), and if P. and P- are equal and between 1.05 and 1.50
Dt, there are two possible options:   (1) the pitot tube  may be cali-
brated according to the procedure outlined in Sections 4.1.2 through
4.1.5 below, or  (2) a baseline  (isolated tube) coefficient value of
0.84 may be assigned to the pitot tube.  Note, however,  that if the
pitot tube is part of an assembly, calibration may still be required,
despite  knowledge of the baseline coefficient value  (see Section 4.1.1).
     If  Dt, P.,  and PB are outside the specified limits, the pitot tube
must be  calibrated as outlined  in 4.1.2  through 4.1.5 below.
                              C-15

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     4.1.1  Type S Pitot Tube Assemblies.  During sample and velocity
traverses, the isolated Type S pitot tube is not always used; in many
instances, the pitot tube is used in combination with other source-
sampling components (thermocouple, sampling probe, nozzle) as part
of an "assembly."  The presence of other sampling components can
sometimes affect the baseline value of the Type S pitot tube
coefficient  (Citation 9 in Section 6); therefore an assigned (or
otherwise known) baseline coefficient value may or may not be valid
for  a given  assembly.  The baseline and  assembly coefficient values
will be  identical only when the relative placement of the components
in the assembly  is such that aerodynamic interference effects are
eliminated.   Figures 2-6 through  2-8 illustrate interference-free
component arrangements for Type S pitot  tubes  having external tubing
diameters between 0.48 and 0.95 cm  (3/16 and 3/8 in.).   Type S pitot
tube assemblies  that fail to meet any or all of the specifications of
Figures  2-6 through 2-8 shall  be  calibrated according to the procedure
outlined in Sections 4.1.2  through  4.1.5 below,  and prior to calibra-
tion,  the values of the  intercomponent  spacings  (pitot-nozzle, pitot-
thermocouple, pitot-probe  sheath) shall  be measured and recorded.
     Note:   Do not use any Type S pitot tube  assembly which  is
constructed such that the impact pressure  opening  plane of  the pitot
tube is  below the entry plane of the nozzle (see Figure 2-6b).
     4.1.2   Calibration Setup.   If the Type S pitot tube  is  to be
calibrated, one leg of the tube  shall  be permanently marked  A, and the
other,  B.  Calibration shall be done in a flow system  having the follow-
 ing  essential design features:
      4.1.2.1  The flowing gas stream must be confined  to  a  duct of
 definite cross-sectional  area, either circular or  rectangular.  For
                              C-16

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                          TYPE SPITOT TUBE
                                      I
                          > 1.90 cm (3/4 in.) FOR Dn • 1.3 cm (1/2 in.)
             SAMPLING NOZZLE
        A.  BOTTOM VIEW; SHOWING MINIMUM PITOT-NOZZLE SEPARATION.
SAMPLING
 PROBE
              SAMPLING
               NOZZLE
                              NOZZLE ENTRY
                                  PLANE
STATIC PRESSURE
 OPENING PLANE
                                                               IMPACT PRESSURE
                                                                OPENING PLANE
           6.
SIDE VIEW; TO PREVENT PtTOT TUBE
FROM INTERFERING WITH GAS FLOW
STREAMLINES APPROACHING THE
NOZZLE THE IMPACT PRESSURE
OPENING PLANE OF THE PITOT TUBE
SHALL BE EVEN WITH OR ABOVE THE
NOZZLE ENTRY PLANE.
       Figure 2-6.  Proper pitot tube -  sampling nozzle configuration to present
       aerodynamic interference; buttonhook - type nozzle; centers of nozzle
       and pitot opening aligned; Dt between 0.48 and 0.95 cm (3/16 and
       3/8 in.).
                               C-17

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                      THERMOCOUPLE
                                                                                                         Z ^5.08 cm

                                                                                                         ' (2 in.)
co
         THERMOCOUPLE
                                                  1.90 cm (3/4 in.)
                                                    i,
                          TYPE SPITOT TUBE
                                                             OR
s
a
               TYPE SPITOT TUBE
         SAMPLE PROBE
  SAMPLE PROBE
                                Figure 2-7.  Proper thermocouple placement to prevent interference;
                                Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).

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o

t—•
',-0
TYPE SPITOTTUBE
                                              SAMPLE PROBE
          .62 cm (3 in.)
                    Figure 28.  Minimum pitot sample probe separation needed to prevent interference;
                    Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).

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circular cross-sections, the minimum duct diameter shall be 30.5 cm
(12 inO; for rectangular cross-sections, the width (shorter side)
shall be at least 25.4 cm (10 in.).
     4.1.2.2  The cross-sectional area of the calibration duct must
be constant over a distance of 10 or more duct diameters.  For a
rectangular cross-section, use an equivalent diameter, calculated
from the following equation, to determine the number of duct diameters:
                   71 u
          De  =  (L + w)                              Equation 2-1
where:
     D  - Equivalent diameter
     L  = Length
     W  = Width
     To ensure the presence of stable, fully developed  flow patterns
at the calibration site, or "test section," the site must  be located
at least eight diameters downstream and two diameters upstream from
the  nearest  disturbances.
      Note:   The  eight-  and two-diameter criteria  are not absolute;
other test  section  locations may be used  (subject to approval of the
Administrator),  provided  that  the flow at the  test site is stable and
demonstrably parallel  to  the duct axis.
      4.1.2.3  The flow system  shall have  the  capacity to generate a
test-section velocity around 915 m/min (3000  ft/min).   This velocity
                                         i
must be constant with time to  guarantee  steady flow during calibration.
Note that Type S pitot tube coefficients  obtained by single-velocity
calibration at 915 m/min  (3000 ft/min) will  generally be valid to
within +3 percent for the measurement of velocities above  305 m/min
                               C-20

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(1000 ft/min) and to within +5 to 6 percent for the measurement of
velocities between 180 and 305 m/min (600 and 1000 ft/min).  If a
more precise correlation between C  and velocity is desired, the flow
system shall have the capacity to generate at least four distinct,
time-invariant test-section velocities covering the velocity range
from 180 to 1525 m/min (600 to 5000 ft/min), and calibration data
shall be taken at regular velocity intervals over this range (see
Citations 9 and 14 in Section 6 for details).
     4.1.2.4  Two entry ports, one each for the standard and Type S
pitot tubes, shall be cut in the test section; the standard pitot entry
port shall be located slightly downstream of the Type S port, so that
the standard and Type S impact openings will lie in the same cross-
sectional plane during calibration.  To facilitate alignment of the
pitot tubes during calibration, it  is advisable that the test section
be constructed of plexiglas or some other transparent material.
     4.1.3  Calibration Procedure.  Note that  this procedure is a
general  one and must  not  be used without first referring to the special
considerations presented  in Section 4.1.5.   Note also that this pro-
cedure  applies only to single-velocity  calibration.  To obtain calibration
data for the A and B  sides of  the Type  S pitot tube, proceed as follows:
     4.1.3.1  Make sure that the manometer  is  properly filled and  that
the  oil  is  free  from  contamination  and  is of the proper density.   Inspect
and  leak-check all pitot  lines; repair  or replace  if necessary.
     4.1.3.2  Level and zero  the manometer.  Turn  on the fan and  allow
the  flow to stabilize.  Seal  the Type S entry  port.
     4.1.3.3  Ensure  that the  manometer is  level and zeroed.   Position
the  standard  pitot  tube at the calibration  point  (determined as outlined
                                C-21

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in Section 4.1.5.1), and align the tube so that its tip is pointed
directly into the flow.  Particular care should be taken in aligning
the tube to avoid yaw and pitch angles.  Make sure that the entry
port surrounding the tube is properly sealed.
     4.1.3.4  Read Ap$tcj and record its value in a data table similar
to the one shown in Figure 2-9.  Remove the standard pi tot tube from
the duct and disconnect it from the manometer.  Seal the standard
entry port.
     4.1.3.5  Connect the Type S pi tot tube to the manometer.  Open
the Type S entry port.  Check the manometer level and zero.   Insert
and align the Type S pitot tube so that its A side impact opening  is
at the same point as was the standard pi tot tube and is pointed directly
into the flow.  Make sure that the entry port surrounding the tube is
properly sealed.
     4.1.3.6  Read Ap  and enter its value in the data table.  Remove
the Type S pitot tube from the duct and disconnect it from the manometer.
     4.1.3.7  Repeat steps 4.1.3.3 through 4.1.3.6 above until three
pairs of Ap readings have been obtained.
     4.1.3.8  Repeat steps 4.1.3.3 through 4.1.3.7 above for  the B side
of the Type S pi tot tube.
     4.1.3.9  Perform calculations, as described  in  Section 4.1.4  below.
     4.1.4  Calculations.
     4.1.4.1  For each of the  six  pairs of Ap readings  (i.e.i three
from side A and three from side B) obtained  in  Section 4.1.3  above,
calculate the value of the Type S  pitot tube  coefficient as follows:
                              C-22

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PITOTTUBE IDENTIFICATION NUMBER:
CALIBRATED BY:	
DATE:

RUN NO.
1
2
3
"A" SIDE CALIBRATION
APstd
cm H20
(in. H20)




Ap($)
cm H20
(in. H20)



Cp (SIDE A)
cp(s)





DEVIATION
Cp(j)-Cp(A)





RUN NO.
1
2
3
"B" SIDE CALIBRATION
Ap«d
cmH20
(in. H20)




Ap($)
cmH20
(in. H20)



Cp (SIDE B)
Cp(s)





DEVIATION
Cp(5)-Cp(B)




   AVERAGE DEVIATION = a (A ORB)
                                   I |Cp(s)'Cp(A ORB)
     Cp (SIDE A)-Cp (SIDE B) |-*-MUST BE <0.01

                 Figure 2-9. Pilot tube calibration data.
       MUST BE
                              C-23

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          S(s) = S(std)
where:
     C / \   = Type S pi tot tube coefficient
     C / o.j\ = Standard pitot tube coefficient; use 0.99 if the
      p(std;
               coefficient is unknown and the tube is designed
               according to the criteria of Sections 2.7.1 to 2.7.5
               of this method.
     &p .  .   = Velocity head measured by the standard pitot tube,
               cm H20 (in. H20)
     Ap      - Velocity head measured by the Type S pitot tube,
               cm H20 (in. HgO)
     4.1.4.2  Calculate C~  (side A), the mean A-side coefficient, and
C_ (side B), the mean B-side coefficient; calculate the difference
between these two average values.
     4.1.4.3  Calculate the deviation of each of the three A-side values
of C / x from U  (side A), and the deviation of each B-side value of
C / x from C~  (side B).  Use the following equation:
          Deviation  =  C / » - C~  (A or B)           Equation 2-3
     4.1.4.4  Calculate o, the average deviation from the mean, for
both the A and B sides of the pitot tube.  Use the following equation:
                            lCp(s) ~S   (Aor
     a  (side A or B) = - - = -        Equation 2-4
                               C-24

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     4.1.4.5  Use the Type S pitot tube only if the values of a
(side A) and a (side B) are less than or equal  to 0.01 and if the
absolute value of the difference between C_ (A) and C"  (B) is 0.01
or less.
     4.1.5  Special considerations.
     4.1.5.1  Selection of calibration point.
     4.1.5.1.1  When an isolated Type S pitot tube is calibrated,
select a calibration point at or near the center of the duct, and
follow the procedures outlined in Sections 4.1.3 and 4.1.4 above.
The Type S pitot coefficients so obtained, i.e., C_ (side A) and
C_ (side B), will be valid, so long as either:   (1) the isolated
pitot tube is used; or (2) the pitot tube is used with other com-
ponents (nozzle, thermocouple, sample probe) in an arrangement that
is free from aerodynamic interference effects  (see Figures 2-6 through
2-8).
     4.1.5.1.2  For Type S pitot tube-thermocouple combinations
(without sample probe), select a calibration point at or near the
center of the duct, and follow the procedures outlined in Sections
4.1.3 and 4.1.4 above.  The coefficients so obtained will be valid
so long as the pitot tube-thermocouple combination is used by itself
or with other components in an interference-free arrangement (Figures
2-6 and 2-8).
     4.1.5.1.3  For assemblies with sample probes, the calibration
point should be located at or near the center of the duct; however,
                            C-25

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insertion of a probe sheath into a small  duct may cause significant
cross-sectional area blockage and yield incorrect coefficient
values (Citation 9 in Section 6).  Therefore, to minimize the
blockage effect, the calibration point may be a few inches off-center
if necessary.  The actual  blockage effect will be negligible when the
theoretical blockage, as determined by a  projected-area model of the
probe sheath, is 2 percent or less of the duct cross-sectional area
for assemblies without external sheaths (Figure 2-10a), and 3 percent
or less for assemblies with external sheaths (Figure 2-10b).
     4.1.5.2  For those probe assemblies  in which pitot tube-nozzle
interference is a factor (i.e., those in  which the pitot-nozzle
separation distance fails to meet the specification illustrated in
Figure 2-6a), the value of C , » depends  upon the amount of free-space
between the tube and nozzle, and therefore is a function of nozzle
size.  In these instances, separate calibrations shall be performed
with each of the commonly used nozzle sizes in place.  Note that the
single-velocity calibration technique is  acceptable for this purpose,
even though the larger nozzle sizes (>0.635 cm or 1/4 in.) are not
ordinarily used for isokinetic sampling at velocities around
915 m/min  (3000 ft/min), which is the calibration velocity; note
also that  it  is not necessary to draw an isokinetic sample during
calibration  (see Citation 19 in Section 6).
     4.1.5.3   For a probe assembly constructed such that its pitot
tube is  always used in  the  same orientation, only one side of the
pitot  tube need be  calibrated  (the side which will face the flow).
The  pitot  tube must still meet  the alignment specifications of
Figure'2-2 or 2-3,  however, and must  have an average deviation (a)
value  of 0.01  or  less  (see  Section 4.1.4.4).
                              C-26

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       (a)
                       (b)
                  ESTIMATED
                  SHEATH
                  BLOCKAGE
r  t
[pUC
UCTAREA
          x 100
Figure 2-10. Projected-area models for typical pitot tube assemblies.

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     4.1.6  Field Use and Recallbration.
     4.1.6.1  Field Use.
    •4.1.6.1.1  When a Type S pitot tube (isolated tube or assembly) is
used in the field, the appropriate coefficient value (whether assigned
or obtained by calibration) shall be used to perform velocity calculations.
For calibrated Type S pitot tubes, the A side coefficient shall be used
when the A side of the tube faces the flow, and the B side coefficient
shall be used when the B side faces the flow; alternatively, the
arithmetic average of the A and B side coefficient values may be
used, irrespective of which side faces the flow.
     4.1.6.1.2  When a probe assembly is used to sample a small duct
(12 to 36 in. in diameter), the probe sheath sometimes blocks a
significant part of the duct cross-section, causing a reduction in
the effective value of C_(s)-  Consult Citation 9 in Section 6 for
details.  Conventional pitot-sampling probe assemblies are not recom-
mended for use in ducts having inside diameters smaller than 12 inches
(Citation 16  in Section 6).
     4.1.6.2  Recalioration.
     4.1.6.2.1  Isolated Pitot Tubes.  After each field use, the pitot
tube shall  be carefully reexamined  in top, side, and end views.  If the
pitot  face  openings are still aligned within the specifications illus-
trated in  Figure  2-2  or 2-3, it  can be  assumed  that the baseline coef-
ficient  of the pitot  tube  has not changed.   If, however, the tube has
been damaged  to  the  extent that  it  no longer meets the specifications of
Figure 2-2  or 2-3,  the damage shall either be repaired to restore
proper alignment  of the  face openings or the tube shall be discarded.
     4.1.6.2.2   Pitot Tube Assemblies.   After each field use,  check the
face opening  alignment of  the pitot tube, as in Section 4.1.6.2.1;  also,
                            C-28

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  remeasure  the  intercomponent  spacings  of the  assembly.   If  the  inter-
  component  spacings  have not changed  and  the face  opening alignment  is
  acceptable,  it can  be assumed that the coefficient  of the assembly
  has  not changed.   If the face opening  alignment is  no longer within the
  specifications of Figures 2-2 or 2-3,  either  repair the  damage  or
  replace the  pitot tube (calibrating  the  new assembly, if necessary).
  If the intercomponent spacings have  changed,  restore the original
  spacings or  recalibrate the assembly.
       4.2  Standard  pitot tube (if applicable).   If  a standard pitot tube
  is used for  the velocity traverse, the tube shall be constructed
  according  to the criteria of  Section 2.7 and  shall  be assigned  a
'  baseline coefficient value of 0.99.   If the standard pitot  tube is
  used as part of an  assembly,  the tube shall be  in an interference-
  free arrangement (subject to  the approval of  the  Administrator).
       4.3  Temperature Gauges.  After each field  use, calibrate  dial
  thermometers, liquid-filled bulb thermometers,  thermocouple-
  potentiometer systems, and other gauges  at a  temperature within
  10 percent of the average absolute stack temperature.  For  temperatures
  up to 405°C  (761°F), use an ASTM mercury-in-glass reference thermometer,
  or equivalent, as a reference; alternatively, either a reference
  thermocouple and potentiometer (.calibrated by NBS)  or thermometric
  fixed points, e.g., ice bath  and boiling water  (corrected for barometric
  pressure)  may be used.  For temperatures above  405°C (761°F), use an
  NBS-calibrated reference thermocouple-potentiometer system  or an
  alternate  reference, subject  to the  approval  of the Administrator.
       If, during calibration,  the absolute temperatures measured with
  the gauge  being calibrated and the reference  gauge  agree within 1.5
  percent, the temperature data taken  in the field  shall be considered
  valid.  Otherwise,  the pollutant emission test shall  either be
                                C-29

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considered invalid or adjustments (if appropriate)  of the  test  results
shall be made, subject to the approval  of the Administrator.
     4.4  Barometer.  Calibrate the barometer used  against a  mercury
barometer.
5.  Calculations
     Carry out calculations, retaining at least one extra  decimal
figure beyond that of the acquired data.  Round off figures after
final calculation.
     5.1  Nomenclature.
                                            2    2
     A    = Cross-sectional area of stack, m  (ft ).
     B    = Water vapor in the gas stream (from Method 5 or Reference
      W5
            Method 4), proportion by volume.
     C    = Pitot tube coefficient, dimensionless.
      P
     K    = Pitot tube constant,
                 m     gg-moleHmm Hg)   '
)|
J
          <>   sec  L (K)(mm H20)
     for the metric system and
          RC AQ _ft [(Ib/lb-moleUin. Hgfl 1/2
          °°*Hy sec [  (°R)(in. H20)     J
      for the English system.
      M.    = Molecular weight of stack gas, dry basis  (see Section 3.6)
            g/g-mole  (Ib/lb-mole).
      M    = Molecular weight of stack gas, wet basis, g/g-mole
             (Ib/lb-mole).
           = Md(l  - Bws)  +  18.0 Bws                    Equation 2-5
      P.    = Barometric  pressure at  measurement site, mm Hg (in. Hg).
      P    = Stack static pressure,  mm Hg  (in. Hg).

                           C-30

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     P    = Absolute stack gas pressure, mm Hg (in.  Hg).
      s
            w~. + P                                  Equation 2-6
            bar
    P td = Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
    Q  .  = Dry volumetric stack gas flow rate corrected to standard
       *
           conditions, dscm/hr (dscf/hr).
    t    = Stack temperature, °C (°F).
    T    = Absolute stack temperature, °K (°R).
         = 273 + t  for metric                       Equation 2-7
         = 460 + ts for English                      Equation 2-8
    T  t(j = Standard absolute temperature, 293 °K (528°R).
    v    = Average stack gas velocity, m/sec (ft/sec).
    Ap  = Velocity head of stack  gas, mm H20  (in. H20).
    3600 = Conversion  factor, sec/hr.
    18.0 = Molecular weight of water, g/g-mole  (Ib/lb-mole).
    5.2  Average  stack gas velocity.
                                                       Equation 2-9
     5.3  Average stack gas dry volumetric flow rate.
     Qsd -  3600 (L^, vsA                           Equation  2-,0

6.  Bibliography
     1.  Mark, L. S.  Mechanical  Engineers'  Handbook.   New York.
McGraw-Hill Book Co., Inc.  1951.
     2.  Perry, 0. H.  Chemical Engineers'  Handbook.   New York
McGraw-Hill Book Co., Inc.  1960.
                          C-31

-------
     3.  Shigehara, R. T., W. F. Todd, and W. S. Smith.  Significance
of Errors in Stack Sampling Measurements.  U. S. Environmental
Protection Agency, Research Triangle Park, N. C.  (Presented at the
Annual Meeting of the Air Pollution Control Association, St. Louis, Mo.,
June 14-19, 1970.)
     4.  Standard Method for Sampling Stacks for Particulate Matter.
In:  1971 Book of ASTM Standards, Part 23.  Philadelphia, Pa.  1971.
ASTM Designation D-2928-71.
     5.  Vennard, J. K.  Elementary Fluid Mechanics.  New York.
John Wiley and Sons, Inc.  1947.
     6.  Fluid Meters - Their Theory and Application.  American Society
of Mechanical Engineers, New York, N.Y.  1959.
     7.  ASHRAE Handbook of Fundamentals.  1972.  p. 208.
     8.  Annual Book of ASTM Standards, Part 26.  1974.  p. 648.
     9.  Vollaro, R. F.  Guidelines for Type S  Pitot Tube Calibration.
U. S.  Environmental Protection Agency, Research Triangle Park, N. C.
 (Presented at 1st Annual Meeting, Source Evaluation Society,  Dayton, Ohio,
 September 18, 1975.)
      10.  Vollaro,  R. F.  A Type S Pitot Tube Calibration Study.  U. S.
 Environmental Protection  Agency, Emission  Measurement  Branch,  Research
 Triangle Park,  N.  C.  July 1974.
      11.   Vollaro,  R.  F.  The  Effects  of Impact Opening Misalignment on
 the  Value of the Type S  Pitot  Tube  Coefficient. U.  S.  Environmental
 Protection Agency,  Emission  Measurement  Branch, Research Triangle Park,
 N. C.   October  1976.
                           C-32

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     12.  Vollaro, R. F.  Establishment of a Baseline Coefficient Value
for Properly Constructed Type S Pitot Tubes.  U.  S.  Environmental
Protection Agency, Emission Measurement Branch, Research Triangle
Park, N. C.  November 1976.
     13.  Vollaro, R. F.  An Evaluation of Single-Velocity Calibration
Technique as a Means of Determining Type S Pi tot Tube Coefficients.
U. S. Environmental Protection Agency, Emission Measurement Branch,
Research Triangle Park, N. C.  August 1975.
     14.  Vollaro, R. F.  The Use of Type S Pi tot Tubes for the Measurement
of Low Velocities.  U. S. Environmental Protection Agency, Emission
Measurement Branch, Research Triangle Park, N. C.  November 1976.
     15.  Smith, Marvin L.  Velocity Calibration of EPA Type Source
Sampling Probe.  United Technologies Corporation, Pratt and Whitney
Aircraft Division, East Hartford, Conn.  1975.
     16.  Vollaro, R. F.  Recommended Procedure for Sample Traverses in
Ducts Smaller than 12 Inches in Diameter.  U. S. Environmental Protection
Agency, Emission Measurement Branch, Research Triangle Park, N. C.
November 1976.
     17.  Ower, E. and R. C. Pankhurst.  The Measurement of Air Flow,
4th  Ed. London, Pergamon Press.  1966.
     18.  Vollaro, R. F.  A Survey of Commercially Available Instrumentation
for  the Measurement of Low-Range Gas Velocities.  U. S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park,
N. C.   November 1976.   (Unpublished Paper)
                          C-33

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     19.  Gnyp, A. W., C. C. St. Pierre, D. S. Smith, D. Mozzon, and
J. Steiner.  An'Experimental Investigation of the Effect of Pitot Tube-
Sampling Probe Configurations on the Magnitude of the S Type Pi tot Tube
Coefficient for Commercially Available Source Sampling Probes.  Prepared
by the University of Windsor for the Ministry of the Environment,
Toronto, Canada.  February 1976.
                           C-34

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 SLIDE 103-0

        METHOD — 2
Determination of Stack Gas Velocity
    and Volumetric Flow Rate
                                                          NOTES
  SLIDE  103-1
                                    C-35

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  SLIDE 103-2
   TYPE S PTFOT TUBE MANOMETER ASSEMBLY
                                                                 NOTES
                                 FLEXIBLE TUBING
                                 625MMIV.INI
 L = DISTANCE TO FURTHEST SAMPLING
   POINT PIUS 30 CM (12 IN I

 •PITOT TUBE — TEMPERATURE SENSOR SPACING
 SLIDE  103-3


     APPLICABILITY OF METHOD 2
 This method is only applicable at sites which:
  1. Meet the criteria of method 1
  2. Do not contain cyclonic or non parallel tlow

ALTERNATIVES WHEN UNACCEPTABLE
           CONDITIONS EXIST
   (Subject to Approval of the Administrator)

   1. Install straightening vanes.
   2. Calculate total volumetric flow rate
    stoichiometrically.
   3. Move to a measurement site at which flow is
    acceptable.
   4. Use  procedures  as described in the cyclonic
    flow special problems session.
                                      C-37

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SLIDE 103-4
                                                                NOTES
SLIDE  103-5
       DIFFERENTIAL PRESSURE GAUGE
 An inclined manometer or equivalent device is required
 to measure AR
 A differential pressure gauge of greater sensitivity shall
 be used if any of the following conditions exist:
  1. arithmetic average of all AP readings is < 0.05 in. \-\2O
  2. traverses of > 12 pts., and 10% of AP readings are below
    0.05 in. H2O
  3. traverses of  < 12 pts., and more than 1  ^P reading is
    below 0.05 in. H2O

 Note:  Standard manometer used in source testing is a 10 in.
       inclined vertical manometer (0.01 in. divisions on a 0 to
       1 in. scale, and 0.1 in. divisions on a 1 to 10 in. scale).
                                      C-39

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 SLIDE  103-6                                                 NOTES

(cont.)
 • Alternative approach to determine if a more sensitive
   differential pressure guage is required:
                    S     1/AP, + K
   If T is >  1.05, a  more sensitive differential  pressure
   guage must be used.
      Where:
           AP, = individual velocity head reading at a traverse
                point
             n = total number of points
             K = 0.13 mm H2O  for metric units and 0.005 in.
                H2O for English units
  SLIDE  103-7
             TEMPERATURE SENSOR
   The temperature sensor must be accurate to within
 1.5% of Minimum Absolute Stack Temperature.
   Temperature sensors typically used in testing include:
  • Thermocouple
  • Bimetallic Thermometer
  • Mercury-in-Glass Thermometer
  • Liquid-Filled Bulb Thermometer
 Note: When the stack temperature measurement is used to
      calculate moisture, the sensitivity is ± 2°F.
                                        C-41

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SLIDE 103-8
                                                            NOTES
 SLIDE  103-9

       PRESSURE PROBE AND GUAGE
  Static pressure measurement must be accurate to
within 0.1 in. Hg (1.36 in. H:O).
  Pressure sensors typically  used to measure static
pressure during testing include:
 • a  piezometer tube and mercury or water-filled U-tube
   manometer
 • the static tap of a standard pitot tube
 • one leg of the type S pitot tube
                                    C-43

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 SLIDE  103-10                                                NOTES
           BAROMETRIC PRESSURE
    Barometric pressure measurement must be accurate
  to within 0.1 in. Hg.
    Barometric pressure during testing is obtained by:

                  INSTRUMENT
    Mercury, aneroid or other barometer (with required
  sensitivity)
                     OTHER
    Obtain  barometric pressure from nearby National
  Weather Service station (station pressure) and adjust
  for elevation differences between sampling site and
  weather station.
  Note: The station pressure must  be used not  the
       pressure corrected to sea level.
 SLIDE  103-11
       PITOT TUBE CALIBRATION
Perform Dimensional Specification Test
                   and/or
Calibrate in wind tunnel against standard pitot
tube (preferably with NBS traceable coefficient)
                                       C-45

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SLIDE 103-12
NOTES

SLIDE 103-13
                               C-47

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SLIDE 103-14
                                                    NOTES
 SLIDE 103-15
                                 C-49

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SLIDE  103-16
                                                    NOTES
SLIDE 103-17
                              C-51

-------
SLIDE 103-18
NOTES
SLIDE 103-19
                               C-53

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SLIDE 103-20
NOTES
SLIDE 103-21
                               C-55

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 SLIDE 103-22
                                       NOTES
   TYPE-S PITOT TUBE INSPECTION DATA SHEET
PITOT TUBE ASSEMBLY LEVEL? .
                                    YES.
                               . YES (EXPLAIN BELOW).
PITOT TUBE OPENINGS DAMAGED?	
», =	M  10°),   „, =	°KIO°),   p, =	°(-5u
-y =	°.   < > =	!.   A =	CM (IN.)
z = A sin y = 	CM (IN.); 0.32 CM Ktt IN.).
w = AsinO  =	CM (IIM.I;  0.08 CM KVulN.)
P.	CM (IN.)    Pb	CM (IN.)
                         NO
                        .NO
                                                 s°i
        .CM (IN.I   _t_ =
.(1.05 -  and - 1.50)
COMMENTS:
CALIBRATION REQUIRED? .
DATE:
                        -CONDUCTED BY:
 SLIDE 103-23
     "S" Typ
   Fliot Tube

                          V  (8 Oiams
                                         C-57

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 SLIDE 103-24
                                   NOTES
       PITOT TUBE CALIBRATION DATA SHEET

CALIBRATION PITOT TUBE:   TYPE STD.   SIZE (OD) JV.   ID NUMBER _2_
TYPE S PITOT TUBE ID NUMBER  8S  €„,,,,,, = 1.0
CALIBRATION:   DATE 3/10/76    PERFORMED
"A" SIDE CALIBRATION
AP.UJ
cmH,O
(IN. HZ0)
0.20
1 0.30

0.50

1.00


!

Ap,
cm HjO
(IN. H20)
0.28
0.41

0.69

1.38



AVERAGE
\a
Cp(SI
0.845
0.856

0.851

0.850



0.850

\b
DEV.
-0.005
0.006

-0.001

0




       = Cp(mtd,
 b  DEV = Cpjs, = Cp, (MUST BE sO.01).
   Cp(A) = Cp(B) = 0.005 (MUST BE sO.01).
= 1.0 /0.714  = 0.845
  SLIDE 103-25


 DIFFERENTIAL PRESSURE GAUGE CALIBRATION
  TO PRESSURE SOURCE OR
  VENTED TO ATMOSPHERE
                           TO VACUUM SYSTEM OR
                           VENTED TO ATMOSPHERE
                                          C-59

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 SLIDE  103-26
                                                            NOTES
   TEMPERATURE SENSOR CALIBRATION
 Calibrate initially and after each field use.
 Post test calibration must be performed at a temperature
 within 10% of the average absolute stack temperature.

         CALIBRATION REFERENCES
    UP TO 761°F                ABOVE 761°F
ASTM Mercury-in-glass       NBS-Calibrated reference
reference thermometer            thermocouple

   ALTERNATIVE CALIBRATION REFERENCES
 Thermometric fixed points (ice bath and boiling water)
 SLIDE 103-27
                                     C-61

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SLIDE 103-28
                                                           NOTES
 SLIDE 103-29
  TEMPERATURE SENSOR CALIBRATION
                EVALUATION

              THERMOCOUPLE
  Absolute  temperature values  must agree within
± 1.5% at each point.
 • Plot data on linear graph paper, draw best fit line.
 • Data may be extrapolated above and below calibration
  points.
               THERMOMETER
  Absolute temperature values must agree within
+ 1.5% at each point.
 • Thermometer may be used over the range of calibration
  points.
 • If correction factor is needed it must be affixed  to
  thermometer.

                                    C-63

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SLIDE 103-30
NOTES
SLIDE 103-31
                               C-65

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 SLIDE  103-32
NOTES
 SLIDE 103-33
 VELOCITY MEASUREMENT PROCEDURES
1. Leak-check pilot tube and differential pressure gauge.
2. For circular stacks less than 10 ft. in diameter, two ports
  are sufficient. Use four ports when stack diameter is
  greater than 10ft.
3. Pilot tubes longer than  10 ft. should be structurally
  reinforced to prevent bending of  tube and misalign-
  ment errors.
4. Identify each sample port and traverse point with a
  letter or number.
5. Read velocity head and temperature at least twice at
  each point and record the average.
                                         C-67

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  SLIDE 103-34

(conL)
    6. Care should be taken to prevent touching the pitot
      tube tip to the side of the stack.
    7. Plug unused sampling ports and seal port being used
      as tightly as possible.
    8. After traverse, check differential pressure gauge zero;
      repeat traverse if zero has shifted.
    9. If  liquid droplets  are  present, use a liquid trap in
      positive pressure leg of pitot tube.
   10. A post-test leak check is required after each run of the
      pitot tube and velocity pressure system.
NOTES
  SLIDE  103-35
                  STATIC PRESSURE MEASUREMENT
  PRESSURE PROBE AND GAUGE
                             STANDARD PITOT TUBE
                                                       TYPE S PITOT TUBE
               MANOMETER
                                       MANOMETER
                                                               MANOMETER
                                            C-69

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                            SECTION D.  METHOD 3

Subject                                                               Page

1.  Method 3--gas analysis for carbon dioxide, oxygen, excess air,
    and dry molecular weight (taken from Environmental Protection
    Agency Performance Test Methods manual)                           D-3

2.  Slides                                                            D-19
                                      D-l

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        METHOD 3--GAS ANALYSIS FOR CARBON DIOXIDE, OXYGEN,
              EXCESS AIR, AND DRY MOLECULAR WEIGHT
 1.  Principle and Applicability
     1.1  Principle.  A gas sample is extracted from a stack, by one
of the following methods:  (1) single-point, grab sampling; (2)  single-
point, integrated sampling; or (3) multi-point, integrated  sampling.
The gas sample is analyzed for percent carbon dioxide (C0?), percent
oxygen (Og), and, if necessary, percent carbon monoxide (CO).  If a
dry molecular weight determination is to be made, either an Orsat
or a Fyrite  analyzer may be used for the analysis; for excess air
or emission rate correction factor determination, an Orsat  analyzer
must be used.
     1.2  Applicability.  This method is applicable for determining
C02 and 0« concentrations, excess air, and dry molecular weight of
a sample from a gas stream of a fossil-fuel combustion process,   The
method may also be applicable to other processes where it has been
determined that compounds other than C02, 02, CO, and nitrogen (N-)
are not present in concentrations sufficient to affect the results.
     Other methods, as well as modifications to the procedure
described herein, are also applicable for some or all of the above
determinations.  Examples of specific methods and modifications
include:  (1) a multi-point sampling method using an Orsat analyzer
to analyze individual grab samples obtained at each point;  (2) a
method using C02 or 0« and stoichiometric calculations to determine
dry molecular weight and excess air; (3) assigning a value of 30.0
 Mention of trade names or specific products does not constitute
 endorsement by the Environmental Protection Agency.
                           D-3

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for dry molecular weight, in lieu of actual measurements, for
processes burnjng natural gas, coal, or oil.  These methods and
modifications may be used, but are subject to the approval of the
Administrator, U.S. Environmental Protection Agency.
2.  Apparatus
     As an alternative to the sampling apparatus and systems described
herein, other sampling systems (e.g., liquid displacement) may be
used provided such systems are capable of obtaining a representative
sample and maintaining a constant sampling rate, and are otherwise
capable of yielding acceptable results.  Use of such systems is
subject to the approval of the Administrator.
     2.1  Grab Sampling (Figure 3-1).
     2.1.1  Probe.  The probe should be made of stainless steel or
borosilicate glass tubing and should be equipped with an in-stack
or out-stack filter to remove particulate matter (a plug of glass
wool is satisfactory for this purpose).  Any other material inert to
02» CCL, CO, and N2 and resistant to temperature at sampling conditions
may be used for the probe; examples of such material are aluminum,
copper, quartz glass and Teflon.
     2.1.2  Pump.  A one-way squeeze bulb, or equivalent, is used
to transport the gas sample to the analyzer.
     2.2  Integrated Sampling (Figure 3-2).
     2.2.1  Probe.  A probe such as that described in Section 2.1.1
is suitable.
                             D-4

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                   PROBE
                                           FLEXIBLE TUBING
       \
           FILTER (GLASS WOOL)
                               SQUEEZE BULB
TO ANALYZER
                            Figure 3-1. Grab-sampling tram.
                                           RATE METER
     AIR-COOLED
     CONDENSER
\
   FILTER
(GLASS WOOL)
                                           QUICK DISCONNECT

                                                      _n
                                 RIGID CONTAINER
                      Figure 32.  Integrated gas sampling train.
                                D-5

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     2.2.2  Condenser.   An air-cooled or water-cooled condenser,
or other condenser that will  not remove 02, C02, CO, and N2,  may
be used to.remove excess moisture which would interfere with
the operation of the pump and flow meter.
     2.2.3  Valve.  A needle valve is used to adjust sample gas
flow rate.
     2.2.4  Pump.  A leak-free, diaphragm-type pump, or equivalent,
is used to transport sample gas to the flexible bag.  Install a
small surge tank between the pump and rate meter to eliminate the
pulsation effect of the diaphragm pump on the rotameter.
     2.2.5  Rate Meter.  The rotameter, or equivalent rate meter,
used should be capable of measuring flow rate to within +2 percent
of the selected flow rate.  A flow rate range of 500 to 1000
cm /min is suggested.
     2.2.6  Flexible Bag.  Any leak-free plastic (e.g., Tedlar,
Mylar, Teflon) or plastic-coated aluminum (e.g., aluminized
Mylar) bag, or equivalent, having a capacity consistent with  the
selected flow rate and time length of the test run, may be used.   A
capacity in the range of 55 to 90 liters is suggested.
     To leak-check the bag, connect it to a water manometer and pressurize
the bag to 5 to 10 cm H20 (2 to 4 in. H20).  Allow to stand for 10
minutes.  Any displacement in the water manometer indicates a
leak.  An alternative leak-check method is to pressurize the  bag
to 5 to 10 cm H20 (2 to 4 in. HgO) and allow to stand overnight.   A
deflated bag indicates a leak.
                           D-6

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     2.2.7  Pressure Gauge.  A water-filled U-tube manometer, or
equivalent, of about 28 cm (12 in.) is used for the flexible bag
leak-check.
     2.2.8  Vacuum Gauge.  A mercury manometer, or equivalent, of at
least 760 mm Hg (30 in. Hg) is used for the sampling train leak-check.
     2.3  Analysis.  For Orsat and Fyrite analyzer maintenance and
operation procedures, follow the instructions recommended by the
manufacturer, unless otherwise specified herein.
     2.3.1  Dry Molecular Weight Determination.  An Orsat analyzer or
Fyrite type combustion gas analyzer may be used.
     2.3.2  Emission Rate Correction  Factor or Excess Air Determination.
An Orsat analyzer must be used.  For  low C02  (less than 4.0 percent)
or high 02  (greater than 15.0 percent) concentrations, the measuring
burette of  the Orsat must have at  least 0.1 percent subdivisions.
3.   Dry Molecular Weight Determination
     Any of the three  sampling and analytical  procedures described
below may  be  used for  determining  the dry  molecular weight.
     3.1   Single-Point,  Grab  Sampling and  Analytical  Procedure.
     3.1.1  The sampling point in  the duct shall  either  be at the
centroid of the cross  section or at  a point no closer to the walls
than 1.00  m (3.3  ft),  unless  otherwise  specified  by the  Administrator.
     3.1.2 Set up  the equipment as  shown  in  Figure 3-1, making  sure
all  connections ahead  of the  analyzer are  tight and leak-free.   If  an
Orsat  analyzer is  used,  it is recommended  that the analyzer  be  leak-
checked  by following  the procedure in Section 5;  however, the leak-
check  is  optional.
                           D-7

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     3.1.3  Place the probe in the stack, with the tip of the  probe
positioned at the sampling point; purge the sampling line.  Draw a
sample into the analyzer and immediately analyze it for percent CCL
and percent CL.  Determine the percentage of the gas that is N« and
CO by subtracting the sum of the percent CCL and percent CL from
100 percent.  Calculate the dry molecular weight as indicated  in
Section 6.3.
     3.1.4  Repeat the sampling, analysis, and calculation procedures,
until the dry molecular weights of any three grab samples differ from
their mean by.no more than 0.3 g/g-mole (0.3 Ib/lb-mole).  Average
these three molecular weights, and report the results to the nearest
0.1 g/g-mole (Ib/lb-mole).
     3.2  Single-Point, Integrated Sampling and Analytical Procedure.
     3.2.1  The sampling point in the duct shall be located as speci-
fied in Section 3.1.1.
     3.2.2  Leak-check (optional) the flexible bag as in Section 2.2.6.
Set up the equipment as shown in Figure 3-2.  Just prior to sampling,
leak-check  (optional) the train by placing a vacuum gauge at the
condenser inlet, pulling a vacuum of at least 250 mm Hg (10 in. Hg),
plugging the outlet at the quick disconnect, and then turning  off the
pump.  The vacuum should remain stable for at least 0.5 minute.
Evacuate the flexible bag.  Connect the probe and place it in  the
stack, with the tip of the probe positioned at the sampling point;
purge the sampling line.  Next, connect the bag and make sure  that
all  connections are tight and leak free.
                           D-8

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     3.2.3  Sample at a constant rate.  The sampling run should be
simultaneous with, and for the same total length of time as, the
pollutant emission rate determination.  Collection of at least 30
               o
liters (1.00 ft ) of sample gas is recommended; however, smaller
volumes may be collected, if desired.
     3.2.4  Obtain one integrated flue gas sample during each pollutant
emission rate determination.  Within 8 hours after"the sample is taken,
analyze it for percent C02 and percent 02 using either an Orsat
analyzer or a Fyrite type combustion gas analyzer.  If an Orsat
analyzer is used, it is recommended that the Orsat leak-check
described in Section 5 be performed before this determination;
however, the check is optional.  Determine the percentage of the
gas that is N2 and CO by subtracting the sum of the percent C02 and
percent 02 from 100 percent.  Calculate the dry molecular weight as
indicated in Section 6.3.
     3.2.5  Repeat the analysis and calculation procedures until the
individual dry molecular weights for any three analyses differ from
their mean by no more than 0.3 g/g-mole  (0.3 Ib/lb-mole).  Average
these three molecular weights, and report the results to the nearest
0.1 g/g-mole (0.1 Ib/lb-mole).
     3.3. Multi-Point, Integrated Sampling and Analytical Procedure.
     3.3.1  Unless otherwise specified by the Administrator, EPA, a
minimum of eight traverse points shall be used for circular stacks having
diameters less than 0.61 m (24 in.), a minimum of nine shall be used for
rectangular stacks having equivalent diameters less than 0.61 m (24 in.),
and a minimum of twelve traverse points shall be used for all other
cases.  The traverse points shall be located according to Method 1.  The
use of fewer points is subject to the approval of the Administrator.
                            D-9

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     3.3.2  Follow the procedures outlined in Sections 3.2.2
through 3,2.5, except for the following:   traverse all sampling
points and sample at each point for an equal length of time.
Record sampling data as shown in Figure 3-3.
4.  Emission Rate Correction Factor or Excess Air Determination
     Note:  A Fyrite type combustion gas  analyzer is not acceptable
for excess air or emission rate correction factor determination,
unless approved by the Administrator.  If both percent C0« and
percent (L are measured, the analytical results of any of the three
procedures given below may also be used for calculating the dry
molecular weight.
     Each of the three procedures below shall be used only when
specified in an applicable subpart of the standards.  The use of
these procedures for other purposes must have specific prior approval
of the Administrator.
     4.1  Single-Point, Grab Sampling and Analytical Procedure.
     4.1.1  The sampling point in the duct shall either be at the
centroid of the cross-section or at a point no closer to the walls
than 1.00 m (3.3 ft), unless otherwise specified by the Administrator,
     4.1.2  Set up the equipment as shown in Figure 3-1, making sure
all connections ahead of the analyzer are tight and leak-free.  Leak-
check the Orsat analyzer according to the procedure described in
Section 5.  This leak-check 1s mandatory.
     4.1.3  Place the probe in the stack, with the tip of the probe
positioned at the sampling point; purge the sampling line.  Draw
                           D-10

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TIME




TRAVERSE
FT.




AVERAGE
Q
1pm





% DEV.a





a%DEV= (1JL?I9)100     (MUSTBE<10%)
     Figure 3-3. Sampling rate data.
                     D-ll

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a sample into the analyzer.   For emission rate correction factor
determination, immediately analyze the sample, as outlined in Sections
4.1.4 and 4.1.5, for percent C02 or percent 02.  If excess air is
desired, proceed as follows:  (1) immediately analyze the sample,  as in
Sections 4.1.4 and 4.1.5, for percent C02, 02> and CO; (2) determine the
percentage of the gas that is N2 by subtracting the sum of the percent
C02, percent 02, and percent CO from 100 percent; and (3) calculate
percent excess air as outlined in Section 6.2.
     4.1.4  To ensure complete absorption of the C0«> Op, or if appli-
cable, CO, make repeated passes through each absorbing solution until
two consecutive readings are the same.  Several passes (three or four)
should be made between readings.  (If constant readings cannot be
obtained after three consecutive readings, replace the absorbing solution.)
     4.1.5  After the analysis is completed, leak-check (mandatory)
the Orsat analyzer once again, as described in Section 5.  For the
results of the analysis to be valid, the Orsat analyzer must pass
this leak test before and after the analysis.  Note:  Since this
single-point, grab sampling and analytical procedure is normally
conducted in conjunction with a single-point, grab sampling and
analytical procedure for a pollutant, only one analysis is ordinarily
conducted.  Therefore, great care must be taken to obtain a valid
sample and analysis.  Although in most cases  only C02 or 02 is
required, it is recommended that both C02 and 02 be measured, and
that Citation 5 in the Bibliography be used to validate the analytical
data.
                             D-12

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     4.2  Single-Point, Integrated Sampling and Analytical  Procedure.
     4.2.1  The sampling point in the duct shall be located as
specified in Section 4.1.1.
     4.2.2  Leak-check (mandatory) the flexible bag as in Section 2.2.6.
Set up the equipment as shown in Figure 3-2.  Just prior to sampling,
leak-check (mandatory) the train by placing a vacuum gauge  at the
condenser inlet, pulling a vacuum of at least 250 mm Hg (10 in.  Hg),
plugging the outlet at the quick disconnect, and then turning off the
pump.  The vacuum shall remain stable for at least 0.5 minute.
Evacuate the flexible bag.  Connect the probe and place it  in the
stack, with the tip of the probe positioned at the sampling point;
purge the sampling line.  Next, connect the bag and make sure that all
connections are tight and leak free.
     4.2.3  Sample at a constant rate, or as specified by the
Administrator.  The sampling run must be simultaneous with, and  for
the same total length of time as, the pollutant emission rate
determination.  Collect at least 30 liters  (1.00 ft ) of sample
gas.  Smaller volumes may be collected, subject to approval of  the
Administrator.
     4.2.4  Obtain one integrated flue gas  sample during each pollutant
emission rate determination.  For emission  rate correction  factor
determination, analyze the sample within 4  hours after it is taken
for percent CCL or percent Op (as outlined  in Sections 4.2.5 through
4.2.7).  The Orsat analyzer must be leak-checked (see Section 5) before
the analysis.  If excess air is desired, proceed as follows:  (1) within
4 hours after the sample is taken, analyze  it (as in Sections 4.2.5
                             D-13

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through 4.2.7) for percent C02» 02, and CO; (2) determine the percentage
of the gas that is Np by subtracting the sum of the percent C02, percent
02, and percent CO from TOO percent; (3) calculate percent excess air,
as outlined in Section 6.2.
     4.2.5  To ensure complete absorption of the C02> 02, or if applicable,
CO, make repeated passes through each absorbing solution until two
consecutive readings are the same.  Several passes (three or four)
should be made between readings.  (If constant readings cannot be obtained
after three consecutive readings, replace the absorbing solution.)
     4.2.6  Repeat the analysis until the following criteria are met:
     4.2.6.1  For percent C02, repeat the analytical procedure until the
results of any three analyses differ by no more than (a) 0.3 percent by
volume when C02 is greater than 4.0 percent or (b) 0.2 percent by volume
when C02 is less than or equal to 4.0 percent.  Average the three acceptable
values of percent C02 and report the results tu the nearest 0.1 percent.
     4.2.6.2  For percent 02, repeat the analytical procedure until the
results of any three analyses differ by no more than (a) 0.3 percent by
volume when 02 is less than 15.0 percent or (b) 0.2 percent by volume
when 02 is greater than or equal to 15.0 percent.  Average the three
acceptable values of percent 02 and report the results to the nearest
0.1 percent.
     4.2.6.3  For percent CO, repeat the analytical procedure until the
results of any three analyses differ by no more than 0.3 percent.
Average the th^ee acceptable values of percent CO and report the results
to the nearest 0.1 percent.
                            D-14

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     4.2.7  After the analysis is completed, leak-check (mandatory)
the Orsat analyzer once again, as described in Section 5.   For the
results of the analysis to be valid, the Orsat analyzer must pass
this leak test before and after the analysis.  Note:  Although in
most instances only CCL or 02 is required, it is recommended that
both C02 and 02 be measured, and that Citation 5 in the Bibliography
be used to validate the analytical data.
     4.3  Multi-Point, Integrated Sampling and Analytical  Procedure.
     4.3.1  Both the minimum number of sampling points and the
sampling point location shall be as specified in Section 3.3.1 of
this method.  The use of fewer points than specified is subject to
the approval of the Administrator.
     4.3.2  Follow the procedures outlined in Sections 4.2.2 through
4.2.7, except for the following:  Traverse all sampling points and
sample at each point for an equal length of  time.   Record sampling
data as shown in Figure 3-3.
5.  Leak-Check Procedure for Orsat Analyzers
     Moving an Orsat analyzer frequently causes it  to leak.  Therefore,
an Orsat analyzer should be thoroughly leak-checked on site before the
flue gas sample is introduced into it.  The  procedure for leak-checking
an Orsat analyzer is:
     5.1.1  Bring the liquid level in each pipette  up to the reference
mark on the capillary tubing and then close  the pipette stopcock.
     5.1.2  Raise the leveling bulb sufficiently to bring the confining
liquid meniscus onto the graduated portion of the burette and then
close the manifold stopcock.
                           D-15

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     5.1.3  Record the meniscus position.
     5.1.4  Observe the meniscus in the burette and the liquid level
in the pipette for movement over the next 4 minutes.
     5.1.5  For the Orsat analyzer to pass the leak-check, two
conditions must be met:
     5.1.5.1  The liquid level in each pipette must not fall  below
the bottom of the capillary tubing during this 4-minute interval.
     5.1.5.2  The meniscus in the burette must not change by more
than 0.2 ml during this 4-minute interval.
     5.1.6  If the analyzer fails the leak-check procedure, all
rubber connections and stopcocks should be checked until the cause
of the leak is identified.  Leaking stopcocks must be disassembled,
cleaned, and regreased.  Leaking rubber connections must be replaced,
After the analyzer is reassembled, the leak-check procedure must be
repeated.
6.  Calculations
     6.1  Nomenclature.
     M.    = Dry molecular weight, g/g-mole (Ib/lb-mole).
     %EA   - Percent excess air.
     XC02  « Percent C02 by volume (dry basis).
     %0«   = Percent 0« by volume  (dry basis).
     %CO   = Percent CO by volume  (dry basis)-
     %N2   = Percent N~ by volume  (dry basis)'
     0.264 = Ratio of 02 to N2 in air, v/v.
                          D-16

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     0.280 = Molecular weight of Np or CO, divided by 100.
     0.320 = Molecular weight of 02 divided by 100.
     0.440 = Molecular weight of COp divided by 100.
     6.2  Percent Excess Air.  Calculate the percent  excess  air (if
applicable), by substituting the appropriate values of percent 02»
CO, and N2 (obtained from Section 4.1.3 or 4.2.4) into Equation 3-1.
     %EA  =
                    %Q2 - 0.5% CO
100       Equation  3-1
              0.264 %N2 - (%02 - 0.5% CO)
              ^»                          ^Hl
     Note:  The equation above assumes that ambient air is used  as
the source of 02 and that the fuel does not contain appreciable
amounts of N2 (as do coke oven or blast furnace gases).  For those
cases when appreciable amounts of N2 are present (coal, oil, and
natural gas do not contain appreciable amounts of N2) or when oxygen
enrichment is used, alternate methods, subject to approval of the
Administrator, are required.
     6.3  Dry Molecular Weight.  Use Equation 3-2 to calculate the
dry molecular weight of the stack gas.

     Md  =  0.440(%C02) + 0.320(%02) + 0.280(%N2 + %CO)   Equation  3-2
     Note:  The above equation does not consider argon in air (about
0.9 percent, molecular weight of 37.7).  A negative error of about
0.4 percent is introduced.  The tester may opt to include argon  in
the analysis using procedures subject to approval of the Administrator.
                            D-17

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7.  Bibliography
     1.  Altshuller, A.P.  Storage of Gases and Vapors in Plastic
Bags.  International Journal of Air and Water Pollution.  6;75-81.
1963.
     2.  Conner, William D. and J. S. Nader.  Air Sampling with Plastic
Bags.  Journal of the American Industrial Hygiene 'Association.
25_:291-297.  1964.
     3.  Burrell Manual for Gas Analysts, Seventh edition.  Burrell
Corporation, 2223 Fifth Avenue, Pittsburgh, Pa. 15219.  1951.
     4.  Mitchell, W.J. and M.R. Midgett.  Field Reliability of the
Orsat Analyzer.  Journal of Air Pollution Control Association.
26:491-495.  May 1976.
     5.  Shlgehara, R.T., R.M. Neulicht, and W.S. Smith.  Validating
Orsat Analysis Data from Fossil Fuel-Fired Units.  Stack Sampling
News.  4_(2):21-26.  August, 1976.
                            D-18

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SLIDE  104-0                                                  NOTES

       METHOD — 3
       Gas Analysts for
Carbon Dioxide, Excess Air and
     Dry Molecular Weight
 SLIDE  104-1


                EPA METHOD 3
                   PRINCIPLE
A gas sample is collected by one of the following methods:
   • Single-point grab sampling
   • Single-point integrated sampling
   • Multi-point integrated sampling
The sample is analyzed for the following components:
   • Carbon dioxide (CO2)
   • Oxygen (62)
   • Carbon monoxide (CO) (if necessary)
                 APPLICABILITY
  This method is applicable for determining dry molecular
weight and excess air correction factor from fossil-fuel
combustion sources.
  SLIDE  104-2

              GRAB SAMPLING TRAIN
    FILTER
  (GLASS WOOL)
                  FLEXIBLE TUBING
                                               . TO ANALYZER
                               SQUEEZE BULB
                                          D-19

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SLIDE  104-3
                                                               NOTES
 SLIDE  104-4
            INTEGRATED GAS SAMPLING TRAIN
   FILTER
 (GLASS WOOLI
                                          RIGID CONTAINER
                                       D-21

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SLIDE 104-5
                                                   NOTES
 SLIDE 104-6
                                D-23

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 SLIDE 104-7
                                                              NOTES
            ORSAT ANALYZER
   SAMPLE
    INLET
THREE-WAY INLET VALVE TO MANIFOLD

   INLET VALVE TO CO PIPETTE

    INLET VALVE TO O, PIPETTE

       INLET VALVE TO CO, PIPETTE

                MANIFOLD

                 VOLUME
                REFERENCE
                 MARK
                                  WATER
                                  JACKET
SIDE VIEW OF TYPICAL
 PIPETTE ABSORBER
 SLIDE  104-8


       ORSAT ANALYZER REAGENTS
          GAS CONFINING SOLUTION
• A solution containing sodium sulfate, sulfuric acid and
 methyl orange
        CARBON DIOXIDE ABSORBENT
• A solution of potassium or sodium hydroxide
            OXYGEN ABSORBENT
• A solution of  alkaline pyrogallic acid or chromous
 chloride
       CARBON MONOXIDE ABSORBENT
• A solution of cuprous chloride or a sulfate solution
                                       D-25

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SLIDE  104-9
NOTES
           FYRITE ANALYZER
SLIDE  104-10
                               D-27

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 SLIDE  104-11
NOTES
 SLIDE  104-12


      CALIBRATION OF ANALYZERS

   AMBIENT AIR CHECK (O2 reagent only)
The average of 3 replicates should be 20.8 ± 0.7%.
   • a measured average value > 21.5% indicates poor
    operator technique
   • a measured average value < 20.1% indicates a
    faulty analyzer and/or poor technique

         CALIBRATION GAS CHECK
The average of 3 replicates should be + 0.5% of the
known concentration of each gas.
   • high measured values indicate poor technique
   • low values indicate faulty analyzer  and/or poor
    technique
                                      D-29

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   SLIDE  104-13

                ROTAMETER CAUBRAT1ON CURVE
NOTES
                    0.5                l.o

                  SAMPLING RATE. I/mm at 21"C and 760 mm Hg
  SLIDE  104-14

              SAMPLING METHODS
             Single-Point Grab Sampling
1. Sample point should be a centriod of the cross section or
  at a point 3.28 ft. from the walls of a large stack.
2. Place probe securely in stack and seal sampling port to
  prevent dilution of stack gas.
3. Purge sample line and attach to analyzer.
4. Aspirate sample into analyzer.
  SLIDE  104-15

              SAMPLING METHODS
           Single-Point Integrated Sampling
1. Sample point and probe placement is same as for single-
  point grab sampling.
2. Leak-check the flexible bag.
3. Leak-check the sampling train.
4. Connect probe to train and purge the system.
5. Connect evacuated flexible bag and begin sampling.
6. Sample at constant rate; collect 30 to 90  liters of gas
  simultaneous with pollutant emission test.
                                         D-31

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 S-LIDE 104-16
NOTES
             SAMPLING METHODS
           Multi-Point Integrated Sampling
1. This procedure uses same sample train and equipment pre-
  paration as the single-point integrated sampling method.
2. Locate sampling points according to method 1.
3. Sample each point at the same rate and for the same time
  increment.
4. Collect 30 to 90 I. of gas simultaneous  with pollutant
  emission test.
  SLIDE  104-17

          PLASTIC BAG LEAK-CHECK SYSTEM
            MANOMETER
 TO AIR
 PRESSURE f
      Q.
  SLIDE 104-18

 INTEGRATED SAMPLE TRAIN LEAK-CHECK
                PROCEDURE
   1. Attach vacuum gauge to condenser inlet.
   2. Draw a vacuum of 10 in. Hg and plug line where
     bag attaches.
   3. Turn off pump; vacuum reading should remain
     stable for 30 seconds.
                                       D-33

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  SLIDE  104-13                                              NOTES

ORSAT ANALYZER LEAK-CHECK PROCEDURE
    1. Bring liquid level in each pipette up to reference
      mark. Close pipette stopcock.
    2. Bring  liquid  level of  confining  liquid onto
      graduated portion of the burette. Close manifold
      stopcock.
    3. Record meniscus position.
    4. Observe pipette and burette for 4 minutes.
       The orsat analyzer passes leak-check if:
    1. The liquid level in each pipette does  not fall
      below bottom of capillary tubing.
    2. The meniscus in the burette does not change by
      more than 0.2 ml.
 SLIDE  104-20

DRY MOLECULAR WEIGHT DETERMINATION
 1. Sample collection by any one of the three sampling
   methods.
 2. Sample must be analyzed within 8 hrs. after collection.
 3. Analysis may be conducted using an orsat or fyrite
   analyzer.
 4. Repeat analysis until any three analyses differ from
   their mean by no more than 0.3 Ib/lb-mole.
 5. Average the three molecular weights and report results
   to nearest 0.1 Ib/lb-mole.
 SLIDE  104-21

      DRY MOLECULAR WEIGHT EQUATION


Md = 0.44(%CO2) + 0.32(%02) + 0.28(%N2 + %CO)


     where:    md  = dry molecular weight
           %CC>2  = Percent CO-2 by volume (dry basis)
            %O-2  = Percent O2 by volume (dry basis)
            %CO  = Percent CO by volume (dry basis)
            %N2  = Percent N2 by volume (dry basis)
            0.44  = molecular weight of CO2 divided by 100
            0.32  = molecular weight of O2 divided by 100
            0.28  = molecular weight of N2 divided by 100
                                       D-35

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 SLIDE 104-22

EMISSION RATE CORRECTION FACTOR
                    OR
     EXCESS AIR DETERMINATION
 1. Sampling method is specified in the standard.
 2. Fyrite analyzer cannot be used.
 3. Sample must be analyzed within 4 hours after
  collection.
 4. Pre-test and post-test leak-check of the orsat
  analyzer are mandatory
 5. Make repeated passes through each absorbing
  solution until two consecutive readings are the
  same.
                NOTES
  SLIDE  104-23

 (cont)

 6. Repeat analysis until results for any three
   analyses differ by no more than:

          CO2               O2                CO
   1. 0.3% by volume when  1. 0.3% by volume when 1. 0.3% by volume
     CO2 is > 4.0%.         O2 is < 15.0%.
   2. 0.2% by volume when  2.0.2% by volume when
     CO2 is < 4.0%.         O2 is > 15.0%.

         7. Average the acceptable values and report results
           to the nearest 0.1%.
  SLIDE 104-24

         PERCENT EXCESS AIR EQUATION
 %EA =
                  .%O2 - 0.5%CO
           0.264%N2 - (%02 - 0.5%CO)
100
    where: %EA = Percent excessive air
          %O2 = Percent 02 by volume (dry basis)
         %CO = Percent CO by volume (dry basis)
          %N2 = Percent N2 by volume (dry basis)
         0.264 = Ratio of O2 to N2 in air, V/V
                                      D-37

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                            SECTION E.  METHOD 4

Subject                                                               page

1.  Method 4—determination of moisture content in stack gases
    (taken from Environmental Protection Agency Performance Test
    Methods manual)                                                   E-3

2.  Slides                                                            E-21
                                      E-l

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           METHOD 4—DETERMINATION OF MOISTURE CONTENT
                        IN STACK GASES
1.  Principle and Applicability
     1.1  Principle.  A gas sample is extracted at a constant rate from
the source; moisture is removed from the sample stream and determined
either volumetrically or gravimetrically.
     1.2  Applicability.  This method is applicable for determining the
moisture content of stack gas.
     Two procedures are given.  The first is a reference method, for
accurate determinations of moisture content (such as are needed to
calculate emission data).  The second is an approximation method, which
provides estimates of percent moisture to aid in setting isokinetic
sampling rates prior to a pollutant emission measurement run.  The
approximation method described herein is only a suggested approach;
alternative means for approximating the moisture content, e.g., drying
tubes, wet bulb-dry bulb techniques, condensation techniques, stoichio-
metric calculations, previous experience, etc., are also acceptable.
     The reference method is often conducted simultaneously with
a pollutant emission measurement run; when it is, calculation of percent
isokinetic, pollutant emission rate, etc., for the run shall be based  upon
the results of the reference method or its equivalent; these calculations
shall not be based upon the results of the approximation method, unless
the approximation method is shown, to the satisfaction of the Administrator,
U. S. Environmental Protection Agency, to be capable of yielding results
within 1 percent H.O of the reference method.
                            E-3

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     Note:  The reference method may yield questionable results
when applied to saturated gas streams or to streams that contain
water droplets.  Therefore, when these conditions exist or are
suspected, a second determination of the moisture content shall
be made simultaneously with the reference method, as follows:  Assume
that the gas stream is saturated.  Attach a temperature sensor [capable
of measuring to + 1° C (2° F)] to the reference method probe.  Measure
the stack gas temperature at each traverse point (see Section 2.2.1)
during the reference method traverse; calculate the average stack gas
temperature.  Next, determine the moisture percentage, either by:
(1) using a psychrometric chart and making appropriate corrections if
stack pressure is different from that of the chart, or (2) using
saturation vapor pressure tables.  In cases where the psychrometric
chart or the saturation vapor pressure tables are not applicable (based
on evaluation of the process), alternate methods, subject to the approval
of the Administrator, shall be used.
2.  Reference Method
     The procedure described in Method 5 for determining moisture
content is acceptable as a reference method.
     2.1  Apparatus.  A schematic of the sampling train used in
this reference method is shown in Figure 4-1.  All components
shall be maintained and calibrated according to the procedure
outlined in Method 5.
     2.1.1  Probe.  The probe is constructed of stainless steel or
glass tubing, sufficiently heated to prevent water condensation, and
is equipped with a filter, either in-stack (e.g., a plug of glass
                             E-4

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               FILTER
          (EITHER IN STACK
          OR OUT OF STACK)
STACK
WALL
CONDENSER ICE BATH SYSTEM INCLUDING
                SILICA GEL TUBE
                                          PROBE
m
r
cn
                                                                                         MAIN VALVE
                                                                                   AIR TIGHT
                                                                                     PUMP
                                    Figure 4-1.  Moisture sampling train-reference method.

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wool inserted into the end of the probe) or heated out-stack (e.g.,
as described in Method 5), to remove participate matter.
     When stack conditions permit, other metals or plastic tubing
may be used for the probe, subject to the approval of the
Administrator.
     2.1.2  Condenser.  The condenser consists of four impingers
connected in series with ground glass, leak-free fittings or any
similarly leak-free non-contaminating fittings.  The first, third, and
fourth impingers shall be of the Greenburg-Smith design, modified
by replacing the tip with a 1.3 centimeter (1/2 inch) ID glass tube
extending to about 1.3 cm (1/2 in.) from the bottom of the flask.
The second impinger shall be of the Greenburg-Smith design with the
standard tip.  Modifications (e.g., using flexible connections
between the impingers, using materials other than glass, or using
flexible vacuum lines to connect the filter holder to the condenser)
may be used, subject to the approval of the Administrator.
     The first two impingers shall contain known volumes of water,
the third shall be empty, and the fourth shall contain a known
weight of 6- to 16-mesh indicating type silica gel, or equivalent
desiccant.   If the silica gel has been previously used, dry at
175°C  (350°F) for 2 hours.  New silica gel may be used as received.
A thermometer, capable of measuring temperature to within 1°C
 (2°F), shall be placed at the outlet of.the fourth impinger, for
monitoring purposes.
      Alternatively,  any system may be used (subject  to  the  approval
  of the Administrator) that cools  the  sample gas  stream  and  allows
                             E-6

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measurement of both the water that has been condensed and the
moisture leaving the condenser, each to within 1 ml or 1 g.
Acceptable means are to measure the condensed water, either gravi-
metrically or volumetrically, and to measure the moisture leaving
the condenser by:   (1) monitoring the temperature and pressure at
the exit of the condenser and using Dalton's law of partial pressures,
or (2) passing the  sample gas stream through a tared silica gel (or
equivalent desiccant) trap, with exit gases kept below 20°C (68°F), and
determining the weight gain.
      If means other than silica gel are used to determine the amount of
moisture leaving the condenser, it is recommended that silica gel  (or
equivalent) still be used between the condenser system and pump, to
prevent moisture condensation in the pump  and metering devices and to
avoid  the need to make corrections for moisture in the metered volume.
      2.1.3  Cooling System.  An ice bath container and crushed ice
(or equivalent)  are used to aid in condensing moisture.
      2.1.4  Metering System.  This system  includes a vacuum gauge,
leak-free pump,  thermometers capable of measuring  temperature to
within 3°C  (5.4°F), dry  gas meter capable  of measuring volume to
within 2 percent, and related equipment as shown in Figure 4-1.
Other metering systems,  capable of maintaining  a constant sampling
rate  and determining sample gas volume, may be  used, subject to the
approval of the  Administrator.
      2.1.5  Barometer.   Mercury, aneroid,  or other barometer
capable of  measuring atmospheric pressure  to within 2.5  mm Hg  (0.1
in. Hg) may be used.   In many cases, the barometric reading may be
obtained from a  nearby national weather service station, in which
                             E-7

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case the station value (which is the absolute barometric pressure)
shall be requested and an adjustment for elevation differences
between the weather station and the sampling point shall be applied
at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m (100 ft) eleva-
tion increase or vice versa for elevation decrease.
     2.1.6  Graduated Cylinder and/or Balance.  The.se items are
used to measure condensed water and moisture caught in the silica
gel to within 1 ml or 0.5 g.  Graduated cylinders shall have
subdivisions no greater than 2 ml.  Most laboratory balances are
capable of weighing to the nearest 0.5 g or less.  These balances
are suitable for use here.
     2.2  Procedure.  The following procedure is written for a
condenser system (such as the impinger system described in Section
2.1.2) Incorporating volumetric analysis to measure the condensed
moisture* and silica gel and gravimetric analysis to measure the
moisture leaving the condenser.
     2.2.1  Unless otherwise specified by the Administrator, a minimum of
eight traverse  points shall be used for circular stacks having diameters
less than 0.61  m (24 in.), a minimum of nine points shall be used for
rectangular stacks having equivalent diameters  less than 0.61 m  (24 in.),
and  a minimum of twelve traverse  points shall be used  in all other cases.
The  traverse points shall be located according  to Method 1.  The use of
fewer points is subject to the approval of the  Administrator.  Select a
suitable probe  and probe  length  such that all traverse  points can be
sampled.   Consider sampling from opposite sides of the  stack  (four total
sampling ports) for large stacks, to permit  use of shorter probe  lengths.
Mark the probe with heat  resistant tape or by some other method  to
                             E-8

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denote the proper distance into the stack or duct for each sampling
point.  Place known volumes of water in the first two impingers.  Weigh
and record the.weight of the silica gel to the nearest 0.5 g, and
transfer the silica gel to the fourth impinger; alternatively, the
silica gel may first be transferred to the impinger, and the weight of
the silica gel plus impinger recorded.
     2.2.2  Select a total sampling time such that a minimum total gas
volume of 0.60 scm (21 scf) will be collected, at a rate no greater than
       •3
0.021 m /min  (0.75 cfm).  When both moisture content and pollutant
emission rate are to be determined, the moisture determination shall be
simultaneous with, and for the same total  length of time as, the pollutant
emission rate run, unless otherwise specified  in an applicable subpart of
the standards.
      2.2.3  Set  up the sampling  train  as shown in Figure 4-1.  Turn on
the probe heater and  (if  applicable) the filter  heating system to
temperatures  of  about  120°C  (248°F), to  prevent  water  condensation
ahead of  the  condenser; allow  time for the temperatures to  stabilize.
Place crushed ice in  the  ice bath  container.   It is  recommended,  but
not required,  that a  leak check  be done, as follows:   Disconnect  the
probe from  the  first  impinger  or (if applicable) from  the  filter  holder.
Plug  the  inlet  to the first  impinger  (or filter  holder) and pull  a
380 mm (15  in.)  Hg vacuum; a  lower vacuum  may be used, provided  that
 it is not exceeded during the  test.  A leakage rate  in excess of
4 percent of the average  sampling  rate or  0.00057 m  /min  (0.02  cfm),
whichever is  less,  is unacceptable.   Following the  leak check,
 reconnect the probe  to the sampling train.
                              E-9

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     2.2.4  During the sampling run, maintain a sampling rate
within 10 percent of constant rate, or as specified by the
Administrator. - For each run, record the data required on the
example data sheet shown in Figure 4-2.  Be sure to record the
dry gas meter reading at the beginning and end of each sampling
time increment and whenever sampling is halted.  Take other
appropriate readings at each sample point, at least once during
each time increment.
     2.2.5  To begin sampling, position the probe tip at the first
traverse point.  Immediately start the pump and adjust the flow to the
desired rate.  Traverse the cross section, sampling at each traverse
point for an equal length of time.  Add more ice and, if necessary, salt
to maintain a temperature of less than 20°C (68°F) at the silica gel
outlet.
     2.2.6  After collecting the sample, disconnect the probe from the
filter holder  (or from the first impinger) and conduct a leak check
(mandatory) as described in Section 2.2.3.  Record the leak rate.  If
the leakage rate exceeds the allowable rate, the tester shall either
reject the test results or shall correct the sample volume as in
Section 6.3 of Method 5.  Next, measure the volume of the moisture
condensed to  the nearest ml.  Determine the increase in weight of the
silica gel (or silica gel plus impinger) to the nearest 0.5 g.  Record
this information  (see example data sheet, Figure 4-3) and calculate the
moisture percentage, as described in 2.3 below.
     2.3  Calculations.  Carry out the following calculations, retaining
 at least one  extra decimal figure beyond that  of the acquired data.
 Round  off  figures after final calculation.
                            E-10

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PLANT	
LOCATION.
OPERATOR.
DATE	
RUN NO..
AMBIENT TEMPERATURE.
BAROMETRIC PRESSURE.
PROBE LENGTH m«W	
                                                 SCHEMATIC OF STACK CROSS SECTION
TRAVERSE POINT
NUMBER















TOTAL
SAMPLING
TIME
(8). min.
















AVERAGE
STACK
TEMPERATURE
°C (°F)

















PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE METER
(AH).
mmlin.) HjO

















METER
READING
GAS SAMPLE
VOLUME
m3(ft3)

















AVm
m3 (h*)

















GAS SAMPLE TEMPERATURE
AT DRY GAS METER
INLET
(Tminl. °C (°FI















Av».
Av».
OUTLET
(Tmoul), °C <°F)















Avj.

TEMPERATURE
OF GAS
LEAVING
CONDENSER OR
LAST IMPINGER,
°c <°n

















                                         Figure 4-2. Field moisture determination-reference method.

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FINAL
INITIAL
DIFFERENCE
IMPINGER
VOLUME.
ml



SILICA GEL
WEIGHT.
g



Figure 43.  Analytical data - reference method.
                  E-12

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2.3.1  Nomenclature.
*Lc   = Proportion of water vapor, by volume, in the gas stream.
 Wo
Mw    = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-mole).
Pm    = Absolute pressure, (for this method, same as barometric
        pressure) at the dry gas meter, mm Hg (in.  Hg).
Pstd  = standard absolute pressure, 760 mm Hg-(29.92 in. Hg).
R     = Ideal gas constant, 0.06236 (mm Hg)(m3)/(g-mole)(°K)
        for metric units and 21.85 (in. Hg)(ft3)/(lb-mole)(°R)
        for English units.
Tm    - Absolute temperature at meter, °K (°R).
Tstd  = Standard absolute temperature, 293°K (528°R).
Vm    = Dry gas volume measured by dry gas meter, dcm (dcf).
AV    = Incremental dry gas volume measured by dry gas meter at
        each traverse point, dcm (dcf).
V  /  . ,v = Dry gas volume measured by the dry gas meter,  corrected
        to standard conditions, dscm (dscf).
V c/stci\ = Volume of water vapor condensed corrected to  standard
        conditions, scm (scf).
V    / .,} = Volume of water vapor collected in silica gel  corrected
        to standard conditions, scm (scf).
V,.    = Final volume of condenser water, ml.
V.    = Initial volume, if any, of condenser water, ml.
toy    = Final weight of silica gel or silica gel plus impinger, g.
W-    = Initial weight of silica gel  or silica gel  plus  impinger, g.
Y     = Dry gas meter calibration factor.
PW    = Density of water, 0.9982 g/ml  (0.002201  Ib/ml).
                        E-13

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    2.3.2  Volume  of water  vapor  condensed.
    ,        -.   
-------
     2.3.5  Moisture Content.

                           +V
                              ws9(std)                 Equation4-4
      ws     Vwc(std) + Vwsg(std) + Vm(std)
     Note:  In saturated or moisture droplet-laden gas streams,  two
calculations of the moisture content of the stack gas shall  be made,  one
using a value based upon the saturated conditions (see Section 1.2),
and another based upon the results of the impinger analysis.   The
lower of these two values of B   shall be considered correct.
                              WS
     2.3.6  Verification of constant sampling rate. For each time
increment, determine the AV .  Calculate the average.  If the
                           m
value for any time increment differs from the average by more than
10 percent, reject the results and repeat the run.
3.  Approximation Method
     The approximation method described below is presented only  as
a suggested method (see Section  1.2).
     3.1  Apparatus.
     3.1.1  Probe.   Stainless steel or glass tubing, sufficiently
heated to prevent water condensation and equipped with a filter
(either in-stack or  heated out-stack) to remove particulate matter.
A plug of glass wool,  inserted into the end of the probe, is a
satisfactory  filter.
     3.1.2  Impingers.  Two midget impingers, each with 30 ml
capacity, or  equivalent.
     3.1.3  Ice Bath.  Container and ice, to aid in  condensing
moisture  in impingers.
                             E-15

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    3.1.4  Drying Tube.  Tube packed with new or regenerated 6- to 16-
mesh indicating-type silica gel (or equivalent desiccant), to dry the
sample gas and to protect the meter and pump.
     3.1.5  Valve.  Needle valve, to regulate the sample gas flow rate.
     3.1.6  Pump.  Leak-free, diaphragm type, or equivalent, to pull the
gas sample through the train.
     3.1.7  Volume meter.  Dry gas meter, sufficiently accurate to
measure the sample volume within 2%, and calibrated over the range of
flow rates and conditions actually encountered during sampling.
     3.1.8  Rate Meter.  Rotameter, to measure the flow range from
0. to 3 1pm (O.to 0.11 cfm).
     3.1.9  Graduated Cylinder.  25 ml.
     3.1.10  Barometer,  Mercury, aneroid, or other barometer, as
described in Section 2.1.5 above.
     3.1.11  Vacuum Gauge.  At least 760 mm Hg (30 in. Hg) gauge, to be
usad for the sampling leak check.
     3.2  Procedure.
     3.2.1  Place exactly 5 ml distilled water in each impinger.
Leak check the sampling train as follows:  Temporarily insert a vacuum
gauge at or near the probe inlet; then, plug the probe inlet and pull
a vacuum of at least 250 mm Hg (10 in. Hg).  Note the time rate of
change of the dry gas meter dial; alternatively, a rotameter (0-40
cc/min) may be temporarily attached to the dry gas meter outlet to.
determine the leakage rate.  A leak rate not in excess of 2 percent
of the average sampling rate is acceptable.  Note:  Carefully release
the probe inlet plug before turning off the pump.
                           E-16

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  HEATED PROBE
               \
SILICA GEL TUBE
              \
RATE METER,

    VALVE
FILTER
(GLASS WOOL)
   ICE BATH
    MIDGET IMPINGERS
             PUMP
         Figure 4-4.  Moisture-sampling train - approximation method.
   LOCATION
   TEST
                               COMMENTS
   DATE
   OPERATOR
   BAROMETRIC PRESSURE
CLOCK TIME





GAS VOLUME THROUGH
METER. (Vm),
m3 (ft3)





RATE METER SETTING
m3/min. (ft^/min.)





METER TEMPERATURE.
°C (°F)





     Figure 4-5. Field moisture determination - approximation method.
                                E-17

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    3.2.2  Connect the probe, insert it into the stack, and sample



at a constant rate of 2 1pm (0.071 cfm).  Continue sampling until



the dry gas meter registers about 30 liters (1.1 ft ) or until



visible liquid droplets are carried over from the first impinger



to the second.  Record temperature, pressure, and dry gas meter



readings as required by Figure 4-5.



     3.2.3  After collecting the sample, combine the contents of



the two impingers and measure the volume to the nearest 0.5 ml.



     3.3  Calculations.  The calculation method presented is



designed to estimate the moisture in the stack gas; therefore,



other data, which are only necessary for accurate moisture determina-



tions, are not collected.  The following equations adequately



estimate the moisture content, for the purpose of determining



isokinetic sampling rate settings.



     3.3.1  Nomenclature.



     B     = Approximate proportion, by volume, of water vapor  in
      Will


              the  gas stream  leaving the second  impinger, 0.025.



     BU,C   = Water vapor in  the  gas stream, proportion by volume.
      ws


     M     = Molecular weight of water, 18.0 g/g-mole  (18.0  Ib/lb-mole)
      W


     P     = Absolute pressure (for this method,  same as barometric



              pressure) at  the dry  gas meter.



     P  . .  =  Standard absolute pressure, 760 mm Hg  (29.92 in. Hg).



     R     =  Ideal gas constant, 0.06236 (m Hq)(m3)/(n-mole)(°K) for



              metric units  and 21.85 (in. Hg)(ft3)/lb-mole)(°R)  for



              English units.
                         E-18

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     T      = Absolute temperature at meter, °K (°R).
     Tstd   = s.tandard absolute temperature, 293°K (528°R).
     V-     = Final volume of impinger contents, ml.
     V.j     = Initial volume of impinger contents, ml.
     V      = Dry gas volume measured by dry gas meter, dcm (dcf).
     \L(std)= Dry gas volume measured by dry gas meter, corrected
              to standard conditions, dscm (dscf).
     V/std\=Volume of water vapor condensed, corrected to
              standard conditions, scm (scf).
     Y      = Dry gas meter calibration factor.
     a      = Density of water, 0.9982 g/ml (0.002201 Ib/ml).
      w
     3.3.2  Volume of water vapor collected.

     tf            (Vf-
     V(std)  -

               = K1 (Vf - V^                         Equation 4-5
Where:
     K^ = 0.001333 m /ml for metric units.
        = 0.04707 ft3/ml for English units.
     3.3.3  Gas Volume.
     if        _  II  V I   '"   I /   3 I" I           V  P
     Vm(std)  -  Vm Y ' *	  M  -T- )  _ „  v    m  •
                                                   m
                                                      Equation 4-6
                           E-19

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     where:
          K2 = 0.3858  K/mm Hg for metric units.
             = 17.64 °R/in. Hg for English units.
     3.3.4  Approximate moisture content.
                                                 Vwc(std)
     Bws
                                                          Equation 4-7
4.  Calibration
     4.1  For the reference method, calibrate equipment as specified in
the following sections of Method 5:  Section 5.3 (metering system);
Section 5.5 (temperature gauges); and Section 5.7 (barometer).  The
recommended leak check of the metering system (Section 5.6 of Method 5)
also applies to the reference method.  For the approximation method, use
the procedures outlined in Section 5.1.1 of Method 6 to calibrate the
metering system, and the procedure of Method 5, Section 5.7 to calibrate
the barometer.
5.  Bibliography
     1.  Air Pollution Engineering Manual (Second Edition). Danielson,
J. A.  (ed.).  U. S. Environmental Protection Agency, Office of Air
Quality Planning and Standards.  Research Triangle Park, N. C. Publication
No. AP-40.  1973.
     2. Devorkin, Howard, et al.  Air Pollution Source Testing Manual.
Air Pollution Control District,  Los Angeles, Calif.  November, 1963.
      3. Methods for Determination of Velocity, Volume, Dust and Mist
 Content of Gases.  Western Precipitation Division of Joy Manufacturing
 Co.  Los Angeles,  Calif.  Bulletin WP-50.   1968.
                                   E-20

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 SLIDE 105-0                                               NOTES


    METHOD — 4

Determination of Moisture
     in Stack Gases
 SLIDE 105-1
                PRINCIPLE
  A sample is extracted at a constant rate. Mois-
ture  is removed and determined volumetrically
or gravimetrically.
             APPLICABILITY
  The method  is applicable for determining
moisture content of stack gas.
  SLIDE 105-2


          SUMMARY OF METHODS

             REFERENCE METHOD
 • used for accurate determination of moisture content
 • usually conducted simultaneously with  a  pollutant
   measurement run
 • results used to calculate isokinetics  and  pollutant
   emission rate
           APPROMIXATION METHOD
 • used to estimate percent moisture to aid in setting iso-
   kinetic sampling rate
                                       E-21

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 SLIDE 105-3
NOTES
(cont.)        SUMMARY OF METHODS

             PARTIAL PRESSURE METHOD
    • used to determine moisture content in saturated gas
     streams and gas streams that contain water droplets.

           WET BULB - DRY BULB METHOD
    • a popular alternative approximation method for low
     temperature applications.
 SLIDE  105-4
 MOISTURE SAMPLING TRAIN (REFERENCE METHOD).
      FILTER
   (CITHER IN STACK
   OR OUT Of STACK)
                             CONDENSER-ICE BATH SVSTEM
                              INCLUDING SILICA GEL TUBE
  SLIDE 105-5
                   PROCEDURE
  1. Determine traverse points using Method 1.
  2. Select sampling time such that minimum gas volume
    of 21 SCF will be collected at rate no greater than 0.75
    CFM.
  3. Leak-check sampling train (optional).
  4. Maintain sampling rate within 10% of constant rate.
  5. After sampling, leak-check sampling train (mandatory).
  6. Verify the constant sampling rate.
                                        E-23

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  SLIDE 105-6
                                                               NOTES
          MOISTURE SAMPLING TRAIN
            APPROXIMATION METHOD
  SLIDE  105-7
                PROCEDURE
1. Place 5.0 ml of distilled water in each impinger.
2. Assemble and leak-check sampling train.
3. Sample at a constant rate of 0.07 CFM until a sample
  volume of 1.1 ft' is obtained.
4. Combine contents of impingers and measure volume
  to nearest 0.5 ml.
 SLIDE  105-8

         PARTIAL PRESSURE METHOD
1. Assume saturation.
2. Attach temperature sensor to reference method
  probe.
3. Measure stack gas temperature at each traverse
  point.
4. Calculate the average stack gas temperature.
5. Determine moisture fraction using saturation vapor
  pressure table.
                                      E-25

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 SLIDE  105-9                                            NOTES

MOISTURE EQUATION - PARTIAL PRESSURE

                      S.V.R
          Where:  B^ = proportion (by volume)  of water
                     vapor in a gas mixture
               S.V.R - saturated vapor pressure of water
                     at average stack temperature
                  P = absolute pressure of the stack
 SLIDE 105-10

  EXAMPLE MOISTURE CALCULATION
                  DATA
Average stack temperature            140°F
Barometric pressure              29.2 in. Hg
Static pressure                  + 0.5 in. Hg
Saturated vapor pressure           5.88 in. Hg

             CALCULATION


              _    5.88

                •" 29.7



              B_ = 0.1980
  SLIDE  105-11

        WET BULB- DRY BULB METHOD

 1. Measure the wet bulb temperature.

 2. Measure the dry bulb temperature.

 3. Estimate moisture content using psychrometric chart.


                                   E-27

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 SLIDE 105-12
                                           NOTES
               MOISTURE EQUATION
              (WET BULB - DRY BULB)
                           V.R
Where:  V.R = S.V.R -
(0.000367) (P) ft,-U
      S.V.R = saturated water vapor pressure at the wet
            bulb temperature
         P = absolute pressure in the stack
         td = dry bulb temperature
         t, = wet bulb temperature
       V.R = water vapor pressure
                                      E-29

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                            SECTION F.  METHOD 5

Subject                                                               Page

1.  Method 5--determination of participate emissions from stationary
    sources (taken from Environmental Protection Agency Performance
    Test Methods manual)                                              F-l

2.  Slides                                                            F-43
                                      F-l

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             METHOD 5—DETERMINATION OF PARTICIPATE
               EMISSIONS FROM STATIONARY SOURCES
1.  Principle and Applicability
     1.1  Principle.  Participate matter is withdrawn isokinetically
from the source and collected on a glass fiber filter maintained at
a temperature in the range of 120 +_14°C (248 +_25°F) or such other
temperature as specified by an applicable subpart of the standards
or approved by the Administrator, U. S. Environmental Protection
Agency, for a particular application.  The particulate mass, which
includes any material that condenses at or above the filtration
temperature, is determined gravimetrically after removal of uncombined
water.
     1.2  Applicability.  This method is applicable for the determina-
tion of particulate emissions from stationary sources.
2.  Apparatus
     2.1  Sampling Train.  A schematic of the sampling train used in
this method is shown in Figure 5-1.  Complete construction details
are given in APTD-0581  (Citation 2 in Section 7); commercial models
of this train are also  available.  For changes from APTD-0581 and
for allowable modifications of the train shown in Figure 5-1, see
the following subsections.
     The operating  and  maintenance procedures for the sampling train
are described in APTD-0576  (Citation 3 in Section 7).  Since correct
usage  is important  in obtaining valid results, all users should read
APTD-0576 and adopt the operating and maintenance procedures outlined
in it,  unless otherwise specified herein.  The sampling train consists
of the  following components:
                            F-3

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     2.1.1  Probe Nozzle.   Stainless steel (316) or glass with sharp,
tapered leading edge.  The angle of taper shall be ^30° and the
taper shall be on the outside to preserve a constant internal  diameter.
The probe nozzle shall be of the button-hook or elbow design,  unless
otherwise specified by the Administrator.  If made of stainless steel,
the nozzle shall be constructed from seamless tubing; other materials
of construction may be used, subject to the approval of the
Administrator.
     A range of nozzle sizes suitable for isokinetic sampling should
be available, e.g., 0.32 to 1.27 cm (1/8 to 1/2 in.)--or, larger if
higher volume sampling trains are used—inside diameter (ID) nozzles
in increments of 0.16 cm (1/16 in.).  Each nozzle shall be calibrated
according to the procedures outlined in Section 5.
     2.1.2  Probe Liner.  Borosilicate or quartz glass tubing with a
heating system capable of maintaining a gas temperature at the exit
end during sampling of 120 +_ 14°C (248 + 25°F), or such other tempera-
ture as specified by  an applicable  subpart of  the standards or
approved  by the Administrator for a particular application.   (The
tester may opt to operate the equipment at a temperature lower than
that specified.)  Since the  actual  temperature at the  outlet  of the
probe  is  not  usually  monitored during sampling, probes constructed
according to APTD-0581 and utilizing the  calibration curves of
APTD-0576 (or calibrated according  to the  procedure outlined  in
APTD-0576) will  be considered acceptable.
                           F-4

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       o:
i
en
                      TEMPERATURE SENSOR
            - PROBE

             TEMPERATURE
               SENSOR
                                                         IMPINGER TRAIN OPTIONAL.MAY BE REPLACED
                                                              BY AN EQUIVALENT CONDENSER
                                           HEATED AREA   THERMOMETER
                                                                          THERMOMETER
 PITOT TUBE
                       PROBE
REVERSE TYPE
 PITOT TUBE
                             PITOTMANOMETER        IMPINGERS               ICE BATH
                                                            BY PASS VALVE
                                     ORIFICE
                           THERMOMETERS
                                                                            VACUUM
                                                                            GAUGE
                                                                     MAIN VALVE
                                       DRY GAS METER
                                        AIRTIGHT
                                          PUMP
                                                                                         CHECK
                                                                                         VALVE
                                                                                         VACUUM
                                                                                           LINE
                                       F.ujuro 5 1. Paniculate sampling (r,im.

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     Either borosilicate or quartz glass probe liners may be used
for stack temperatures up to about 480°C (900°F); quartz liners
shall be used, for temperatures between 480 and 900°C (900 and 1650°F).
Both types of liners may be used at higher temperatures than specified
for short periods of time, subject to the approval of the Administrator.
The softening temperature for borosilicate is 820°C (1508°F), and for
quartz it is 1500°C (2732°F).
     Whenever practical, every effort should be made to use borosilicate
or quartz glass probe liners.  Alternatively, metal liners (e.g., 316
stainless steel, Incoloy 825,  or other corrosion resistant metals)
made of seamless tubing may be used, subject to the approval of the
Administrator.
     2.1.3  Pitot Tube.  Type S, as described in Section 2.1 of
Method 2, or other device approved by the Administrator.  The pi tot
tube shall be attached to the probe (as shown in Figure 5-1) to allow
constant monitoring of the stack gas velocity.  The impact (high
pressure) opening plane of the pi tot tube shall be even with or
above the nozzle entry plane  (see Method 2, Figure 2-6b) during
sampling.  The Type S pitot tube assembly shall have a known coefficient,
determined as outlined in Section 4 of Method 2.
     2.1.4  Differential Pressure Gauge.  Inclined manometer or
equivalent device (two), as described in Section 2.2 of Method 2.
One  manometer shall be used for velocity head (Ap) readings, and
the  other, for orifice differential pressure readings.
  Mention of trade  names or specific products does not constitute
  endorsement by the  Environmental Protection Agency.
                                  F-6

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     2.1.5  Filter Holder.  Borosllicate glass, with a glass frit
filter support and a silicone rubber gasket.  Other materials of
construction Te.g., stainless steel, Teflon, Viton) may be used,
subject to the approval of the Administrator.  The holder design shall
provide a positive seal against leakage from the outside or around the
filter.  The holder shall be attached immediately.at the outlet of
the probe (or cyclone, if used).
     2.1.6  Filter Heating System.  Any heating system capable of
maintaining a temperature around the filter holder during sampling
of 120 + 14°C (248 +_25°F), or such other temperature as specified by
an applicable subpart  of the standards or approved by the
Administrator for a particular application.  Alternatively, the tester
                                             /
may opt to operate the equipment at a temperature  lower than that
Specified.  A temperature gauge capable of measuring temperature to
within 3°C  (5.4°F) shall be installed so that  the  temperature around
the filter holder can  be regulated and monitored during sampling.
Heating systems  other  than the one shown in APTD-0581 may be used.
     2.1.7  Condenser. The following system shall be used  to determine
the stack gas moisture content:  Four impingers connected in series
with leak-free ground  glass fittings or any  similar  leak-free non-
contaminating fittings.  The first, third,  and fourth impingers shall
be of  the Greenburg-Smith design, modified  by  replacing the tip with
a 1.3  cm  (1/2 in.)  ID  glass tube extending  to  about  1.3 cm  (1/2 in.)
from the  bottom  of  the flask.  The second impinger shall  be of  the
Greenburg-Smith  design with the standard tip.   Modifications  (e.g.,
                            F-7

-------
using flexible connections between the impingers, using materials
other than glass, or using flexible vacuum lines to connect the
filter holder* to the condenser) may be used, subject to the
approval of the Administrator.  The first and second impingers shall
contain known quantities of water (Section 4.1.3), the third shall
be empty, and the fourth shall contain a known weight of silica gel,
or equivalent desiccant.  A thermometer, capable of measuring tempera-
ture to within 1°C (2°F) shall be placed at the outlet of the fourth
impinger for monitoring purposes.
     Alternatively, any system that cools the sample gas stream and
allows measurement of the water condensed and moisture leaving the
condenser, each to within 1 ml or 1 g may be used, subject to the
approval of the Administrator.  Acceptable means are to measure the
condensed water either gravimetrically or volumetrically and to measure
the moisture leaving the condenser by:  (1) monitoring the temperature
and pressure at the exit of the condenser and using Dal ton's law of
partial pressures; or (2) passing the sample gas stream through a
tared silica gel (or equivalent desiccant) trap with exit gases kept
below 20°C (68°F) and determining the weight gain.
     If means other than silica gel are used to determine the amount of
moisture leaving the condenser, it is recommended that silica gel (or
equivalent) still be used between the condenser system and pump to
prevent moisture condensation  in the pump and metering devices and
                                         X
to avoid the need to make corrections for moisture in the metered
volume.
                            F-8

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     Note:   If a determination of the participate matter collected
in the impingers is desired in addition to moisture content, the
impinger system described above shall be used, without.modification.
Individual  States or control agencies requiring this information
shall be contacted as to the sample recovery and analysis of the
impinger contents.
     2.1.8  Metering System.  Vacuum gauge, leak-free pump, thermometers
capable of measuring temperature to within 3°C (5.4°F), dry gas meter
capable of measuring volume to within 2 percent, and related equipment,
as shown in Figure 5-1.  Other metering systems capable of maintaining
sampling rates within 10 percent of isokinetic and of determining
sample volumes to within 2 percent may be used, subject to the approval
of the Administrator.  When the metering system is used in conjunction
with a pi tot tube, the system shall enable checks of isokinetic rates.
     Sampling trains utilizing metering systems designed for higher
flow rates than that described in APTD-0581 or APTD-0576 may be used
provided that the specifications of this method are met.
     2.1.9  Barometer.  Mercury, aneroid, or other barometer capable
of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
In many cases, the barometric reading may be obtained from a nearby
national weather  service station, in which case the station value
(which is the absolute barometric pressure) shall be requested and
an adjustment for elevation differences between the weather station
and sampling point shall be applied at a rate of minus 2.5 mm Hg
(0.1 in. Hg) per  30 m  (100 ft) elevation increase or vice versa
for elevation decrease.
                                   F-9

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     2.1.10  Gas Density Determination Equipment.   Temperature
sensor and pressure gauge, as described in Sections 2.3 and 2.4 of
Method 2, and gas analyzer, if necessary, as described in Method 3.
The temperature sensor shall, preferably, be permanently attached
to the pi tot tube or sampling probe in a fixed configuration, such
that the tip of the sensor extends beyond the leading edge of the
probe sheath and does not touch any metal.  Alternatively, the sensor
may be attched just prior to use in the field.  Note, however, that
if the temperature sensor is attached in the field, the sensor must
be placed in an interference-free arrangement with respect to the
Type S pitot tube openings (see Method 2, Figure 2-7).  As a second
alternative, if a difference of not more than 1 percent in the average
velocity measurement is to be introduced, the temperature gauge need
not be attached to the probe or pitot tube.  (This alternative is
subject to the approval of the Administrator.)
     2.2  Sample Recovery.  The following items are needed:
     2.2.1  Probe-Liner and Probe-Nozzle Brushes.   Nylon bristle
brushes with stainless steel wire handles.  The probe brush shall
have extensions  (at least as long as the probe) of stainless steel,
Nylon, Teflon, or similarly inert material.  The brushes shall be
properly sized and shaped to brush out the probe liner and nozzle.
     2.2.2  Wash Bottles—Two.  Glass wash bottles are recommended;
polyethylene wash bottles may be used at the option of the tester.
It  is  recommended that acetone not be stored in polyethylene bottles
for longer  than  a month.
                                   F-10

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     2.2.3  Glass Sample Storage Containers.  Chemically resistant,
borosilicate glass bottles, for acetone washes, 500 ml or 1000 ml.
Screw cap liners shall either be rubber-backed Teflon or shall be
constructed so as to be leak-free and resistant to chemical  attack
by acetone.  (Narrow mouth glass bottles have been found to be less
prone to leakage.)  Alternatively, polyethylene bottles may be used.
     2.2.4  Petri Dishes.  For filter samples, glass or polyethylene,
unless otherwise specified by the Administrator.
     2.2.5  Graduated Cylinder and/or Balance.  To measure condensed
water to within 1 ml or 1 g.  Graduated cylinders shall have sub-
divisions no greater than 2 ml.  Most laboratory balances are capable
of weighing to the nearest 0.5 g or  less.   Any of these balances is
suitable for use here and in Section 2.3.4.
     2.2.6  Plastic Storage Containers.  Air-tight containers to
store silica gel.
     2.2.7  Funnel and Rubber Policeman.  To  aid in  transfer of silica
gel  to container; not necessary if silica gel  is weighed in the field.
     2.2.8  Funnel.  Glass or polyethylene, to aid in  sample recovery.
     2.3  Analysis.   For analysis, the  following equipment is needed:
     2.3.1  Glass Weighing Dishes.
     2.3.2  Desiccator.
     2.3.3  Analytical Balance.  To  measure to within  0.1 mg.
     2.3.4  Balance.  To measure to  within  0.5 g.
     2.3.5  Beakers.  250 ml.
     2.3.6  Hygrometer.  To measure  the relative humidity of the
laboratory  environment.
                            F-ll

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     2.3.7  Temperature Gauge.  To measure the temperature of the
laboratory environment.
3.  Reagents'
     3.1  Sampling.  The reagents used in sampling are as follows:
     3.1.1  Filters.  Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent penetration)
on 0.3-micron dioctyl phthalate smoke particles.  The filter efficiency
test shall be conducted in accordance with ASTM standard method
D 2986-71.  Test data from the supplier's quality control program are
sufficient for this purpose.
     In  sources containing S02 or S03,  the  filter material must of a type  that
is unreactive to SCL or SCU.  Citation  10  in Section 7 may be used to  select
the appropriate filter.
      3.1.2   Silica Gel.   Indicating type, 6  to 16 mesh.   If previously
used, dry at 175°C (350°F)  for 2  hours.   New silica  gel  may be used
as  received.  Alternatively,  other types  of  desiccants  (equivalent or
better)  may  be used,  subject  to the approval  of the  Administrator.
      3.1.3   Water.  When  analysis of  the material caught in the
impingers is required,  distilled  water shall  be used.   Run blanks
prior to field use to eliminate a high blank on test samples.
      3.1.4   Crushed Ice.
      3.1.5   Stopcock Grease.   Acetone-insoluble, heat-stable silicone
grease.   This  is  not necessary if screw-on connectors with Teflon
sleeves, or  similar,  are  used.  Alternatively, other types of stopcock
grease  may  be  used, subject to the approval  of the Administrator.
                                 F-12

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     3.2  Sample Recovery.  Acetone—reagent grade, <0.001  percent
residue, in glass bottles—is required.  Acetone from metal  containers
generally has a high residue blank and should not be used.   Sometimes,
suppliers transfer acetone to glass bottles from metal containers;
thus, acetone blanks shall be run prior to field use and only
acetone with low blank values (<0.001 percent) shall be used.  In
no case shall a blank value of greater than 0.001 percent of the
weight of acetone used be subtracted from the sample weight.
     3.3  Analysis.  Two reagents are required for the analysis:
     3.3.1  Acetone.  Same as 3.2.
     3.3.2  Desiccant.  Anhydrous calcium sulfate, indicating type.
Alternatively, other types of desiccants may be used, subject to the
approval of the Administrator.
4.   Procedure
     4.1  Sampling.  The complexity of this method is such that, in
order to obtain reliable results, testers should be trained and
experienced with the test procedures.
     4.1.1  Pretest Preparation.  All  the components  shall be maintained
and  calibrated according  to  the  procedure described in APTD-0576, unless
otherwise specified herein.
     Weigh several 200 to 300 g  portions of silica gel in air-tight
containers to  the  nearest 0.5 g.  Record the total weight of the
silica  gel plus  container, on each container.  As an  alternative, the
silica  gel need  not be preweighed, but may be weighed directly in its
impinger or sampling holder  just prior to train assembly.
     Check filters visually  against light for irregularities and
flaws or pinhole leaks.   Label filters of the proper  diameter on the
back side near the edge  using numbering machine ink.  As an alternative,
                               F-13

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label the shipping containers (glass or plastic petri dishes) and
keep the filters in these containers at all times except during
sampling and weighing.
     Desiccate the filters at 20 + 5.6°C (68 + 10°F) and ambient
pressure for at least 24 hours and weigh at intervals of at least
6 hours to a constant weight, i.e., <0.5 mg change from previous
weighing; record results to the nearest 0.1 mg.  During each
weighing the filter must not be exposed to the laboratory atmosphere
for a period greater than 2 minutes and a relative humidity above
50 percent.  Alternatively (unless otherwise specified by the
Administrator), the filters may be oven dried at 105°C (220°F) for
2 to 3 hours, desiccated for 2 hours, and weighed.  Procedures other
than those described, which account for relative humidity effects,
may be used, subject to the approval of the Administrator.
     4.1.2  Preliminary Determinations.  Select the sampling site and
the minimum number of sampling points according to Method 1 or as
specified by the Administrator.  Determine the stack pressure,
temperature, and the range of velocity heads using Method 2; it is
recommended that a leak-check of the pitot lines (see Method 2,
Section 3.1) be performed.  Determine the moisture content using
Approximation Method 4 or its alternatives for the purpose of making
isokinetic sampling rate settings.  Determine the stack gas dry
molecular weight, as described in Method 2, Section 3.6; if integrated
Method 3 sampling is used for molecular weight determination, the
integrated bag sample shall be taken simultaneously with, and for
the  same total length of time as, the particulate sample run.
                                  F-14

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     Select a nozzle size based on the range of velocity heads, such
that it is not necessary to change the nozzle size  in order to maintain
isokinetic sampling rates.  During the run, do not  change the nozzle
size.  Ensure that the proper differential pressure gauge is chosen for
the range of velocity heads encountered  (see Section 2.2 of Method 2).
     Select a suitable probe liner and probe length such that all
traverse points can be sampled.  For large stacks,  consider sampling
from opposite sides of the stack to reduce the length of probes.
     Select a total sampling time greater than or equal to the minimum
total sampling time specified in the test procedures for the specific
industry such that (1) the sampling time per point  is not less than 2
min.(or some greater time interval as specified by  the Administrator),
and (2) the sample volume taken (corrected to standard conditions) will
exceed the required minimum total gas sample volume.  The latter is
based on an approximate average sampling rate.
     It is recommended that the number of  minutes sampled at each  point be
an  integer or an integer plus one-half minute,  in order to avoid  timekeeping
errors.  The sampling time at each point shall  be the same.
      In some circumstances,  e.g., batch cycles, it may be necessary to
 sample for shorter times at the traverse points and to obtain  smaller
 gas sample volumes.   In these cases, the Administrator's  approval  must
 first be obtained.
      4.1.3  Preparation of Collection Train.   During  preparation and
 assembly of the sampling train, keep all openings where contamination
                                 F-15

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can occur covered until  just prior to assembly or until  sampling
is about to begin.
     Place 100 ml of water in each of the first two impingers, leave
the third impinger empty, and transfer approximately 200 to 300 g of
preweighed silica gel from its container to the fourth impinger.
More silica gel may be used, but care should be taken to ensure that
it is not entrained and carried out from the impinger during sampling.
Place the container in a clean place for later use in the sample
recovery.  Alternatively, the weight of the silica gel plus impinger
may be determined to the nearest 0.5 g and recorded.
     Using a tweezer or clean disposable surgical gloves, place a
labeled  (identified) and weighed filter in the filter holder.  Be sure
that the filter  is properly  centered and the gasket properly placed
so as to prevent the sample  gas stream from circumventing the filter.
Check the filter for tears after assembly is completed.
     When glass  liners are used, install the selected nozzle using
a  Viton  A 0-ring when stack  temperatures are less than 260°C  (500'F)
and an asbestos  string gasket when  temperatures  are higher.  See
APTD-0576 for  details.   Other connecting systems using either  316
stainless steel  or Teflon ferrules  may  be used.  When metal  liners
are used,  install the nozzle as above or by a  leak-free  direct
mechanical  connection.   Mark the  probe  with heat resistant  tape or
by some  other  method to  denote  the  proper distance  into  the stack or
duct  for each  sampling  point.
                          F-16

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     Set up the train as in Figure 5-1, using (if necessary)  a very
light coat of silicone grease on all ground glass joints, greasing
only the outer-portion (see APTD-0576) to avoid possibility of
contamination by the silicone grease.  Subject to the approval of
the Administrator, a glass cyclone may be used between the probe and
filter holder when the total paniculate catch is expected to exceed
100 mg or when water droplets are present in the stack gas.
     Place crushed ice around the impingers.
     4.1.4  Leak-Check Procedures.
     4.1.4.1  Pretest Leak-Check.  A pretest leak-check is recommended,
but not required.  If the tester opts to conduct the pretest leak-check,
the following procedure shall be used.
     After the sampling train has been assembled, turn on and set the
filter and probe heating systems at the desired operating temperatures.
Allow time for the temperatures to stabilize.  If a Viton A 0-ring or
other leak-free connection is used in assembling the probe nozzle to
the probe liner, leak-check the train at the sampling site by plugging
the nozzle and pulling a 380 mm Hg (15 in. Hg) vacuum.
     Note:  A lower vacuum may be used, provided that it is not exceeded
during the test.
     If an asbestos string is used, do not connect the probe to the
train during the leak-check.  Instead, leak-check the train by first
plugging the inlet to the filter holder (cyclone, if applicable) and
pulling a 380 mm Hg (15 in. Hg) vacuum (see Note immediately above).
Then connect the probe to the train and leak-check at about 25 mm Hg
(1 in. Hg) vacuum; alternatively, the probe may be leak-checked with
                                   F-17

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 the  rest of the sampling train, in one step, at 380 mm Hg (15 in.  Hg)
 vacuum.  Leakage rates in excess of 4 percent of the average sampling
                 2
 rate or 0.00057 m /min (0.02 cfm), whichever is less, are unacceptable.
     The following leak-check instructions for the sampling train
 described in APTD-0576 and APTD-0581 may be helpful.  Start the pump
 with bypass valve fully open and coarse adjust valve completely closed.
 Partially open the coarse adjust valve and slowly close the bypass
 valve until the desired vacuum is reached.  Do not reverse direction
 of bypass valve; this will cause water to back up into the filter
 holder.  If the desired vacuum is exceeded, either leak-check at
 this higher vacuum or end the leak check as shown below and start over.
     When the leak-check is completed, first slowly remove the plug
from the inlet to the probe, filter holder, or cyclone (if applicable)
and immediately turn off the vacuum pump.  This prevents the water in
the impingers from being forced backward into the filter holder and
silica gel  from being entrained backward into the third impinger.
     4.1.4.2  Leak-Checks During Sample Run.  If, during the sampling
run, a component (e.g., filter assembly or impinger) change becomes
necessary,  a leak-check shall be conducted immediately before the
change is made.  The leak-check shall be done according to the procedure
outlined in Section 4.1.4.1 above, except that it shall be done at a
vacuum equal to or greater than the maximum value recorded up to that
point in the test.  If the leakage rate is found to be no greater than
0.00057 m /min (0.02 cfm) or 4 percent of the average sampling rate
                         F-18

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(whichever is less), the results are acceptable, and no correction
will need to be applied to the total volume of dry gas metered;
if, however, a higher leakage rate is obtained, the tester shall
either record the leakage rate and plan to correct the sample volume
as shown in Section 6.3 of this method, or shall void the sampling run.
     Immediately after component changes, leak-checks are optional;
if such leak-checks are done, the procedure outlined in Section 4.1.4.1
above shall be used.
     4.1.4.3  Post-test Leak-Check.  A leak-check is mandatory at the
conclusion of each sampling run.  The leak-check shall be done in
accordance with the procedures outlined in Section 4.1.4.1, except
that it shall be conducted at a vacuum equal to or greater than the
maximum value reached during the sampling run.  If the leakage rate
is found to be no greater than 0.00057 m /min  (0.02 cfm) or 4 percent
of the average sampling rate (whichever is less), the results are
acceptable, and no correction need  be applied  to the total volume of
dry gas metered.  If, however, a higher leakage rate is obtained, the
tester shall either record the leakage rate and correct the sample
volume as  shown in Section 6.3 of this method,  or shall void the
sampling run.
     4.1.5 Particulate Train Operation.   During the sampling run,
maintain an isokinetic sampling rate  (within  10 percent of true
isokinetic unless otherwise  specified by the Administrator) and a
temperature around  the filter of 120 +. 14eC  (248 £ 25°F), or such other
                                   F-19

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temperature as specified by an applicable subpart of the standards
or approved by the Administrator.
     For each run, record the data required on a data sheet such as
the one shown in Figure 5-2.   Be sure to record the initial dry gas
meter reading.  Record the dry gas meter readings at the beginning
and end of each sampling time increment, when changes in flow rates
are made, before and after each leak check, and when sampling is halted.
Take other readings required by Figure 5-2 at least once at each sample
point during each time increment and additional readings when significant
changes (20 percent variation in velocity head readings) necessitate
additional adjustments in flow rate.  Level and zero the manometer.
Because the manometer level and zero may drift due to vibrations and
temperature changes, make periodic checks during the traverse.
     Clean the portholes prior to the test run to minimize the chance
of sampling deposited material.  To begin sampling, remove the nozzle
cap, verify that the filter and probe heating systems are up to
temperature, and that the pi tot tube and probe are properly positioned.
Position the nozzle at the first traverse point with the tip pointing
directly into the gas stream.  Immediately start the pump and adjust
the flow to isokinetic conditions.  Nomographs are available, which
aid in the rapid adjustment of the isokinetic sampling rate without
excessive computations.  These nomographs are designed for use when the
Type S pitot tube coefficient is 0.85 +0.02, and the stack gas
equivalent density  (dry molecular weight) is equal to 29 +_4.  APTD-0576
details the procedure for using the nomographs.  If C  and M. are
outside the above stated ranges, do not use the nomographs unless
appropriate steps (see Citation 7 in Section 7) are taken  to compensate
for the deviations.
                            F-20

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PLANT
LOCATION.
OPERATOR.
DATE	
RUN NO.
SAMPLE BOX NO..
METER BOX NO._
METERAH@	
CFACTOR	
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE.
ASSUMED MOISTURE. %_
PROBE LENGTH, m 
°C (°F)














VELOCITY
HEAD
|APS),
mmlin.JH^O














PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE
METER
mm HjO

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      When the stack is under significant negative pressure (height
 of  impinger stem), take care to close the coarse adjust valve before
 inserting the probe into the stack to prevent water from backing into
 the filter holder.  If necessary, the pump may be turned on with the
 coarse adjust valve closed.   .
     When the probe is in position, block off the openings around
 the probe and porthole to prevent unrepresentative dilution of the
 gas stream.
     Traverse the stack cross-section, as required by Method 1 or as
 specified by the Administrator, being careful not to bump the probe
 nozzle into the  stack walls  when sampling near the walls or when
 removing or inserting the probe through the portholes; this minimizes
 the chance of extracting deposited material.
     During the  test run, make periodic adjustments to keep the
temperature around the filter holder at the proper level; add more
 ice and, if necessary, salt  to maintain a temperature of less than
20°C (68°F)  at the condenser/silica gel outlet.  Also, periodically
check the level  and zero of  the manometer.
     If the pressure drop across the filter becomes too high, making
 isokinetic sampling difficult to maintain, the filter may be replaced
 in the midst of a sample run.  It is recommended that another complete
filter assembly be used rather than attempting to change the filter
 itself.  Before a new filter assembly is installed, conduct a leak-check
 (see Section 4.1.4.2).  The  total particulate weight shall include the
 summation of all filter assembly catches.
                                    F-22

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     A single train shall be used for the entire sample run, except
in cases where simultaneous sampling is required in two or more
separate ducts or at two or more different locations within the same
duct, or, in cases where equipment failure necessitates a change of
trains.  In all other situations, the use of two or more trains will
be subject to the approval of the Administrator. .
     Note that when two or more trains are used, separate analyses of
the front-half and (if applicable) impinger catches from each train
shall be performed, unless identical nozzle sizes were used on all
trains, in which case, the front-half catches from the individual trains
may be combined (as may the impinger catches) and one analysis of front-
half catch and one analysis of impinger catch may be performed.  Consult
with the Administrator for details concerning the calculation of
results when two or more trains are used.
     At the end of the sample run, turn off the coarse adjust valve,
remove the probe and nozzle from  the stack, turn off the pump, record
the final dry gas meter reading,  and conduct a post-test leak-check, as
outlined in Section 4.1.4.3.  Also, leak-check the pitot lines as
described in Method 2, Section 3.1; the lines must pass this leak-check,
in order to validate the velocity head data.
     4.1.6  Calculation of Percent  Isokinetic.  Calculate percent
isokinetic  (see Calculations, Section  6)  to determine whether the run
was valid or another test run should be made.   If there was difficulty
in maintaining isokinetic rates due to source conditions, consult with
the Administrator  for  possible variance on the  isokinetic rates.
                             F-23

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     4.2  Sample Recovery.  Proper cleanup procedure begins as soon
as the probe .is removed from the stack at the end of the sampling
period.  Allow the probe to cool.
     When the probe can be safely handled, wipe off all external
particulate matter near the tip of the probe nozzle and place a cap
over it to prevent losing or gaining particulate matter.  Do not cap
off the probe tip tightly while the sampling train is cooling down
as this would create a vacuum in the filter holder, thus drawing water
from the impingers into the filter holder.
     Before moving the sample train to the cleanup site, remove the
probe from the sample train, wipe off the silicone grease, and cap
the open outlet of the probe.  Be careful not to lose any condensate
that might be present.  Wipe off the silicone grease from the filter
inlet where the probe was fastened and cap it.  Remove the umbilical
cord from the last impinger and cap the impinger.  If a flexible line
is used between the first impinger or condenser and the filter holder,
disconnect the line at the filter holder and let any condensed water
or liquid drain into the impingers or condenser.  After wiping off the
silicone grease, cap off the filter holder outlet and impinger inlet.
Either ground-glass stoppers, plastic caps, or serum caps may be used
to close these openings.
     Transfer the probe and filter-impinger assembly to the cleanup
area.  This area should be clean and protected from the wind so that
the chances of contaminating or losing the sample will be minimized.
                            F-24

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     Save a portion of the acetone used for cleanup as a blank.  Take
200 ml of this acetone directly from the wash bottle being used and
place it in a glass sample container labeled "acetone blank."
     Inspect the train prior to and during disassembly and note any
abnormal conditions.  Treat the samples as follows:
     Container No. 1.  Carefully remove the filter from'the filter holder
and place it in its identified petri dish container.  Use a pair of
                                                i
tweezers and/or clean disposable surgical gloves to handle the filter.
If it is necessary to fold the filter, do so such that the particulate
cake is inside the fold.  Carefully transfer to the petri dish any
particulate matter and/or filter fibers which adhere to the filter
holder  gasket, by using a dry Nylon bristle brush and/or a sharp-edged
blade.  Seal the container.
      Container No. 2.  Taking care to  see that  dust on the outside
of the  probe or other exterior surfaces does not get  into the  sample,
quantitatively recover particulate matter or any condensate from the
probe nozzle, probe  fitting,  probe liner, and front half  of the
filter  holder by washing  these components with  acetone  and placing
the  wash  in  a glass  container.   Distilled water may be  used instead
of acetone when approved  by  the  Administrator and  shall  be used when
specified by the Administrator;  in these  cases, save  a  water  blank
and  follow the Administrator's directions on analysis.   Perform the
acetone rinses as  follows:
                                  F-25

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      Carefully remove the probe nozzle and clean the inside surface
by  rinsing with acetone from a wash bottle and brushing with a Nylon
bristle brush.  Brush until  the acetone rinse shows  no visible particles,
after which make a final rinse of the inside surface with acetone. .
     Brush and rinse the inside parts of the Swagelok fitting with
acetone in a similar way until  no visible particles  remain.
     Rinse the probe liner with acetone by tilting and rotating the
probe while squirting acetone into its upper end so that all inside
surfaces will be wetted with acetone.  Let the acetone drain from the
lower end into the sample container.   A funnel (glass or polyethylene)
may be used to aid in transferring liquid washes to the container.   Follow
the acetone rinse with a probe brush.  Hold the probe in an inclined
position, squirt acetone into the upper end as the probe brush is being
pushed with a twisting action through the probe; hold a sample container
underneath the lower end of  the probe, and catch any acetone and particu-
late matter which is brushed from the probe.  Run the brush through the
probe three times or more until no visible particulate matter is carried
out with the acetone or until none remains in the probe liner on visual
inspection.  With stainless  steel or other metal probes, run the brush
through in the above prescribed manner at least six times since metal
probes have small crevices in which particulate matter can be entrapped.
Rinse the brush with acetone, and quantitatively collect these washings
in the sample container.  After the brushing, make a final acetone rinse
of the probe as described above.
                                  F-26

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     It Is recommended that two people be used to clean the probe
to minimize sample losses.  Between sampling runs, keep brushes clean
and protected from contamination.
     After ensuring that all joints have been wiped clean of silicone
grease, clean the inside of the front half of the filter holder by
rubbing the surfaces with a Nylon bristle brush and rinsing with
acetone.  Rinse each surface three times or more if needed to remove
visible particulate.  Make a final rinse of the brush and filter
holder.  Carefully rinse out the glass cyclone, also (if applicable).
After all acetone washings and particulate matter have been collected
in the sample container, tighten the lid on the sample container so
that acetone will not leak out when it is shipped to the laboratory.
Mark the height of the fluid level to determine whether or not
leakage occurred during transport.  Label the container to clearly
identify its contents.
     Container No. 3.  Note the  color of the  indicating silica gel
to determine if it has been completely spent  and make  a notation of
its condition.  Transfer  the silica gel"from  the fourth impinger to
its original container and  seal.  A funnel  may make  it easier to pour
the silica  gel without spilling.  A rubber  policeman may be used as
an aid  in  removing the silica  gel from the  impinger.   It is not
necessary  to remove  the small  amount of dust  particles that may adhere
to the  impinger wall  and  are difficult to remove.  Since the gain in
weight  is  to be used for  moisture calculations, do not use any water
                                   F-27

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or other liquids to transfer the silica gel.   If a balance is
available in the field, follow the procedure  for container No.  3
in Section 4.3.
     Impinger Water.  Treat the impingers as  follows:  Make a
notation of any color or film in the liquid catch.  Measure the
liquid which is in the first three impingers  to within +1  ml  by
using a graduated cylinder or by weighing it  to within +0.5 g by
using a balance (if one is available).  Record the volume  or weight
of liquid present.  This information is required to calculate the
moisture content of the effluent gas. .
     Discard the liquid after measuring and recording the  volume or
weight, unless analysis of the Impinger catch is required  (see Note,
Section 2.1.7).
     If a different type of condenser is used, measure the amount of
moisture condensed either volumetrically or gravimetrically.
     Whenever possible, containers should be shipped in such a way that
they remain upright at all times.
     4.3  Analysis.  Record the data required on a sheet such as the
one shown in Figure 5-3.  Handle each sample container as  follows:
     Container No.  1.  Leave the contents in the shipping container
or transfer the filter and any loose particulate from the sample
container to a tared glass weighing dish.  Desiccate for 24 hours
in a desiccator containing anhydrous calcium sulfate.  Weigh to a
constant weight and report the results to the nearest 0.1  mg.  For
purposes of this Section, 4.3, the term  "constant weight" means
                          F-28

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Plant.
Date	
Run No	
Filter No	
Amount liquid lost during transport
Acetone blank volume, ml	
Acetone wash volume, ml	
Acetone blank concentration, mg/mg (equation 5-4).
Acetone wash blank, mg (equation 5-5)	
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICIPATE COLLECTED.
mg
FINAL WEIGHT


^^xCl
TARE WEIGHT


2^x^
Less acetone blank
Weight of paniculate matter
WEIGHT GAIN






FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME,
ml




SILICA GEL
WEIGHT,
9



g* ml
     •CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
       INCREASE BY DENSITY OF WATER (1g/ml).
                                   INCREASE" 9  = VOLUME WATER, ml
                                      1 g/ml

                         Figure 5-3.  Analytical data.
                             F-29

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 a  difference of no more than 0.5 mg or 1 percent of total weight
 less tare weight, whichever is greater, between two consecutive
 weighings, with no less than 6 hours of desiccation time between
 weighings.
     Alternatively, the sample may be oven dried at 105°C (220°F) for
 2 to 3 hours, cooled in the desiccator, and weighed to a constant
weight, unless otherwise specified by the Administrator.  The tester
may also opt to oven dry the sample at 105°C (220°F) for 2 to 3 hours,
weigh the sample, and use this weight as a final weight.
     Container No. 2.  Note the level of liquid in the container and
confirm on the analysis sheet whether or not leakage occurred during
transport.  If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the Administrator,
to correct the final results.  Measure the liquid in this container
either volumetrically to +1 ml or gravimetrically to +0.5 g.  Transfer
the contents to a tared 250-ml beaker and evaporate to dryness at ambient
temperature and pressure.  Desiccate for 24 hours and weigh to a
constant weight.  Report the results to the nearest 0.1 mg.
     Container No. 3.  Weigh the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 g using a balance.  This step may be con-
ducted in the field.
     "Acetone Blank" Container.  Measure acetone in this container
either volumetrically or gravimetrically.  Transfer the acetone to
a tared 250-ml beaker and evaporate to dryness at ambient temperature
and pressure.  Desiccate for 24 hours and weigh to a constant weight.
Report the results to the nearest 0.1 mg.
                              F-30

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     Note:  At the option of the tester, the contents of Container
No. 2 as well as the acetone blank container may be evaporated at
temperatures higher than ambient.  If evaporation is done at an
elevated temperature, the temperature must be below the boiling point
of the solvent; also, to prevent "bumping," the evaporation process
must be closely supervised, and the contents of the beaker must be
swirled occasionally to maintain an even temperature.  Use extreme
care, as acetone is highly flammable and has a low flash point.
5.  Calibration
     Maintain a laboratory log of all calibrations.
     5.1  Probe Nozzle.  Probe nozzles shall be calibrated before
their initial use in the field.  Using a micrometer, measure the
inside diameter of the nozzle to the nearest 0.025 mm (0.001 in.).
Make three separate measurements using different diameters each time,
and obtain the average of the measurements.  The difference between
the high and low numbers shall not exceed 0.1 mm (0.004 in.).  When
nozzles become nicked, dented, or corroded, they shall be reshaped,
sharpened, and recalibrated before use.  Each nozzle shall be per-
manently and uniquely identified.
     5.2  Pi tot Tube.  The Type S pi tot tube assembly shall .be calibrated
according to the procedure outlined in Section 4 of Method 2.
     5.3  Metering System.  Before its initial use in the field, the
metering system shall be calibrated according to the procedure outlined
in APTD-0576.  Instead of physically adjusting the dry gas meter dial
readings to correspond to the wet test meter readings, calibration
factors may be used to mathematically correct the gas meter dial readings
to the proper values. Before  calibrating the metering  system,  it  is  sug-
gested that a leak-check be conducted.  For metering systems having diaphragm
                                  F-31

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 pumps, the normal leak-check procedure will  not detect leakages within
 the .pump.  For these cases the following leak-check procedure is
 suggested:make a 10-minute calibration run  at 0.00057 m3/min (0.02 cfm);
 at the end of the run, take the difference of the measured wet test meter
 and dry gas  meter volumes; divide the difference by 10, to get the leak
 rate.  The leak rate should not exceed 0.00057 m3/min (0.02 cfm).
     After each field use, the calibration of the metering system
shall be checked by performing three calibration runs at a single,
intermediate orifice setting (based on the previous field test), with
the vacuum set at the maximum value reached  during the test series.
To adjust the vacuum, insert a valve between the wet test meter and
the inlet of the metering system.  Calculate the average value of the
calibration  factor.  If the calibration has  changed by more than 5 per-
cent, recalibrate the meter over the full range of'orifice settings, as
outlined in  APTD-0576.
     Alternative procedures, e.g., using the orifice meter coeffi-
cients, may  be used, subject to the approval of the Administrator.
     Note:  If the dry gas meter coefficient values obtained before
and after a  test series differ by more than  5 percent, the test
series.shall either be voided, or calculations for the test series
shall be performed using whichever meter coefficient value (i.e.,
before or after) gives the lower value of total sample volume.
     5.4  Probe Heater Calibration.  The probe heating system shall be
calibrated before its initial use in the field according to the pro-
cedure outlined in APTD-0576.  Probes constructed according to APTD-0581
need not be  calibrated if the calibration curves in APTD-0576 are used.
     5.5  Temperature Gauges.  Use the procedure in Section 4.3 of
Method 2 to calibrate in-stack temperature gauges.  Dial thermometers,
                                   F-32

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such as are used for the dry gas meter and condenser outlet, shall be
calibrated against mercury-in-glass thermometers.
     5.6  Leak Check of Metering System Shown in Figure 5-1.  That
portion of the sampling train from the pump to the orifice meter
should be leak checked prior to initial use and after each shipment.
Leakage after the pump will result in less volume being recorded than
is actually sampled.  The following procedure is suggested (see
Figure 5-4):  Close the main valve on the meter box.  Insert a one-
hole rubber stopper with rubber tubing attached into the orifice
exhaust pipe. . Disconnect and vent the low side of the orifice manometer.
Close off the low side orifice tap.  Pressurize the system to 13 to
18 cm (5 to 7 in.) water column by blowing into the rubber tubing.
Pinch off the tubing and observe the manometer for one minute.  A loss
of pressure on the manometer indicates a leak in the meter box; leaks,
if present, must be corrected.
     5.7  Barometer.  Calibrate against a mercury barometer.
6.  Calculations
     Carry out calculations, retaining at least one extra decimal
figure beyond that of the acquired data.  Round off figures after
the final calculation.  Other forms of the equations may be used as
long as they  give equivalent results.
     6.1  Nomenclature.
                                               2    2
     A      = Cross-sectional area of  nozzle, m   (ft  ).
     B      = Water vapor  in the gas stream, proportion by volume.
      W5>
     C      = Acetone blank residue concentration, mg/g.
      a
     c      = Concentration of  particulate matter in  stack gas, dry
              basis, corrected  to  standard conditions, g/dscm  (g/dscf).
     I      = Percent of isokinetic sampling.
                            F-33

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CO
-p.
                    RUBBER
                    TUBING
                              RUBBER
                              STOPPER
ORIFICE
                                                                             VACUUM
                                                                              GAUGE
       BLOW INTO TUBING
       UNTIL MANOMETER
      READS 5 TO 7 INCHES
         WATER COLUMN
                           ORIFICE
                          MANOMETER
                                         MAIN VALVE
                                          CLOSED

                                      AIRTIGHT
                                        PUMP
                                         Figure 54. Leak check of meter box.

-------
L.     = Maximum acceptable leakage rate for either a pretest
 a


        - leak check or for a leak check following a component



         change; equal to 0.00057 m /min (0.02 cfm) or 4 percent



         of the average sampling rate, whichever is less.



L.     = Individual leakage rate observed during the leak check



         conducted prior to the "i  " component change (i = 1,



         2, 3 ---- n), m /min (cfm).



L      = Leakage rate observed during the post-test leak check,

          o
         m /min  (cfm).



m      = Total amount of parti cul ate matter collected, mg.
 n


M      = Molecular weight of water, 18.0 g/g-mole  (18.0 Ib/lb-mole).
 W


m_     = Mass of residue of acetone after evaporation, mg.
 a


P.     = Barometric pressure at the sampling site, mm Hg  (in. Hg).
 Dar


P      = Absolute  stack gas pressure, mm Hg  (in. Hg).



P   .   = Standard  absolute pressure, 760 mm  Hg  (29.92 in. Hg).



R      = Ideal gas constant, 0.06236 mm Hg-m /°K-g-mole  (21.85 in.



         Hg-ft3/°R-lb-mole).



T      = Absolute  average  dry gas  meter temperature  (see  Figure 5-2),
          °
           K
 T       =  Absolute  average stack  gas  temperature  (see  Figure 5-2),
          °
           K
 T  .d    =  Standard  absolute temperature,  293°K (528°R).



 V       =  Volume of acetone blank,  ml.
 a


 Va     =  Volume of acetone used in wash, ml.
 uW
                        F-35

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V,     = Total volume of liquid collected in impingers and
         silica gel (see Figure 5-3), ml.
V      = Volume of gas sample as measured by dry gas meter,
         dcm (dcf).
V / .  .1= Volume of gas sample measured by the dry gas meter,
         corrected to standard conditions, dscm (dscf).
V/std)= Volume of water vapor in the gas sample, corrected to
         standard conditions, scm (scf).
v      - Stack gas velocity, calculated by Method 2, Equation 2-9,
         using data obtained from Method 5, m/sec (ft/sec).
W      = Weight of residue in acetone wash, mg.
 a
Y      - Dry gas meter calibration factor.
AH     = Average pressure differential across the orifice meter
         (see Figure 5-2), mm H20 (in. H20).
p      = Density of acetone, rig/ml (see label on bottle).
 a
p      = Density of water, 0.9982 g/ml (0.002201 Ib/ml).
 W
6      = Total sampling time, min.
e,     = Sampling time interval, from the beginning of a run until
         the first component change, min.
8.     = Sampling time interval, between two successive component
         changes, beginning with the interval between the first
         and second changes, min.
6      = Sampling time interval, from the final (n  ) component
         change until the.end of the sampling run, min.
                          F-36

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     13.6  = Specific gravity of mercury.
     60    = Sec/min.
     100   = Conversion to percent.
     6.2  Average dry gas meter temperature and average orifice
pressure drop.  See data sheet (Figure 5-2).
     6.3  Dry Gas Volume.  Correct the sample volume measured by the
dry gas meter to standard conditions (20°C, 760 mm Hg or 68°F,
29.92 in. Hg) by using Equation 5-1.
                   {
                   T
std)
V
Ph,_ + 4H
bar T3T
Pstd
. KVY ptar *(»H/13.6)
1 " Tm
    Vstd) = V
                  y  111 /       o i»u
                                                      Equation 5-1
where:
     KI = 0.3858 pK/mm Hg for metric units
        = 17.64 °R/1n. Hg for English units
     Note:  Equation 5-1 can be used as written unless the leakage
rate observed during any of the mandatory leak checks (i.e., the
post-test leak check or leak checks conducted prior to component
changes) exceeds L .  If !_„ or I_. exceeds L , Equation 5-1 must be
                  a       p     I          a
modified as follows:
     (a)  Case I.  No component changes made during sampling run.   In
this case, replace V  in Equation 5-1 with the expression:
          V* -  ']
                           F-37

-------
      (b)  Case  II.  One or more component changes made during the
 sampling run.   In this case, replace V  in Equation 5-1 by the
expression:
               - La> 91 -      91 - 'S - La>
and substitute only for those leakage rates (l_. or L ) which exceed
     6.4  Volume of water vapor.
     V ,c^ = Vlr( SHI K-^-J =  K, Ylf.           Equation 5-2
'w(std)  * ¥lc,..w
where:
     K2 = 0.001333 m /ml for metric units
        = 0.04707 ft3/ml for English units
     6.5  Moisture Content.
     Bws  =  V ,       V	                       Equation 5-3
      ws     Vm(std)    w(std)
     Mote:  In saturated or water droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be made,
one from the impinger analysis (Equation 5-3), and a second from the
assumption of saturated conditions.  The lower of the two values of
B,,_ shall be considered correct.  The procedure for determining the
 ws
moisture content based upon assumption of saturated conditions is
given in the Note of Section 1.2 of Method 4.  For the purposes of this
method, the average stack gas temperature from Figure 5-2 may be used to
make this determination, provided that the accuracy of the in-stack
temperature sensor is +_ 1°C (2°F).
                                 F-38

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     6.6  Acetone Blank Concentration.
                 ma
     C      =  V  p_                                    Equation 5-4
      a         a  a
     6.7  Acetone Wash Blank.
     Wa  =  Ca Vaw pa                                   Equation 5-5
     6.8  Total Particulate Weight.   Determine the  total particulate
catch from the sum of the weights obtained from containers  1  and 2
less the acetone blank (see Figure 5-3).   Note:  Refer to Section
4.1.5 to assist in calculation of results involving two or  more
filter assemblies or two or more sampling trains.
     6.9  Particulate Concentration.
     c$  =  (0.001 g/mg)  (mn/Vm(stdp                   Equation 5-6
     6.10 Conversion Factors:
     From                    To                      Multiply by
     scf                     m3                       0.02832
     g/ft3                   gr/ft3                  15.43
     g/ft3                   lb/ft3                   2.205 x 10"3
     g/ft3                   g/m3                    35.31
     6.11  Isokinetic Variation.
     6.11.1  Calculation From Raw Data.
     ,  .  100 Ts [K3 V1c * (V, Y/TJ  (Pbar * AH/13.6)]
                           60 9 v  P  A
                                                         Equation 5-7
                          F-39

-------
where:
     K- = 0.00.3454 mm Hg-m3/ml-°K for metric units
        = 0.002669 in.  Hg-ft3/ml-°R for English units.
     6.11.2  Calculation From Intermediate Values.
     ,  .        Ts Vstd) Pstd
        "
           Tstd vs 8 An ps 60 "-««'

        " "4  Ps \ ^'^'^ws'
where :
     K4 = 4.320 for metric units
        = 0.09450 for English units.
     6.12  Acceptable Results.  If 90  percent l I  l 110 percent,  the
results are acceptable.  If the results are low in comparison  to  the
standard  and I is beyond the acceptable range, or, if I is  less  than
90 percent, the Administrator may opt  to accept the results.   Use
Citation 4 to make judgments.  Otherwise, reject the results and  repeat
the test.
7.  Bibliography
     1.  Addendum to Specifications for Incinerator Testing  at Federal
Facilities.  PHS, NCAPC.  Dec. 6, 1967.
     2.  Martin, Robert M.  Construction Details of Isokinetic Source-
Sampling Equipment.  Environmental Protection Agency.   Research
Triangle Park, N. C.  APTD-0581.  April, 1971.
     3.  Rom, Jerome J.  Maintenance,  Calibration, and Operation
of Isokinetic Source Sampling Equipment.  Environmental Protection
Agency.  Research Triangle Park, N. C.  APTD-0576.  March, 1972.
                           F-40

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     4.  Smith, W. S., R. T. Shigehara, and W. F. Todd.  A Method
of Interpreting Stack Sampling Data.  Paper Presented at the
63d Annual Meeting of the Air Pollution Control Association,
St. Louis, Mo.  June 14-19, 1970.
     5.  Smith, W. S., et al.  Stack Gas Sampling Improved and
Simplified With New Equipment.  APCA Paper No. 67-119.  1967.
     6.  Specifications for Incinerator Testing at Federal Facilities.
PHS, NCAPC.  1967.
     7.  Shigehara, R.T.  Adjustments in the EPA Nomograph for
Different Pitot Tube Coefficients and Dry Molecular Weights.  Stack
Sampling News ^:4-ll.  October, 1974.
     8.  Vollaro, R. F.  A Survey of Commercially Available  Instrumentation
For the Measurement of Low-Range Gas Velocities.  U. S. Environmental
Protection Agency, Emission Measurement Branch.  Research Triangle
Park, N. C.  November, 1976 (unpublished paper).
     9.  Annual Book of ASTM Standards.  Part  26.  Gaseous Fuels;
Coal and Coke; Atmospheric Analysis.  American Society  for Testing
and Materials.  Philadelphia, Pa.   1974.  pp.  617-622.
    10.  Felix, L. G.,  G.  I. Clinard, G. E.  Lacey,  and J. D. McCain.
Inertial Cascade Impactor Substrate  Media for Flue Gas Sampling.
U. S. Environmental  Protection Agency.  Research Triangle Park, N. C.
27711, Publication No.  EPA-600/7-77-060.  June  1977,  83  p.
                                   F-41

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SLIDE 106-0                                            NOTES

          METHOD — 5

Determination of Particulate Emissions
       From Stationary Sources
 SLIDE  106-1
                PRINCIPLE

   Particulate matter is withdrawn isokinetically from
 the source and collected on a glass fiber filter main-
 tained at a temperature in the range of 248 ± 25°F.
   The particulate mass is determined gravimetri-
 cally after removal of uncombined water.

              APPLICABILITY

   This method is applicable for the determination
 of particulate emissions from stationary sources.
                                         F-43

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SLIDE  106-2
NOTES
P;EPA :-
  METHOD i
j  Partieulat*t
SLIDE 106-3
                                                  •.••.•••.•.••.••.•••yy---'---:y.::::v.
                                        F-45

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SLIDE 106-4
NOTES
SLIDE  106-5
                                F-47

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SLIDE 106-6
                                               NOTES
SLIDE 106-7
                               F-49

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SLIDE  106-8
NOTES
        COMPONENT CALIBRATION
                PROBE NOZZLE
1. Measure three diameters of the nozzle.
2. Calculate the average measurement.
3. The difference between the high and low measure-
  ment shall not exceed 0.004 in.
4. Nozzle should be uniquely identified.
 SLIDE 106-9
                                       F-51

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SLIDE 106-10
NOTES
             METERING SYSTEM
SLIDE  106-11
 SAMPLE METER SYSTEM CALIBRATION SETUP
                               MANOMETER
                               LEVEL ADJUST
                                 F-53

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SLIDE  106-12
NOTES
 SLIDE  106-  13


    TEMPERATURE GAUGE CALIBRATION

           IMPINGER THERMOMETER
  Calibrate with a mercury-in-glass thermometer which
meets ASTM E-1 No. 63C or 63F specifications.
  1. compare readings in ice bath
  2. compare readings at room temperature
  3. thermometer must  agree within  2°F of the reference
    thermometer at both temperatures

        DRY GAS METER THERMOMETER
  Calibrate with a mercury-in-glass thermometer which
meets ASTM specifications.
  1. compare readings in hot water bath 105° - 122°F
  2. compare readings at room temperature
  3. thermometers must agree within 5.4°F at both points or
    differential at both points within 5.4°F
                                      F-55

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SLIDE 106-14
NOTES
SLIDE  106-15
         PROBE HEATER CALIBRATION

   Calibrate probe heater if not constructed according to
 APTD - 0581 using procedure outlined in APTD - 0576

            BALANCE CALIBRATION
              ANALYTICAL BALANCE
         • Calibrate using Class-S weights.
          (balance should agree within ± 2 mg)

                 TRIP BALANCE
         • Calibrate using Class-S weights
          (balance should agree within ± 0.5 g)
                                    F-57

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SLIDE 106-16
                           NOTES
PROJECTED AREA MODELS FOR TYPICAL
         PITOBE  ASSEMBLIES
        PERCENT
        THEORETICAL =
        BLOCKAGE
       I x w
    DUCT AREA
             X100
 SLIDE 106-17
  ADJUSTMENT OF TYPE "S" PITOT TUBE
COEFFICIENTS TO ACCOUNT FOR BLOCKAGE
 w
 o
 O
 u
 LU
 m
 £L
 z
 S
 e
 u
 S
1 in. CYLINDRICAL MODEL;
USE FOR ASSEMBLIES WITH
NO EXTERNAL SHEATH.
        2Vi in. CYLINDRICAL MODEL;
        USE FOR ASSEMBLIES WITH _
        EXTERNAL SHEATH.
                234

               THEORETICAL BLOCKAGE, %
                              F-59

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SLIDE 106-18
                                               NOTES
               4 &£"?:.•*•* i--"V •*" .^
-------
SLIDE  3.06-20
NOTES
             SAMPLE RECOVERY
                     FILTER
1. Carefully remove filter from filter holder and place it in
  designated petri dish.
2. Seal and label petri dish.

    PROBE AND CONNECTING GLASSWARE
1. Clean outside of probe,  pitot tube and nozzle.
2. Remove nozzle and rinse and brush inside surface until
  rinse is clear.
3. Rinse and brush probe.
        A. a minimum of  3 rinses for glass lined probes
        B. a minimum of  6 rinses for metal lined probes
4. Brush and rinse front half of filter holder.
5. Clean  connecting glassware  which precedes  filter
  holder.
 SLIDE  106-21
                                         F-63

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SLIDE  106-22
NOTES
SLIDE  106-23
  PROBE AND CONNECTING GLASSWARE (cont.)

 6. Securely seal sample bottle and mark liquid level.
 7. Collect acetone blank sample.
                  CONDENSER
 1. Determine liquid quantity in impingers to nearest 1 ml
   or 0.5 g.
 2. Make note of any color or film in impinger water.
                   SILICA GEL
 1. Note color of silica gel to determine if spent.
 2. Determine weight gain to nearest 0.5 g.
                                       F-65

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SLIDE 106-24                                            NOTES

                   ANALYSIS
                     FILTER
1. Desiccate filter for a minimum of 24 hrs.
2. Weigh to a constant weight and record results to near-
  est 0.1 mg.
3. Alternatively, filter may be oven dried at 220°F for 2 to 3
  hrs., cooled in desiccator, and weighed to constant
  weight.
4. Analyze blank filter in same manner as sample filter.
SLIDE 106-25


(cont.)                ANALYSIS
                    ACETONE RINSE
    1. Confirm that no leakage occurred during shipment.
    2. Measure contents of container to nearest 1 ml or 0.5 g.
    3. Transfer to tared beaker; evaporate and desiccate for
      24 hrs.
    4. Weigh to constant weight; report data to nearest 0.1 mg.
    5. Alternatively, acetone rinse may be evaporated at ele-
      vated temperature (below 133°F).
    6. Analyze blank in same manner as the sample.
                                         F-67

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                            SECTION G.   METHOD 6

Subject

1.  Method 6—determination of sulfur dioxide emissions from
    stationary sources (taken from Environmental Protection Agency
    Performance Test Methods manual)                                  G-3

2.  Slides                                                            G-19
                                      6-1

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            METHOD 6—DETERMINATION OF SULFUR DIOXIDE
                EMISSIONS FROM STATIONARY SOURCES
1.   Principle and Applicability
    1.1.   Principle.   A gas sample is extracted from the sampling
point in the stack.  The sulfuric acid mist (including sulfur trioxide)
and the sulfur dioxide are separated.  The sulfur dioxide fraction
is measured by the barium-thorin titration method.
    1.2  Applicability.  This method is applicable for the determina-
tion of sulfur dioxide emissions from stationary sources.  The
minimum detectable limit of the method has been determined to be
3.4 milligrams (nig) of S02/m3 (2.12 x 10"7 lb/ft3).  Although no upper
limit has been established, tests have shown that concentrations as high
              3
as 80,000 mg/m  of SOp can be collected efficiently in two midget impingers
each containing 15 milliliters of 3 percent hydrogen peroxide, at a rate
of 1.0 1pm for 20 minutes.  Based on theoretical calculations, the upper
                                                             3
concentration limit in a 20-liter sample is about 93,300 mg/m .
    Possible interferents are free ammonia, water-soluble cations,
and fluorides.  The cations and fluorides are removed by glass wool
filters and an isopropanol bubbler, and hence do not affect the S0«
analysis.  When samples are being taken from a gas stream with high
concentrations of  very fine metallic fumes (such as in inlets to
control devices),  a high-efficiency glass fiber filter must be used
in place of the glass wool plug  (i.e., the one in the probe) to remove
the cation interferents.
    Free ammonia  interferes by  reacting with SOp  to form particulate
sulfite and by reacting with  the  indicator.  If free ammonia is
                                  G-3

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                                                                               THERMOMETER
     PROBE (END PACKED

      WITH QUARTZ OR

        PYREX WOOL)
en
i
                             STACK WALL
                            MIDGET IMPINGERS
             MIDGET BUBBLER
 SILICA GEL


DRYING TUBE
GLASS WOOL
                                         ICE BATH



                                     THERMOMETER



                                           £=iL
                                                 DRY


                                              GAS METER
                                                        PUMP
                                 Figure 6-1.  S02 sampling train.
                                  SURGE TANK

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present (this can be determined by knowledge of the process and
noticing white participate matter in the probe and isopropanol
bubbler), alternative methods, subject to the approval  of the
Administrator, U. S. Environmental Protection Agency, are required.
2.  Apparatus
     2.1  Sampling.  The sampling train is shown in Figure 6-1,
and component  parts are discussed below.  The tester has the
option of substituting sampling equipment described in Method 8
in place of the midget impinger equipment of Method 6.   However, the
Method 8 train must be modified to include a heated filter between
the probe and isopropanol impinger, and the operation of the sampling
train and sample analysis must be at the flow rates and solution
volumes defined  in Method 8.
    The tester also has the option of -'etermining SCL simultaneously
with particulate matter and moisture determinations by (1) replacing
the water in a Method 5 impinger  system with 3 percent peroxide solution,
or (2) by replacing the Method 5  water impinger system with a Method 8
isopropanol-filter-peroxide system.  The analysis for S0? must be con-
sistent with the procedure in Method 8.
    2.1.1  Probe.   Borosilicate glass, or stainless steel  (other
materials of construction may be  used, subject to the approval of
the Administrator), approximately 6-mm inside diameter, with a heating
system  to prevent  water condensation and a filter (either  in-stack or
heated  out-stack)  to  remove particulate matter, including  sulfuric
acid mist.  A plug of glass wool  is a satisfactory  filter.
     2.1.2   Bubbler and  Impingers.  One midget bubbler, with
medium-coarse glass frit  and  borosilicate or quartz glass  wool
                                  6-5

-------
 packed  in top (see Figure 6-1) to prevent sulfuric acid mist
 carryover, and three 30-ml midget impingers.  The bubbler and
 midget  impingers must be connected in series with leak-free glass
 connectors. Silicone grease may be used, if necessary, to prevent
 leakage.
     At the option of the tester, a midget impinger may be used
 in place of the midget bubbler.
     Other collection absorbers and flow rates may be used, but
are subject to the approval of the Administrator.  Also, collection
efficiency must be shown to be at least 99 percent for each test run
and must be documented in the report.  If the efficiency is found to
be acceptable after a series of three tests, further documentation is
not required.  To conduct the efficiency test, an extra absorber must
be added and analyzed separately.  This extra absorber must not contain
more than 1 percent of the total SCL.
     2.1.3  Glass Wool.  Borosilicate or quartz.
     2.1.4  Stopcock Grease.  Acetone-insoluble, heat-stable
silicone grease may be used, if necessary.
     2.1.5  Temperature Gauge.  Dial thermometer, or equivalent, to
measure temperature of gas leaving impinger train to within 1°C (2°F).
     2.1.6  Drying Tube.  Tube packed with 6- to 16-mesh indicating-
type silica gel, or equivalent, to dry the gas sample and to protect
the meter and pump.  If the silica gel has been used previously, dry
at 175°C (350°F) for 2 hours.  New silica gel may be used as received.
Alternatively, other types of desiccants (equivalent or better) may
be used, subject to approval of the Administrator.
                              6-6

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     2.1.7  Valve.   Needle valve, to regulate sample gas flow
rate.
     2.1.8  Pump.   Leak-free diaphragm pump, or equivalent, to
pull  gas through the train.   Install a small surge tank between the
pump  and rate meter to eliminate the pulsation effect .of the
diaphragm pump on  the rotameter.
     2.1.9  Rate Meter.  Rotameter, or equivalent, capable of
measuring flow rate to within 2 percent of the selected flow rate
of about 1000 cc/min.
     2.1.10  Volume Meter.  Dry gas meter, sufficiently accurate to
measure the sample volume within 2 percent, calibrated  at the selected
flow  rate and conditions actually encountered during sampling, and
equipped with a temperature gauge (dial thermometer, or equivalent)
capable of measuring temperature to within 3°C (5.4°F).
   2.1.11  Barometer.  Mercury, aneroid, or other barometer
capable of measuring atmospheric pressure to within 2.5 mm Hg
(0.1  in. Hg). In many cases, the barometric reading may be obtained
from  a nearby national weather service station, in which case the
station value (which is the absolute barometric pressure) shall
be requested and an adjustment for elevation differences between
the weather station and sampling point shall be applied at a rate
of minus 2.5 mm Hg (0.1 in.  Hg) per 30 m (100 ft) elevation
increase or vice versa for elevation decrease.
                                    G-7

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     2.1.12  Vacuum Gauge and Rotameter.  At least 760 mm Hg (30 in.  Hg)
gauge and 0-40" cc/min rotameter, to be used for leak check of the sampling
train.
     2.2  Sample Recovery.
     2.2.1  Wash Bottles.  Polyethylene or glass, 500 ml, two.
     2.2.2  Storage Bottles.  Polyethylene, 100 ml, to store impinger
samples (one per sample).
     2.3  Analysis.
     2.3.1  Pipettes.  Volumetric type, 5-ml, 20-ml (one per sample),
and 25-ml  sizes.
     2.3.2  Volumetric Flasks.  100-ml size (one per sample) and 1000-ml
size.
     2.3.3  Burettes. -5- and 50-ml sizes.
     2.3.4  Erlenmeyer Flasks.  250 mi-size (one for each sample,
blank, and standard).
     2.3.5  Dropping Bottle.  125-ml size, to add indicator.
     2.3.6  Graduated cylinder.  100-ml size.
     2.3.7  Spectrophotometer.  To measure absorbance at 352 nanometers.
3.  Reagents
     Unless otherwise indicated, all reagents must conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society.  Where such specifications are not
available, use the best available grade.
     3.1  Sampling.
     3.1.1  Water.  Deionized, distilled to conform to ASTM
specification Dll93-74, Type 3.  At the option of the analyst,
                                  G-8

-------
the KMnO. test for oxidizable orgar.ic matter may be omitted when high
concentrations of organic matter are not expected to be present.
     3.1.2  Isopropanol, 80 percent.  Mix 80 ml of isopropanol with 20
ml of deionized, distilled water.  Check each lot of isopropanol for
peroxide impurities as  follows:  shake 10 ml of isopropanol with 10 ml
of freshly prepared 10  percent potassium iodide solution.  Prepare a
blank by similarly treating 10 ml of distilled water.  After 1 minute,
read the absorbance at  352 nanometers on a spectrophotometer (Note:  Use
a 1-cm path length).  If absorbance exceeds 0.1, reject
alcohol for use.
     Peroxides may be removed from isopropanol by redistilling or by
passage through a column of activated alumina; however, reagent grade
isopropanol with suitably low peroxide levels may be obtained from
commercial sources.-  Rejection of contaminated lots may, therefore, be a
more efficient procedure.
     3.1.3  Hydrogen Peroxide, 3 Percent.  Dilute 30 percent hydrogen
peroxide 1:9 (v/v) with deionized, distilled water (30 ml is needed per
sample).  Prepare fresh daily.
     3.1.4  Potassium Iodide Solution, 10 Percent.    Dissolve 10.0
grams KI in deionized,  distilled water and dilute to 100 ml.  Prepare
when needed.
     3.2  Sample Recovery.
     3.2.1  Water.  Deionized, distilled, as in 3.1.1.
     3.2.2  Isopropanol, 80 Percent.  Mix 80 ml of isopropanol with 20
ml of deionized, distilled water.
                            6-9

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     3.3  Analysis.
     3.3.1  Water.   Deionized,  distilled,  as  in 3.1.1.
     3.3.2  Isopropanol,  100 percent.
     3.3.3  Thorin  Indicator.   l-(o-arsonophenylazo)-2-naphthol-3,
6-disulfonic acid,  disodium salt, or equivalent.   Dissolve  0.20  g
in 100 ml  of deionized,  distilled water.
     3.3.4  Barium  Perchlorate  Solution,  0.0100 N.   Dissolve  1.95 g of
barium perchlorate  trihydrate [Ba(C104)2'3H20] in 200 ml  distilled water
and dilute to 1  liter with isopropanol.   Alternatively,  1.22  g of
[BaCl2'2H20] may be used instead of the  perchlorate.  Standardize as  in
Section 5.5.
     3.3.5  Sulfuric Acid Standard, 0.0100 N.  Purchase  or  standardize
to +0.0002 N against 0.0100 N NaOH which  has  previously  been
standardized against potassium acid phthalate (primary standard
grade).
4.  Procedure.
     4.1  Sampling.
     4.1.1  Preparation of collection  train.   Measure 15 ml of 80
                           t.
percent isopropanol into the midget bubbler and 15 ml of 3  percent
hydrogen peroxide into each of the first two  midget impingers.
Leave the final  midget impinger dry.  Assemble the train as shown
in Figure 6-1.  Adjust probe heater to a temperature sufficient  to
prevent water condensation.  Place crushed ice and water around  the
impingers.
     4.1.2  Leak-check procedure.  A leak check prior to the
sampling run is optional; however, a leak check after the sampling
run is mandatory.  The leak-check procedure is as follows:
                          G-10

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     Temporarily attach a suitable (e.g., 0-40 cc/min) rotameter to the
outlet of the dry gas meter and place a vacuum gauge at or near the
probe inlet.  Plug the probe inlet, pull a vacuum of at least 250 mm Hg
(10 in. Hg), and note the flow rate as indicated by the rotameter.  A
leakage rate not in excess of 2 percent of the average sampling rate is
acceptable.  Note:  Carefully release the probe inlet plug before
turning off the pump.
     It is suggested (not mandatory) that the pump be leak-checked
separately, either prior to or after the sampling run.  If done prior to
the sampling run, the pump leak-check shall precede the leak check of
the sampling train described immediately above; if done after the
sampling run, the pump leak-check shall follow the train leak-check.  To
leak check the pump, proceed as follows:  Disconnect the drying tube
                      •  »
from the probe-impinger assembly.  Place a vacuum gauge at the inlet to
either the drying tube or the pump, pull a vacuum of 250 mm (10 in.) Hg,
plug or pinch off the outlet of the flow meter and then turn off the
pump.  The vacuum should remain stable for at least 30 seconds.
     Other leak-check procedures may be used, subject to the approval of
the Administrator, U.S. Environmental Protection Agency.  The  procedure
used in Method  5  is not suitable for diaphragm pumps.
                             G-ll

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     4.1.3  Sample Collection.   Record the initial  dry gas meter reading
and barometric pressure.  To begin sampling, position the tip of the
probe at the sampling point, connect the probe to the bubbler, and start
the pump.  Adjust the sample flow to a constant rate of.approximately
1.0 liter/min as indicated by the rotameter.  Maintain this constant
rate (+10 percent) during the entire sampling run.  Take readings (dry
gas meter, temperatures at dry gas meter and at impinger outlet and rate
meter) at least every 5 minutes.  Add more ice during the run to keep
the temperature of the gases leaving the last impinger at 20°C (68°F) or
less.  At the conclusion of each run, turn off the pump, remove probe
from the stack, and record the final readings.  Conduct a leak check as
in Section 4.1.2.  (This' leak check is mandatory.)   If a leak is found,
                      V *
void the test run or use procedures acceptable to the Administrator to
adjust the sample volume for leakage.  Drain the ice bath, and purge the
remaining part of the train by drawing clean ambient air through the
system for 15 minutes at the sampling rate.
     Clean ambient air can be provided by passing air through a charcoal
filter or through an extra midget impinger with 15 ml of 3 percent H202.
The tester may opt to simply use ambient air, without purification.
                                6-12

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     4.2  Sample Recovery.   Disconnect the impingers after purging.
Discard the contents of the midget bubbler.  Pour the contents of
the midget impingers into a leak-free polyethylene bottle for
shipment.  Rinse the three midget impingers and the connecting
tubes with deionized, distilled water, and add the washings to
the same storage container.  Mark the fluid level.  Seal and
identify the sample container.
     4.3  Sample Analysis.  Note level of liquid in container,
and confirm whether any sample was lost during shipment; note
this on analytical data sheet.  If a noticeable amount of leakage has
occurred, either void the sample or use methods, subject to the approval
of the Administrator, to correct the final results.
     Transfer the contents of the storage container to a 100-ml
volumetric flask and dilute to exactly 100 ml with deionized, distilled
water.   Pipette a 20-ml aliquot of this solution into a 250-ml
Erlenmeyer flask, add 80 ml of 100 percent isopropanol and two to four
drops  of thorin indicator, and titrate to a pink endpoint using
0.0100 N  barium perch!orate.  Repeat and average the titration
volumes.  Run a blank with each series of samples.  Replicate
titrations must agree within  1 percent or 0.2 ml, whichever is larger..
      (Note:  Protect the 0.0100 N barium perchlorate solution from
evaporation at  all  times.)
                               G-13

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 5.   Calibration
      5.1  Metering System.
      5.1.1   Initia.l Calibration.  Before its initial use in the field,
 first leak check the metering system (drying tube, needle valve, pump,
 rotameter, and dry gas meter) as follows:  place a vacuum .gauge at
 the  inlet to the drying tube and pull a vacuum of 250 mm (10 in.) Hg;
 plug  or pinch off the outlet of the flow meter, and then turn off the
 pump.  The vacuum shall remain stable for at least 30 seconds.  Care-
 fully release the vacuum gauge before releasing the flow meter end.
     Next, calibrate the metering system (at the sampling flow rate
 specified by the method) as follows:  connect an appropriately sized
wet test meter (e.g., 1 liter per revolution) to the inlet of the
drying tube.   Make three independent calibration runs, using at least
five revolutions of the dry gas meter per run.   Calculate the calibra-
tion factor,  Y (wet test meter calibration volume divided by the dry
gas meter volume, both volumes adjusted to the  same reference temperature and
pressure), for each run, and average the results.  If any Y value
deviates by more than 2 percent from the average, the metering system
is unacceptable for use.  Otherwise, use the average as the calibration
factor for subsequent test runs.
     5.1.2  Post-Test Calibration Check.  After each field test series,
conduct a calibration check as in Section 5.1.1 above, except for the
following variations: (a) the leak check is not to be conducted, (b) three,
or more revolutions of the dry gas meter may be used, and (c) only
two independent runs need be made.  If the calibration factor does
                                   G-14

-------
not deviate by more than 5 percent from the initial  calibration
factor (determined in Section 5.1.1), then the dry gas meter
volumes obtained during the test series are acceptable.  If the
calibration factor deviates by more than 5 percent,  recalibrate
the metering system as in Section 5.1.1, and for the calculations,
use the calibration factor (initial or recalibration) that yields the
lower gas volume for each test run.
     5.2  Thermometers.  Calibrate against mercury-in-glass thermometers.
     5.3  Rotameter.  The rotameter need not be calibrated, but should
be cleaned and maintained according to the manufacturer's instruction.
     5.4  Barometer.  Calibrate against a mercury barometer.
     5.5  Barium Perch!orate Solution.  Standardize the barium perch-
lorate solution against 25 ml of standard sulfuric acid to which 100 ml
of 100 percent isopropanol has been added.
6.  Calculations
    Carry out calculations, retaining at  least one extra decimal figure
beyond that of the acquired data.  Round  off figures after final calculation,
    6.1  Nomenclature.
    C<;n     = Concentration of sulfur dioxide, dry basis corrected to
     bU2
               standard conditions, mg/dscm (Ib/dscf).
    N       = Normality of barium  perchlorate titrant, milliequivalents/ml.
    P.      = Barometric pressure  at the  exit orifice of the dry gas
     oar
              meter, mm Hg (in. Hg).
    Pstd    = standard absolute pressure, 760 mm Hg  (29.92 in. Hg).
    T       = Average dry gas meter absolute temperature,  °K (°R).
    Tstd    = standard absolute temperature, 293° K  (528°  R).

                                    G-15

-------
     m
        = Volume of sample aliquot titrated, ml.
        = Dry gas volume as measured by the dry gas meter, dcm
          (dcf).
    'soln
V / td\ = Dry gas volume measured by the dry gas meter,
          corrected to standard conditions, dscm (dscf).
        = Total volume of solution in which the sulfur dioxide
          sample is contained, 100 ml.
       = Volume of barium perch!orate titraht used for the
         sample, ml (average of replicate titrations).
       - Volume of barium perchlorate titrant used for the
         blank, ml.
Y      = Dry gas meter calibration factor.
32.03  = Equivalent weight of sulfur dioxide.
6.2  Dry sample gas volume, corrected to standard conditions.'
    'tb
     Vm(std)  '  V
where:
     K.|  « 0.3858 °K/mm Hg for metric units.
         = 17.64 °R/in. Hg for English units.
     6.3  Sulfur dioxide concentration.
                                                     V  P
                                                      m  bar
                                                        m
                                                     Equation 6-1
                                   soln
      'SO,
            «z   —
                            m(std)
                                                     Equation 6-2
where:
         =  32.03 mg/meq. for metric units.
         = 7.061 x 10   Ib/meq. for English units.
                                 G-16

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 7.  Bibliography
     1.  Atmospheric Emissions from Sulfuric Acid Manufacturing
Processes.  U.'S. DHEW, PHS, Division of Air Pollution.  Public
Health Service Publication No. 999-AP-13.  Cincinnati, Ohio.  1965.
     2.  Corbett, P.P.  The Determination of S02 and S(L in Flue
Gases.  Journal of the Institute of Fuel.  24:237-243, 1961.
     3.  Matty, R. E. and E. K. Diehl.  Measuring Flue-Gas SO,, and
S03>  Power.  1_01_: 94-97.  November 1957.
     4.  Patton, W. F. and J. A. Brink, Jr.  New Equipment and
Techniques for Sampling Chemical Process Gases.  J. Air Pollution
Control Association.  1_3:162.  1963.
     5.  Rom, J. J.  Maintenance, Calibration, and Operation of
Isokinetic Source-Sampling Equipment.  Office of Air Programs,
Environmental Protection Agency.  Research Triangle Park, N. C.
APTD-0576.  March 1972.
     6.  Hamil, H. F. and D. E. Camann.  Collaborative Study of
Method for the Determination of Sulfur Dioxide Emissions From
Stationary Sources (Fossil-Fuel Fired Steam Generators).
Environmental Protection Agency, Research Triangle Park, N. C.
EPA-650/4-74-024.  December 1973.
     7.  Annual Book of ASTM Standards.  Part 31; Water, Atmospheric
Analysis.  American Society for Testing and Materials.  Philadelphia,
PA.  1974.  pp. 40-42.
     8.  Knoll, J. E. and M. R. Midgett.  The Application of EPA
Method 6 to High Sulfur Dioxide Concentrations.  Environmental Protection
Agency.  Research Triangle Park, N. C.  EPA-600/4-76-038.  July 1976.
                           G-17

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SLIDE 107-0                                         NOTES

    METHOD —6
    Determination of
Sulfur Dioxide Emissions
From Stationary Sources
SLIDE  107-1

               PRINCIPLE
  A gas sample is extracted from the stack. Sul-
furic acid mist and sulfur dioxide are separated.
  Sulfur dioxide  is measured  by the barium-
thorin titration method.

             APPLICABILITY
 This method is applicable for determination of
sulfur dioxide emissions from stationary sources.
  • minimum detectable limit is 3.4 mg of SO2 per m3
  • theoretical calculations indicate the upper con-
    centration limit in a 20 liter sample is « 93,300 mg
    per m3.
 SLIDE  107-2
         METHOD 6 INTERFERENCES
 1. CATIONS — Removed by glass wool filter and
   isopropanol bubbler.
 2. FLUORIDES — Removed by glass wool filter and
   isopropanol bubbler.
 3. FINE METALLIC FUMES — Removed by high
   efficiency glass fiber filter.
 4. AMMONIA — Use alternative methods (Subject
   to Approval of the Administrator).


                                      G-19

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 SLIDE  107-3

               SO2 SAMPLING TRAIN
          fl
                 THERMOME IfcR
MILXHT BU6BLEH
 IFRITTEO TIP)
 SILICA GtL
DRYING TUBE
  (END PACKED	
WTTH GLASS WOOL!
       STACK
       WALL
                 Hf AUNG
                 ELEMENT
w
jf!
i
' \
ws*
ICE
BATH
MIL
1 I
•JT
GE
7 \
&$f
T IMPI
1 1
»T
is
' \
*£fc
RS
hri
j
'
if
                     THtHMOMtTEfi
                                            NfEDLE
                                             VALVE
                               SURGE TANK
 SLIDE  107-4
                  REAGENTS
  Reagents must conform to specifications estab-
lished by American Chemical Society or use best
available grade.
  • Check each lot of isopropanol for peroxide impurities.
  • Prepare 3% hydorgen peroxide fresh each day.
  • Standardize barium perchlorate solution against
    standard sulfuric acid to which 100 ml of 100% iso-
    propanol has been added.
  • Standardize sulfuric acid 0.0100  N against 0.0100 N
    sodium hydroxide.
 SLIDE  107-5

    SAMPLE METER SYSTEM CALIBRATION SETUP
                                       NOTES
                                        MANOMtlER
   THEHMOMEIER
                            THCRMOME lEfl
                     NEEDLE VALVE
                              AIR OUTLET
     SURGE TANK
                                                 WATER OUT
                                                    AOJUSI
                                         G-21

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 SLIDE 107-6                                            NOTES

     THERMOMETER CALIBRATION
• Impinger thermometer should agree to within 2°F
  of the standard at both points.
• Dry gas meter thermometer should agree to within
  5.4°F of the standard at both points.
                ROTAMETER
• calibration not required
• maintain according to manufacturer's instructions
                BAROMETER
• calibrate according to procedures in Method 2
 SLIDE 107-7

           ON SITE SAMPLING
 1. Prepare collection train.
 2. Conduct pretest leak-check (optional).
 3. Run the test.
 4. Conduct post test leak-check (mandatory).
 5. Purge sample train for 15 minutes.
 SLIDE 107-8
            SAMPLE RECOVERY
1. Disconnect impingers and discard contents of the
  bubbler.
2. Recover contents of the impingers into a leak-free
  polyethylene bottle.
3. Rinse impingers and connecting tubes with distilled
  water; add washings to sample bottle.
4. Mark liquid level, seal, and identify the container.
                                        G-23

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SLIDE 107-9                                              NOTES

                 SAMPLE ANALYSIS
1. Check liquid level of the sample.
2. Transfer sample to a 100 ml volumetric flask and dilute to
  100 ml with deionized distilled water.
3. Pipette a 20 ml aliquot into a 250 ml erlenmeyer flask.
4. Add 80 ml of 100% isopropanol and two to four drops of
  thorin indicator.
5. Titrate to a pink endpoint using 0.0100 N barium perchlorate.
6. Repeat and average titration volumes.
7. Run a blank with each series of samples.
                                          G-25

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                            SECTION H.  METHOD 7

Subject                                                               Page

1.  Method 7—-determination of nitrogen oxide emissions from
    stationary sources (taken from Environmental Protection Agency
    Performance Test Methods manual)                                  H-3

2.  Slides                                                            H-19
                                     H-l

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              METHOD 7--DETERMINATION OF NITROGEN OXIDE
                  EMISSIONS FROM STATIONARY SOURCES
1.  Principle and Applicability
     1.1  Principle.  A grab sample is collected in an evacuated
flask containing a dilute sulfuric acid-hydrogen peroxide absorbing
solution, and the nitrogen oxides, except nitrous oxide, are
measured colorimetrically using the phenoldisulfonic acid (PDS)
procedure.
     1.2  Applicability.  This method is applicable to the measure-
ment of nitrogen oxides emitted from stationary sources.  The range
of the method has been determined to be 2 to 400 milligrams NO  (as
                                                              A
NO^) per dry standard cubic meter, without having to dilute the sample.
2.  Apparatus
     2.1  Sampling  (see Figure /-I).  Other grab sampling systems or
equipment, capable  of measuring sample volume to within +2.0 percent
and collecting a sufficient sample volume to allow analytical reproduci-
bility to within +5 percent, will be considered acceptable alternatives,
subject to approval of the Administrator, U. S. Environmental Protection
Agency.  The following equipment is used in sampling:
     2.1.1  Probe.  Borosilicate glass tubing, sufficiently heated to
prevent water condensation and equipped with an in-stack or out-stack
filter to remove particulate matter (a plug of glass wool is satisfactory
for this purpose).  Stainless steel or Teflon  tubing may also be used
for the probe.  Heating is not necessary if the probe remains dry
during the purging  period.
 Mention of trade names or specific products does not constitute
 endorsement by the Environmental Protection Agency.
                         H-3

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       PROBE
           ^
                                         FLASK VALVE
                                                                                         SQUEEZE BULB

                                                                                      UMP VALVE
                                                                                              PUMP
       I
     FILTER
GROUND-GLASS SOCKET.
     § NO. 12/5
                 fv\/   50mm

             110mm'
3-WAY STOPCOCK;
T-BORE. J PYREX.
2-mm BORE. 8-mm OD
          GROUND-GLASS CONE.
           STANDARD TAPER,
          | SLEEVE NO. 24/40
                                          FLASK
   FLASKSHIELOL_t\
                                                         THERMOMETER
                                                     210 mm
GROUND-GLASS
SOCKET. §NO. 12/5
PYREX
                                                   •FOAM ENCASEMENT
                                                                               BOILING FLASK -
                                                                               2-LITER, ROUND-BOTTOM, SHORT NECK.
                                                                               WITH J SLEEVE NO. 24/40
                            Figure 7-1.  Sampling train, flask valve, and flask.

-------
     2.1.2  Collection Flask.  Two-liter borosilicate, round bottom
flask, with short neck and 24/40 standard taper opening, protected
against implosion or breakage.
     2.1.3  Flask Valve.  T-bore stopcock connected to a 24/40
standard taper joint.
     2.1.4  Temperature Gauge.  Dial-type thermometer, or other
temperature gauge, capable of measuring 1°C (2°F) intervals from -5
to 50°C (25 to 125°F).
     2.1.5  Vacuum Line.  Tubing capable of withstanding a vacuum
of 75 mm Hg (3 in. Hg) absolute pressure, with "T" connection and
T-bore stopcock.
     2.1.6  Vacuum Gauge.  U-tube manometer, 1 meter (36 in.), with
1-mm (0.1-in.) divisions, or other gauge capable of measuring pressure
to within +2.5 mm Hg  (0.10 in. hj).
     2.1.7  Pump.  Capable of evacuating the collection flask to a
pressure equal to or  less than 75 mm Hg (3 in. Hg) absolute.
     2.1.8  Squeeze Bulb.  One-way.
     2.1.9  Volumetric Pipette.  25 ml.
     2.1.10  Stopcock and Ground Joint Grease.  A high-vacuum, high-
temperature chlorofluorocarbon grease is required.  Halocarbon 25-5S
has been found to be  effective.
     2.1.11  Barometer.  Mercury, aneroid, or other barometer capable
of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
In many cases, the barometric reading may be obtained from a nearby
national weather service station, in which case the station value
                          H-5

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(which is the absolute barometric pressure)  shall  be  requested  and
an adjustment for elevation differences  between  the weather station
and sampling point shall  be applied at a rate of minus  2:5  mm Hg
(0.1 in.  Hg) per 30 m (100 ft)  elevation increase, or vice  versa
for elevation decrease.
     2.2   Sample Recovery.  The following equipment  is  required for
sample recovery:
     2.2.1  Graduated Cylinder.  50 ml with  1-ml divisions.
     2.2.2  Storage Containers.  Leak-free polyethylene bottles.
     2.2.3  Wash Bottle.   Polyethylene or glass.
     2.2.4  Glass Stirring Rod.
     2.2.5  Test Paper for Indicating pH.  To cover  the pH  range  of
7 to 14.
     2.3  Analysis.  For the analysis, the following equipment  is needed:
     2.3.1  Volumetric Pipettes.  Two 1  ml,  two 2  ml, one 3 ml, one
4 ml, two 10 ml, and one 25 ml  for each  sample and standard.
     2.3.2  Porcelain Evaporating Dishes.  175- to 250-ml capacity
with lip for pouring, one for each sample and each standard.  The
Coors No. 45006  (shallow-form, 195 ml) has been found to be satisfactory.
Alternatively, polymethyl pentene beakers (Nalge No.  1203, 150 ml),  or
glass beakers (150 ml) may be used.  When glass beakers are used, etching
of the beakers may cause solid matter to be present in the analytical
step; the solids should be removed by filtration  (see Section 4.3).
     2.3.3  Steam Bath.  Low-temperature ovens or thermostatically
controlled  hot plates kept below 70°C (160°F) are acceptable alternatives.
                           H-6

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     2.3.4  Dropping Pipette or Dropper.  Three required.
     2.3.5  Polyethylene Policeman.  One for each sample and each
standard.
     2.3.6  Graduated Cylinder.  100ml with 1-ml divisions.
     2.3.7  Volumetric Flasks.  50 ml (one for each sample and each
standard), 100 ml (one for each sample and each standard, and one for
the working standard KNO-, solution), and 1000 ml (one).
     2.3.8  Spectrophotometer.  To measure absorbance at 410 nm.
     2.3.9  Graduated Pipette.  10 ml with 0.1-ml divisions.
     2.3.10  Test Paper for Indicating pH.  To cover the pH range of 7
to 14.
     2.3.11  Analytical Balance.  To measure to within 0.1 mg.
3.  Reagents
     Unless otherwise indicate:!, it is intended that all reagents
conform to the specifications established by the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are
available; otherwise, use the best available grade.
     3.1  Sampling.  To prepare the absorbing solution, cautiously add
2.8 ml concentrated HgSO^ to 1 liter of deionized, distilled water.  Mix
well and add 6 ml of 3 percent hydrogen peroxide, freshly prepared from
30 percent hydrogen peroxide solution.  The absorbing solution should be
used within 1 week of its preparation.  Do not expose to extreme heat or
direct sunlight.
     3.2  Sample Recovery.  Two reagents are required for sample
recovery:
                           H-7

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     3.2.1  Sodium Hydroxide (1  Nj.   Dissolve 40 g NaOH  in  deionized,
distilled water and dilute to 1  liter.
     3.2.2  Water.  Deionized, distilled to conform to ASTM specifi-
cation 01193-74, Type 3.   At the option of the analyst,'the KMN04 test
for oxidizable organic matter may be omitted when= high concentrations
of organic matter are not expected to be present.
     3.3  Analysis.  For  the analysis,  the following reagents  are
required:
     3.3.1  Fuming SuIfuric Acid.  15 to 18 percent by weight  free
sulfur trioxide.  HANDLE  WITH CAUTION.
     3.3.2  Phenol.  White solid.
     3.3.3  Sulfuric Acid.  Concentrated, 95 percent minimum assay.
HANDLE WITH CAUTION.
     3.3.4  Potassium Nitrate.  Dried at 105 to 110°C (220  to  230°F)
for a minimum of 2 hours  just prior to preparation of standard solution.
     3.3.5  Standard KN03 Solution.   Dissolve exactly 2.198 g  of dried
potassium nitrate (KNO-)  in deionized,  distilled water and  dilute
to 1 liter with deionized, distilled water in a 1000-ml  volumetric
flask.
    •
     3.3.6  Working Standard KNO- Solution.  Dilute 10 ml of the
standard solution to 100 ml with deionized distilled water. One
milliliter of the working standard solution is equivalent to 100 yg
nitrogen dioxide (NOp).
     3.3.7  Water.  Deionized, distilled as in Section 3.2.2.
                         H-8

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     3.3.8  Phenoldisulfonic Acid Solution.  Dissolve 25 g of pure
white phenol in 150 ml concentrated sulfuric acid on a steam bath.
Cool, add 75 ml fuming sulfuric acid, and heat at 100°C (212°F) for
2 hours.  Store in a dark, stoppered bottle.
4.  Procedures
     4.1  Sampling.
     4.1.1  Pipette 25 ml of absorbing solution into a sample flask,
retaining a sufficient quantity for use in preparing the calibration
standards.  Insert the flask valve stopper into the flask with the
valve in the "purge" position.  Assemble the sampling train as shown
in Figure 7-1 and place the probe at the sampling point.  Make sure
that all fittings are tight and leak-free, and that all ground glass
joints have been property-greased with a high-vacuum, high-temperature
chlorofluorocarbon-based stopcock grease.  Turn the flask valve and the
pump valve to their "evacuate" positions.  Evacuate the flask to
75 mm Hg (3 in. Hg) absolute pressure,, or less.  Evacuation to a
pressure approaching the vapor pressure of water at the existing
temperature is desirable.  Turn the pump valve to its "vent" position
and turn off the pump.  Check for leakage by observing the manometer
for any pressure fluctuation.  (Any variation greater than 10 mm Hg
(0.4 in. Hg) over a period of 1 minute is not acceptable, and the
flask is not to be used until the leakage problem is corrected.
Pressure in the flask is not to exceed 75 mm Hg (3 in. Hg) absolute
at the time sampling is commenced.)  Record the volume of the flask
and valve (Vf), the flask temperature (T^, and the barometric pres-
sure.  Turn the flask valve counterclockwise to its "purge" position
                             H-9

-------
 and do the  same with the pump valve.  Purge the probe and the vacuum
 tube using  the squeeze bulb.  If condensation occurs in the probe
 and the flask"valve area, heat the probe and purge until the con-
 densation disappears.  Next, turn the pump valve to its "vent" position.
 Turn  the flask valve clockwise to its "evacuate" position and record
 the difference in the mercury levels in the manometer.  .The absolute
 internal pressure in the flask (P..) is equal to the barometric pres-
 sure  less the manometer reading.  Immediately turn the flask valve to
 the "sample" position and permit the gas to enter the flask until
 pressures in the flask and sample line (i.e., duct, stack) are
equal.  This will usually require about 15 seconds; a longer period
 indicates a "plug" in the probe, which must be corrected before
 sampling is continued.  After collecting the sample, turn the flask
valve to its "purge" position and disconnect the flask from the
 sampling train.  Shake the flask for at least 5 minutes.
     4.1.2  If the gas being sampled contains insufficient oxygen
 for the conversion of NO to ML (e.g., an applicable subpart of the
 standard may require taking a sample of a calibration gas mixture of NO
 in N2), then oxygen shall be introduced into the flask to permit this
 conversion.  Oxygen may be introduced into the flask by one of
 three methods:  (1) Before evacuating the sampling flask, flush
with pure cylinder oxygen, then evacuate flask to 75 mm Hg (3 in.
Hg) absolute pressure or less; or (2) inject oxygen into the flask
after sampling; or (3) terminate sampling with a minimum of 50 mm Hg
 (2 in. Hg) vacuum remaining in the flask, record this final pressure,
and then vent the flask to the atmosphere until the flask pressure is
almost equal to atmospheric pressure.
                                  H-10

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     4.2   Sample Recovery.   Let the flask set for a minimum of 16 hours
and then  shake the contents for 2 minutes.  Connect the flask to a mercury
filled U-tube manometer.   Open the valve from the flask to the
manometer and record the  flask temperature (T^), the barometric
pressure, and the difference between the mercury levels in the
manometer.  The absolute  internal pressure in the flask (PJ is
the barometric pressure less the manometer reading.  Transfer the
contents  of the flask to  a leak-free polyethylene bottle.  Rinse
the flask twice with 5-ml portions of deionized, distilled water
and add the rinse water to the bottle.  Adjust the pH to between 9 and
12 by adding sodium hydroxide (1 N_), dropwise (about 25 to 35 drops).
Check the pH by dipping a stirring rod into the solution and then
touching the rod to the pH test paper.  Remove as little material as
possible during this step.  Mark the height of the liquid level so
that the container can be checked for leakage after transport.  Label
the container to clearly  identify its contents.  Seal the container
for shipping.
     4.3  Analysis.  Note the level of the liquid in container and con-
firm whether or not any sample was lost during shipment; note this on
the analytical data sheet.  If a noticeable amount of leakage has
occurred, either void the sample or use methods, subject to the approval
of the Administrator, to correct the final results.  Immediately prior
to analysis, transfer the contents of the shipping container to a 50-ml
volumetric flask, and rinse the container twice with 5-ml portions of
deionized, distilled water.  Add the rinse water to the flask and dilute
to the mark with deionized, distilled water; mix thoroughly.  Pipette
                                 K-ll

-------
a 25-ml aliquot into the porcelain evaporating dish.   Return  any
unused portion of the sample to the polyethylene storage bottle.
Evaporate the 25-ml  aliquot to dryness on a steam bath and allow  to
cool.  Add 2 ml phenoldisulfonic acid solution to the dried residue and
triturate thoroughly with a polyethylene policeman.   Make sure the solu-
tion contacts all  the residue.  Add 1 ml deionizerf,  distilled water and
four drops of concentrated sulfuric acid.  Heat the  solution  on a
steam bath for 3 minutes with occasional stirring.  Allow the solution
to cool, add 20 ml deionized, distilled water, mix well by stirring,
and add concentrated ammonium hydroxide, dropwise, with constant  stirring,
until the pH is 10 (as determined by pH paper).  If  the sample contains
solids, these must be removed by filtration (centrifugation is an
acceptable alternative, subject to the approval of the Administrator),
as follows:  filter through Whatman No. 41 filter paper into  a 100-ml
volumetric flask; rinse the evaporating dish with three 5-ml  portions
of deionized, distilled water; filter these three rinses.  Wash the
filter with at least three 15-ml portions of deionized, distilled water.
Add the filter washings to the contents of the volumetric flask and
dilute to the mark with deionized, distilled water.   If solids are
absent, the solution can be transferred directly to the 100-ml volumetric
flask and diluted to the mark with deionized, distilled water. Mix
the contents of the flask thoroughly, and measure the absorbance  at
the optimum wavelength used for the standards (Section 5.2.1), using the
blank solution.as a zero reference.  Dilute the sample and the blank
with equal volumes of deionized, distilled water if the absorbance
exceeds A., the absorbance of the 400 ug N0« standard  (see Section 5.2.2).
                                 H-12

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5.  Calibration
     5.1  Flask, Volume.  The volume of the collection flask-flask valve
combination must be known prior to sampling.  Assemble the flask and
flask valve and fill with water, to the stopcock.  Measure the volume of
water to +10 ml.  Record this volume on the flask.
     5.2  Spectrophotometer Calibration.
     5.2.1  Optimum Wavelength Determination.  Calibrate the wavelength
scale of the Spectrophotometer every 6 months.  The calibration may be
accomplished by using an energy source with an intense line emission
such as a mercury lamp, or by using a series of glass filters spanning
the measuring range of the Spectrophotometer.  Calibration materials are
available commercially and from the National Bureau of Standards.
Specific details on the use of such materials should be supplied by the
vendor; general information about calibration techniques can be obtained
from general reference books on analytical chemistry.  The wavelength
scale of the Spectrophotometer must read correctly within +5 nm at all
calibration points; otherwise, the Spectrophotometer shall be repaired
and recalibrated.  Once the wavelength scale of the Spectrophotometer is
in proper calibration, use 410 nm as the optimum wavelength for the
measurement of the absorbance of the standards and samples.
                           H-13

-------
     Alternatively, a scanning procedure may be employed to determine
 the proper measuring wavelength.  If the instrument is a double-beam
 spectrophotometer, scan the spectrum between 400 and 415 nm using a 200 yg
 N0« standard solution in the sample cell and a blank solution in the
 reference cell.  If a peak does not occur, the spectrophotometer is
 probably malfunctioning and should be repaired.  When a peak is obtained
within the 400 to 415 nm range, the wavelength at which this peak occurs
shall be the optimum wavelength for the measurement of absorbance of
both the standards and the samples.  For a single-beam spectrophotometer,
follow the scanning procedure described above, except that the blank and
                                                     4
standard solutions shall be scanned separately.  The optimum wavelength
shall be the wavelength at which the maximum difference in absorbance
between the standard and -the blank occurs.
     5.2.2  Determination-of Spectrophotometer Calibration Factor KC.
Add 0.0 ml, 2.0 ml, 4.0 ml, 6.0 ml, and 8.0 ml of the KN03 working
standard solution (1 ml = 100 yg N02) to a series of five 50-ml volumetric
flasks.  To each flask, add 25 ml of absorbing solution,
 10 ml deionized, distilled water, and sodium hydroxide (IN) dropwise
until the pH is between 9 and 12 (about 25 to 35 drops each).  Dilute
 to the mark with deionized, distilled water.  Mix thoroughly and
pipette a 25-ml aliquot of each solution into a separate porcelain
evaporating dish.  Beginning with the evaporation step, follow the
analysis procedure of Section 4.3, until the solution has been trans-
 ferred to the 100-ml volumetric flask and diluted to the mark.  Measure
 the absorbance of each solution, at the optimum wavelength, as
                                           i
 determined in Section 5.2.1.  This calibration procedure must be repeated
                           H-14

-------
on each day that samples are analyzed.  Calculate the spectrophotometer
calibration factor as follows:
                  A, + 2A, + 3A- + 4A.
         K  =100 -^	^75	^j	-9               Equation 7-1
          c       A^ + A+A+A
                  H1  + M2  + M3  i- M4
where:
     K  = Calibration factor
      C
     A, = Absorbance of the 100-yg N02 standard
     A2 = Absorbance of the 200-yg N02 standard
     A3 = Absorbance of the 300-yg N02 standard
     A. = Absorbance of the 400-vg N02 standard

     5.3  Barometer.  Calibrate against a mercury barometer.
     5.4  Temperature Gauge.   Calibrate dial  thermometers against
mercury-in-glass  thermometers,
     5.5  Vacuum  Gauge.   Calibrate mechanical  gauges,  if used,
against a mercury manometer  such  as  that  specified  in  2.1.6.
      5.6  Analytical  Balance.   Calibrate  against standard weights.
6.   Calculations
      Carry  out the calculations,  retaining  at least one extra
decimal  figure beyond that of the acquired  data.   Round off
figures  after final calculations.
      6.1   Nomenclature.
      A  = Absorbance of sample.
      C  = Concentration of N0x as N02> dry  basis,  corrected to
           standard conditions, mg/dscm (Ib/dscf).
                          H-15

-------
     F   =  Dilution factor (i.e., 25/5, 25/10, etc., required  only



          if sample dilution was needed to reduce the absorbance



          into the range of calibration).



     K   =  Spectrophotometer calibration factor.



     m   =  Mass of NO  as N09 in gas sample, yg.
                   r*      Cm.


     Pf  =  Final absolute pressure of flask, mm Hg (in. Hg).



     P.  =  Initial absolute pressure of flask, mm Hg (iri.  Hg).



     P   .  = Standard absolute pressure, 760 mm Hg (29.92  in.  Hg).



     Tf  =  Final absolute temperature of flask, °K (°R).



     T1  =  Initial absolute temperature of flask, °K (°R).



     T  ..  = Standard absolute temperature, 293°K (528°R).



     V     = Sample volume at standard conditions (dry basis), ml.
     5C


     V.p  =  Volume of flask and valve, ml.



     V   =  Volume of absorbing solution, 25 ml.
     a


     2   =  50/25, the aliquot factor.   (If other than a 25-ml



          aliquot was used for  analysis, the corresponding factor



          must be substituted).



     6.2  Sample volume, dry basis, corrected  to standard



conditions.
sc
        std
-v
=  K]  (Vf - 25 ml)
                                                             Pi
                                                             J-

                                                             'i
                                                      Equation 7-2
                          H-16

-------
where:
     K.J  =  °-3858 JSTRq  for metric units
         = 17.64   . *RUM  for English units
                   in. ng
     6.3  Total vg N02 per sample.
          m = 2K AF                                   Equation 7-3
     Note:  If other than a 25-ml aliquot is used for analysis, the
factor 2 must be replaced by a corresponding factor.
     6.4  Sample concentration, dry basis, corrected to standard
conditions.
      c   =   K2 T~                                    Equation 7-4
                sc
 where:
                    ,3
      K2  =  10   TigTrnT  for metr1c un1ts
            6.243 x 10"5        for English  units
 7.   Bibliography
      1.   Standard Methods of Chemical  Analysis.   6th ed.  New York,
 D.  Van Nostrand Co., Inc.  1962.  Vol. 1, p.  329-330.
      2.   Standard Method of Test for Oxides of Nitrogen in Gaseous
 Combustion Products (Phenoldisulfonic Acid Procedure).   In:  1968 Book
 of ASTM Standards, Part 26.  Philadelphia, Pa.  1968.   ASTM Designation
 D-1608-60, p. 725-729.
      3.   Jacob, M. B.  The Chemical Analysis of Air Pollutants.
 New York.  Interscience Publishers, Inc.  1960.  Vol. 10, p. 351-356.
                          H-17

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     4.  Beatty, R.  L.,  L.  B.  Berger, and H.  H. Schrenk.   Determination
of Oxides of Nitrogen by the Phenoldisulfonic Acid Method,  Bureau of
Mines, U. S. Dept.  of Interior.   R.  I. 3687.   February 1943.
     5.  Hamil, H.  F. and D. E.  Camann.  Collaborative Study of Method
for the Determination of Nitrogen Oxide Emissions from Stationary
Sources (Fossil Fuel-Fired Steam Generators).  Southwest Research
Institute report for Environmental Protection Agency.  Research Triangle
Park, N. C.  October 5,  1973.
     6.  Hamil, H.  F. and R. E.  Thomas.  Collaborative Study of Method
for the Determination of Nitrogen Oxide Emissions from Stationary
Sources (Nitric Acid Plants).   Southwest Research Institute report for
Environmental Protection Agency.  Research Triangle Park, N. C.
May 8, 1974.
                         H-18

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SLIDE 108-0

    METHOD — 7
    Determination of
Nitrogen Oxide Emissions
From Stationary Sources
                  NOTES
SLIDE 108-1

         PRINCIPLE

A GRAB sample is collected in an
evacuated flask.
Nitrogen oxides (NOK), except nitrous
oxide, are measured colorimetrically.

       APPLICABILITY
This method is applicable for the
measurement of  NO,  emissions from
stationary sources.
 SLIDE  108-2

    EVACUATED FLASK SAMPLING TRAIN
           PROBE
 FUER
EVACUATE

PURGE


SAMPLE
                                            SQUEEZE BULB
                             FLASK
                             VALVE  THERMOMETER
                   FLASK SHIELD
                                              PURGE
                                     H-19

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SLIDE  108-3                                         NOTES


SPECIAL ANALYTICAL APPARATUS

   • Porcelain Evaporating Dishes
   • Spectrophotometer
 SLIDE  108-4


        SPECIAL REAGENTS

       ABSORBING SOLUTION
  The absorbing solution consists of concen-
 trated H2SO4, deionized distilled water, and 3%
 hydrogen peroxide.

      STANDARD KNO3 SOLUTION
  The standard KNO3 solution consists of 2.198g
 of potassium nitrate dissolved in 1 liter of deion-
 ized distilled water.

 WORKING STANDARD KNO3 SOLUTION
  The working standard KNO3 solution consists
 of 10 ml of standard solution diluted to 100 ml
 with deionized distilled water.
 SLIDE 108-5

  COLLECTION FLASK CALIBRATION

 1. Assemble clean flasks and valves.
 2. Fill flask with room temperature water.
 3. Measure flask volume to ±10 ml.
 4. Number each flask and record volume on flask
  or foam case.
 5. Only one calibration is required if flasks and
  valves are not switched.
                                      H-21

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 SLIDE 108-6                                        NOTES

SPECTROPHOTOMETER CALIBRATION

 OPTIMUM WAVELENGTH DETERMINATION
   Calibrate against a standard with a certified
  wavelength of 410 nm every 6 months.
   Alternatively, for variable wavelength spectro-
  photometers scan the spectrum between 500
  and 415 nm  using a 200 ng NO2 standard
  solution.
   When a peak is obtained, the wavelength at
  which this peak occurs shall be the optimum
  wavelength.
 SLIDE 108-7

SPECTROPHOTOMETER CALIBRATION

 CALIBRATION FACTOR DETERMINATION
 • Prepare calibration solutions containing 0.0,1.0,
  2.0, 3.0 and 4.0 ml of the KNO3 working stand-
  ard solution.
 • Measure absorbance of each  solution at the
  optimum wavelength.
 • Determine calibration factor each day that sam-
  ples are analyzed.
SLIDE  108-8

    CALIBRATION FACTOR CALCULATION
             Ai + 2A2 + 3A3 + 4A4
                                 +    2
                                    H-23

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SLIDE  108-9,                                            NOTES

            ONSITE SAMPLING
1. Pipette 24 ml of absorbing solution into a sample
  flask.
2. Place probe at sampling point and connect to train.
3. Evacuate flask to 3 in. Hg absolute pressure or less.
4. Turn of pump and check for leaks.
5. Record volume of flask and valve, flask tempera-
  ture, and barometric pressure.
6. Purge the probe and vacuum tubing.
 SLIDE  108-10
 (cont.)          ONSITE SAMPLING
     7. Measure absolute flask pressure.
     8. Turn flask valve to "sample" permitting stack gas to
       enter flask.
     9. Turn flask to "purge"  and disconnect flask from
       train.
    10. Shake flask for at least 5 minutes.
  SLIDE 108-11
  ADDING SUPPLEMENTAL OXYGEN
  1. Flush cyliner with  pure oxygen  prior to
   evacuation.
  2. Inject oxygen into flask after sampling.
  3. Terminate sampling with minimum vacuum
   of 2 in. Hg and vent flask to the atmosphere.
                                         H-25

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   SLIDE  108-12                                             NOTES

                SAMPLE RECOVERY

   1. Let flask set for minimum of 16 hours.
   2. Shake flask for 2 min.
   3. Measure absolute pressure in flask.
   4. Record flask temperature and barometric pressure.
   5. Transfer content of flask to leak-free  polyethylene
    bottle.
   6. Adjust PH to between 9 and 12.
   7. Mark liquid level, seal, and identify container.
   SLIDE 108-13

                    ANALYSIS

   1. Check liquid level of sample container.
   2. Transfer sample to a 50 ml  volumetric flask; di-
     lute to volume and mix thoroughly.
   3. Pipette a 25 ml aliquot into the porcelain evapo-
     ration dish and evaporate on a steam bath.
   4. Add 2 ml phenoldisulfonic acid solution to dried
     residue and triturate.
   5. Add 1 ml deionized distilled water, four drops of
     concentrated sulfuric acid, and heat on a steam
     bath for 3 min.
    SLIDE  108-14

(cont.)                ANALYSIS

    6. Allow solution to cool; add 20 ml deionized distilled
      water; add concentrated ammonium hydroxide until
      PHislO.
    7. Remove solids if necessary.
    8. Transfer solution to a 100 ml volumetric flask and
      dilute to mark with distilled water.
    9. Mix contents of flask thoroughly and measure the
      absorbance using the blank solution as a  zero
      reference.
   10. Dilute the sample and blank with equal volumes of
      distilled water if absorbance exceeds A4.
                                              H-27

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                            SECTION I.  METHOD 8

Subject                                                               Page

1.  Method 8—determination of sulfuric acid mist and sulfur dioxide
    emissions from stationary sources (taken from Environmental  Pro-
    tection Agency Performance Test Methods manual)                   1-1

2.  Slides                                                            1-21
                                     1-1

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          METHOD 8—DETERMINATION OF SULFURIC ACID MIST AND
           SULFUR DIOXIDE EMISSIONS FROM STATIONARY SOURCES

1.  Principle and Applicability
     1.1  Principle.  A gas sample is extracted isokinetically from the
stack.  The sulfuric acid mist (including sulfur trioxide) and the
sulfur dioxide are separated, and both fractions are measured separately
by the barium-thorin titration method.
     1.2  Applicability.  This method is applicable for the determi-
nation of sulfuric acid mist (including sulfur trioxide, and in the
absence of other particulate matter) and sulfur dioxide emissions from
stationary sources.  Collaborative tests have shown that the minimum
detectable limits of the method are 0.05 milligrams/cubic meter (0.03
x 10~  pounds/cubic foot') for sulfur trioxide and 1.2 mg/m (0.74 x 10
     3                ~
Ib'/ft ) for sulfur .dioxide.  No upper limits have been established.
Based on theoretical calculations for 200 milliliters of 3 percent
hydrogen peroxide solution, the upper concentration limit for sulfur
                  33                                 3
dioxide in a 1.0 m  (35.3 ft ) gas sample is about 12,500 mg/m  (7.7 x
10   Ib/ft ).  The upper limit can be extended by increasing the
quantity of peroxide solution in the impingers.
     Possible interfering agents of this method are fluorides, free
ammonia, and dimethyl aniline.  If any of these interfering agents are
present (this can be determined by knowledge of the process), alterna-
tive methods, subject to the approval of the Administrator,
 U.  S. Environmental Protection Agency, are required.
                                 1-3

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      Filterable participate matter may be determined along with S03 and
 S02  (subject to the approval of the Administrator) by inserting a heated
 glass fiber filter between the probe and isopropanol impinger (see
     *
 Section 2.1 of Method 6).   If this option is chosen, participate
 analysis is gravimetric only; HgSO^ acid mist is not determined separately.
 2.  Apparatus
     2.1  Sampling.  A schematic of the sampling train used in this
method is shown in Figure 8-1; it is similar to the Method 5 train
except that the filter position is different and the filter holder does
not have to be heated.  Commercial models of this train are available.
For those who desire to build their own, however, complete construction
details are described in APTD-0581.  Changes from the APTD-0581 document
and allowable modifications to Figure 8-1 are discussed in the following
subsections.
     The operating and maintenance procedures for the sampling train are
described in APTD-0576.  Since correct usage is important in obtaining
valid results, all users should read the APTD-0576 document and adopt
the operating and maintenance procedures outlined in it, unless otherwise
specified herein.  Further details and guidelines on operation and
maintenance are given in Method 5 and should be read and followed
whenever they are applicable.
     2.1.1  Probe Nozzle.   Same as Method 5, Section 2.1.1.
                                                          t
     2.1.2  Probe Liner.  Borosilicate or quartz glass, with a heating
system to prevent visible condensation during sampling.  Do not use
metal probe liners.
     2.1.3  Pi tot Tube.  Same as Method 5, Section 2.1.3.
                                1-4

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                    TEMPERATURE SENSOR




                             - PROBE
                                                                             THERMOMETER
                                                                                      CHECK

                                                                                      VALVE
         7
REVERSE TYPE
 PITOT TUBE
PITOTTUBE

TEMPERATURE SENSOR
                                              ICE BATH          IMPINGERS



                                                   BY-PASS VALVE
                                                                                           VACUUM

                                                                                             LINE
                                                                                        VACUUM

                                                                                         GAUGE
                                                                               MAIN VALVE
                         DKY TEST METER


                              Figure 8-1.  Sulfuric acid mist sampling train.

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     2.1.4  Differential  Pressure  Gauge.   Same  as  Method  5,  Section
2.1.4.
     2.1.5  Filter Holder.   Borosilicete  glass, with  a  glass frit
filter support and a silicone rubber gasket.   Other gasket materials,
e.g., Teflon or Viton, may be used subject to the  approval of the
Administrator.  The holder design  shall  provide a  positive seal  against
leakage from the outside or around the filter.   The filter holder  shall
be placed between the first and second impingers.   Note:   Do not heat
the filter holder.
     2.1.6  Impingers--Four, as shown in Figure 8-1.   The first and
third shall be of the Greenburg-Smith design with standard tips.  The
second and fourth shall be of the Greenburg-Smith design, modified by
replacing the insert with an approximately 13 millimeter  (0.5 in.)
ID glass tube, having an unconstricted tip located 13 mm  (0.5 in.)
from the bottom of the flask.  Similar collection systems, which have
been approved by  the Administrator, may be used.
     2.1.7  Metering System.  Same as Method 5, Section 2.1.8.
     2.1.8  Barometer.  Same as Method 5, Section 2.1.9.
     2.1.9  Gas Density Determination Equipment.  Same as Method 5,
Section  2.1.10.
      2.1.10   Temperature Gauge.   Thermometer,  or equivalent, to measure
the  temperature of  the gas  leaving the impinger train to  within 1°C
(2°F).
      2.2  Sample  Recovery.
      2.2.1  Wash  Bottles.   Polyethylene or glass, 500 ml. (two).
      2.2.2 Graduated  Cylinders.   250ml, 1  liter.   (Volumetric flasks
may  also be used.)
                          1-6

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     2.2.3  Storage Bottles.   Leak-free polyethylene bottles,
1000 ml  size (two for each sampling run).
     2.2.4-  Trip Balance.  500-gram capacity, to measure to +0.5 g
(necessary only if a moisture content analysis is to be done).
     2.3  Analysis.
     2.3.1  Pipettes.  Volumetric 25 ml, 100ml.
     2.3.2  Burette.  50ml.
     2.3.3  Erlenmeyer Flask.  250 ml. (one for each sample blank
and standard).
     2.3.4  Graduated Cylinder.  100 ml.
     2.3.5  Trip Balance.  500 g capacity, to measure to +0.5 g.
     2.3.6  Dropping Bottle.  To add indicator solution, 125-ml size,
3.  Reagents
     Unless otherwise indicated, all reagents are to conform to the
specifications established by the  Committee  on Analytical Reagents of
the American  Chemical Society, where such specifications are available.
Otherwise, use the  best  available  grade.
     3.1  Sampling.
     3.1.1  Filters.  Same as Method 5, Section  3.1.1.
     3.1.2  Silica  Gel.   Same as Method 5, Section  3.1.2.
     3.1.3  Water.   Deionized, distilled to  conform to  ASTM specification
 01193-74, Type  3.   At the option of the analyst,  the KMn04 test for
 oxidizable  organic  matter may be omitted when high  concentrations of
 organic matter  are  not expected to be  present.
                                  1-7

-------
      3.1.4  Isopropanol, 80 Percent.  Mix 800 ml of isopropanol with 200
ml of deiom'zed, distilled water.
      Note:  Experience has shown that only A.C.S. grade isopropanol is
satisfactory.  Tests have shown that isopropanol obtained from commercial
sources occasionally has peroxide impurities that will cause erroneously
high  sulfuric acid mist measurement.  Use the following test for
detecting peroxides in each lot of isopropanol: Shake 10 ml  of the
isopropanol  with 10 ml of freshly prepared 10 percent potassium iodide
solution.  Prepare a blank by  similarly treating 10 ml of distilled
water.  After 1 minute, read the absorbance on a spectrophotometer at
352 nanometers (Note:   Use a 1  cm path length).  If the absorbance
exceeds 0.1, the isopropanol shall not be used.  Peroxides may be removed
from isopropanol by redistilling, or by passage through a column of
activated alumina.  However, reagent-grade isopropanol with suitably low
peroxide levels is readily available from commercial sources; therefore,
rejection of contaminated lots  may be more efficient than following the
peroxide removal procedure.
     3.1.5  Hydrogen Peroxide,  3 Percent.  Dilute 100 ml of 30 percent
hydrogen peroxide to 1 liter with deionized, distilled water.  Prepare
fresh daily.
     3.1.6  Crushed Ice.
     3.2  Sample Recovery.
     3.2.1  Water.  Same as 3.1.3.
     3.2.2  Isopropanol, 80 Percent.  Same as 3.1.4.
     3.3  Analysis.
     3.3.1  Water.  Same as 3.1.3.
                                   1-8

-------
     3.3.2  Isopropanol,  100 Percent.
     3.3.3  Thorin Indicator.  l-(o-arsonophenylazo)-2-naphthol-3,
6-disulfonic acid, disodium salt, or equivalent.  Dissolve 0.20 g
in 100 ml of deionized, distilled water.
     3.3.4  Barium Perchlorate (0.0100 Normal).  Dissolve 1.95 g of
barium perchlorate trihydrate (Ba(C104)2'3H20) in ZOO ml  deionized,
distilled water, and dilute to 1 liter with isopropanol;  1.22 g of
barium chloride dihydrate (BaClg^HgO) may be used instead of the
barium perchlorate.  Standardize with sulfuric acid as in Section 5.2.
This solution must be protected against evaporation at all times.
     3.3.5  Sulfuric Acid Standard (0.0100 N).  Purchase  or standardize
to +0.0002 N against 0.0100 N NaOH that has previously been standardized
against primary standard potassium acid phthalate.
4.  Procedure
     4.1  Sampling.
     4.1.1  Pretest Preparation.  Follow the procedure outlined in
Method 5, Section 4.1.1; filters should be inspected, but need not be
desiccated, weighed, or identified.   If the effluent gas  can be
considered dry, i.e., moisture free,  the silica gel need  not be weighed.
     4.1.2  Preliminary Determinations.  Follow the procedure outlined
in Method 5, Section 4.1.2.
     4.1.3  Preparation of Collection Train.   Follow the procedure
outlined  in Method 5,  Section 4.1.3 (except for the second paragraph
and other obviously inapplicable parts) and use Figure 8-1 instead of
Figure 5-1.  Replace the second paragraph with:   Place 100 ml of
                            1-9

-------
80 percent isopropanol in the first impinger,  100 ml  of 3 percent
hydrogen peroxide in both the second and third impingers; retain a
portion of each reagent for use as a blank solution.   Place about
200 g of silica gel  in the fourth impinger.
     Note:   If moisture content is to be determined by impinger analysis,
weigh each of the first three impingers (plus  absorbing solution) to
the nearest 0.5 g and record these weights.  The weight of the silica
gel (or silica gel  plus container) must also be determined to the nearest
0.5 g and recorded.
     4.1.4  Pretest Leak-Check Procedure.  Follow the basic procedure
outlined in Method 5, Section 4.1.4.1, noting  that the probe heater
shall be adjusted to the minimum temperature required to prevent
condensation, and also that verbage such as, ". . . plugging the
inlet to the filter holder . . . ," shall be replaced by, "... plugging
the inlet to the first impinger . . . ."  The  pretest leak-check is
optional.
     4.1.5  Train Operation.  Follow the basic procedures outlined in
Method 5, Section 4.1.5, in conjunction with the following special
instructions.  Data shall be recorded on a sheet similar to the one
                                                          3
in Figure 8-2.  The sampling rate shall not exceed 0.030 m /min
(1.0 cfm) during the run.  Periodically during the test, observe the
connecting line between the probe and first impinger for signs of
condensation.  If it does occur, adjust the probe heater setting
upward to the minimum temperature required to  prevent condensation.
If component changes become necessary during a run, a leak-check shall
                                  1-10

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 PLANT	
 LOCATION	
 OPERATOR	
 DATE	
 RUN NO	
SAMPLE BOX NO..
METER BOX N0._
METERAH®	
CFACTOR	
PITOT TUBE COEFFICIENT. Cp
STATIC PRESSURE . nvn H0 tln.Mf)).
AMBIENT TEMPERATURE	
BAROMETRIC PRESSURE	
ASSUMED MOISTURE, V,	
PROBE LENGTH, m (It)	
                                    SCHEMATIC OF STACK CROSS SECTION
NOZZLE IDENTIFICATION NO	
AVERAGE CALIBRATED NOZZLE DIAMETER, cm (in,).
PROBE HEATER SETTING	
LEAK RATE.m3/min,(cftn)	
PROBE LINER MATERIAL	
FILTER NO/	
TRAVERSE POINT
NUMBER












TOTAL
SAMPLING
TIME
(01, min.













AVERAGE
VACUUM
nun Hg
(in.Hg)














STACK
TEMPERATURE
(Tc),
°C (*F) .














VELOCITY
HEAD
(A PS),
mm HjO
(in.H20)














PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE
METER,
mm H20
(in. H20)














GAS SAMPLE
VOLUME,
m3 (h3)














GAS SAMPLE TEMPERATURE
AT DRY GAS METER
INLET,
°C(°F)












Avg
Avg
OUTLET,
°C(°F)












Avg

TEMPERATURE
OF GAS
LEAVING
CONDENSER OR
LASTIMPINGER,
°C (°F)














                                                 Figure 8-2.  Field data.

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be.done immediately  before  each  change,  according  to  the  procedure
outlined in Section  4.1.4.2 of Method  5  (with  appropriate modifica-
tions, as mentioned  in  Section 4.1.4 of  this method); record  all
leak rates.  If the  leakage rate(s)  exceed the specified  rate,  the
tester shall either  void the run or  shall  plan to  correct the sample
volume as outlined in Section 6.3 of Method 5.  Immediately after
component changes, leak-checks are optional.   If these leak-checks
are done, the procedure outlined in  Section 4.1.4.1  of Method 5
(with appropriate modifications) shall be used.
     After turning off the pump and recording the final readings at
the conclusion of each run, remove the probe from the stack.   Conduct
a post-test (mandatory) leak-check as in Section 4.1.4.3 of Method  5
(with appropriate modifications) and record the leak rate.  If the
post-test  leakage rate exceeds the specified acceptable rate, the
tester  shall either correct the  sample volume, as outlined in
Section 6.3 of Method  5, or shall void the run.
      Drain the ice  bath and,  with the probe disconnected, purge  the
remaining  part of the  train,  by  drawing clean  ambient  air through the
system for 15 minutes  at the  average  flow rate used  for  sampling.
      Note:  Clean ambient  air can be  provided by  passing  air through
a charcoal filter.   At the option of  the  tester,  ambient air  (without
cleaning)  may  be used.
      4.1.6  Calculation of Percent  Isokinetic.  Follow the procedure
outlined in Method  5,  Section 4.1.6.
                             1-12

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     4.2  Sample Recovery.
     4.2.1  Container No. 1.  If a moisture content analysis is to
be done, weigh-the first impinger plus contents to the nearest 0.5 g
and record this weight.
     Transfer the contents of the first impinger to a 250-ml graduated
cylinder.  Rinse the probe, first impinger, all connecting glassware
before the filter, and the front half of the filter holder with 80 per-
cent isopropanol.  Add the rinse solution to the cylinder.  Dilute to
250 ml with 80 percent isopropanol.  Add the filter to the solution,
mix, and transfer to the  storage container.  Protect the solution against
evaporation.  Mark the level of liquid on the container and identify the
sample container.
     4.2.2  Container  No. 2.  If a moisture content analysis is to be
done, weigh the  second and  third impingers  (plus contents)  to the nearest
0.5 g and record  these weights.  Also, weigh the spent silica gel (or
silica gel plus  impinger) to the nearest 0.5 g.
     Transfer the solutions from the  second and third  impingers to a
1000-ml  graduated cylinder.  Rinse all connecting  glassware (including
back  half of filter  holder) between the filter  and silica  gel  impinger
with  deionized,  distilled water,  and  add this  rinse water  to the  cylinder.
Dilute  to a volume of 1000  ml with deionized,  distilled water.  Transfer
 the  solution to a storage container.   Mark  the  level  of liquid  on the
 container.  Seal  and identify the  sample container.
      4.3 Analysis.
      Note the  level  of liquid in  containers  1  and  2,  and  confirm  whether
 or not  any  sample was lost during  shipment;  note  this on  the analytical
 data sheet.   If a noticeable  amount of leakage has occurred, either void
 the sample  or  use methods, subject to the  approval of the Administrator,
 to correct  the final results.
                                   1-13

-------
     4.3.1  Container No. 1.   Shake the container holding the
 isopropanol solution and the  filter.  If the filter breaks up,
 allow the fragments to settle for a few minutes before removing
 a sample.  Pipette a 100-ml aliquot of this solution into a 250-ml
 Erlenmeyer flask, add 2 to 4  drops of thorin indicator, and titrate
 to a pink endpoint using 0.0100 N barium perchlorate.   Repeat the
 titration with a second aliquot of sample and average  the titration
 values.   Replicate titrations must agree within 1 percent or 0.2 ml,
whichever is greater.
     4.3.2  Container No. 2.   Thoroughly mix the solution in the
container holding the contents of the second and third impingers.
Pipette  a 10-ml aliquot of sample into a 250-ml Erlenmeyer flask.
Add 40 ml of isopropanol, 2 to 4 drops of thorin indicator, and
titrate  to a pink endpoint using 0.0100 N barium perchlorate.  Repeat
the titration with a second aliquot of sample and average the titration
values.   Replicate titrations must agree within 1 percent or 0.2 ml,
whichever is greater.
     4.3.3  Blanks.  Prepare  blanks by adding 2 to 4 drops of thorin
 indicator to 100 ml of 80 percent isopropanol.  Titrate the blanks in
the same manner as the samples.
 5.  Calibration
     5.1  Calibrate equipment using the procedures specified in the
 following sections of Method  5:  Section 5.3 (metering system); Section 5.5
 (temperature gauges); Section 5.7 (barometer).  Note that the recommended
 leak-check of  the metering system, described in Section 5.6 of Method 5,
 also applies to this method.
     5.2  Standardize the barium perchlorate solution with 25 ml of
 standard sulfuric acid, to which 100 ml of 100 percent isopropanol has
 been added.
                                   1-14

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6.  Calculations
     Note:  Carry out calculations retaining at least one extra
decimal figure beyond that of the acquired data.  Round off figures
after final calculation.
     6.1  Nomenclature.
                                               2    2
     A      = Cross-sectional area of nozzle, m  (ft ).
     B      = Water vapor in the gas stream, proportion by volume.
      W5
     Cu en  = Sulfuric acid (including SO,) concentration, g/dscm
      M^iU^                              J
              (Ib/dscf).
     CSQ    = Sulfur dioxide concentration, g/dscm (Ib/dscf).
     I      = Percent of isokinetic sampling.
     N      = Normality of barium perchlorate titrant, g equivalents/
              liter.
     Pfaar   = Barometric pressure at the sampling site, mm Hg (in.  Hg).
     P      = Absolute stack gas pressure, mm Hg (in. Hg).
     P   .   = Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
     T      = Average absolute dry gas meter temperature (see
              Figure 8-2), °K  (PR).
     T      = Average absolute stack gas temperature (see Figure 8-2),
               °
                K
     T td   = Standard  absolute  temperature, 293°K (528°R).
     V      = Volume  of sample aliquot  titrated, 100 ml for H2S
         /
              and  10  ml  for  SO^.
     V,     = Total volume of liquid  collected  in impingers and
              silica  gel , ml .
                            1-15

-------
      V      = Volume of gas sample as measured by .dry gas meter,
              don (dcf).
      V  (5td)= Volume of gas sample measured by the dry gas meter
              corrected to standard conditions, dscm (dscf).
      v      = Average stack gas velocity, calculated by Method 2,
              Equation 2-9, using data obtained from Method 8,
              m/sec (ft/sec).
      V  i   - Total volume of solution in which the sulfuric acid
      soln
              or sulfur dioxide sample is contained, 250 ml or
              1000 ml, respectively.
      V.     = Volume of barium perch!orate titrant used for the
              sample, ml.
      V..    = Volume of barium perchlorate titrant used for the
              blank, ml.
     Y      = Dry gas meter calibration factor.
     AH     = Average pressure drop across orifice meter, mm (in.)
              H20.
     e      = Total  sampling time, min.
     13.6   = Specific gravity of mercury.
     60     = sec/min.
     100    = Conversion to percent.
     6.2  Average dry gas meter temperature and average orifice
pressure drop.   See data sheet (Figure 8-2).
     6.3  Dry Gas Volume.   Correct the sample volume measured  by
the dry gas meter to standard conditions (20°C and 760 mm Hg or
68°F and 29.92 in.  Hg) by using Equation 8-1.
                            1-16

-------
       . v
                      "bar * 'iTe'   .        "W - W13.6)
                                                      Equation 8-1
where :
     K.J = 0.3858 °K/mm Hg for metric units.
        = 17.64 °R/in. Hg for English units.
     Note:  If the leak rate observed during any mandatory leak-checks
exceeds the specified acceptable rate, the tester shall either correct
the value of V  in Equation 8-1 (as described in Section 6.3 of
              m
Method 5), or shall invalidate the test run.
     6.4  Volume of Water Vapor and Moisture Content.  Calculate the
volume of water vapor using Equation 5-2 of Method 5; the weight of
water collected in the impingers and silica gel can be directly
converted to milliliters (the specific gravity of water is 1 g/ml).
Calculate the moisture content of the stack gas, using Equation 5-3
of Method 5.  The "Note" in Section 6.5 of Method 5 also applies to
this method.  Note that if the effluent gas stream can be considered
dry, the volume of water vapor and moisture content need not be calcu-
lated.
     6.5  Sulfuric acid mist (including SCL) concentration.
                    N  (V. - Vtb)
        cn   =  K,      *    ID      a               Equation 8-2
       UOU.      f.  - n
       2  4                 Vm(std)
where:
     K2 = 0.04904 g/milliequivalent for metric units,
        = 1.081 x 10"4 Ib/meq for English units.
                             1-17

-------
     6.6  Sulfur dioxide concentration.
                                 'v
                   u (v  - V  )
                   w ^Vt   vtb;    Va
     Ccn   =  K~   	n	——'               Equation 8-3
      S02      3         Vm(std)
where:
         - 0.03203 g/meq for metric units.
         = 7.061 x 10"5 Ib/meq for English units.
     6.7  Isokinetic Variation.
     6.7.1  Calculation from raw data.
     ,  .      Ts  [K4V1c+ (VmV/Tm) (Pbar * AH/13.6)]
                       60 a vs Ps An
                                                      Equation 8-4
where:
     K. = 0.003464 mm Hg-m3/ml-°K for metric units.
        = 0.002676 in. Hg-ft3/ml-°R for English units.
     6.7.2  Calculation from intermediate valuas.
              Ts Vstd) Pstd
           T5td \ 6 An Ps 60
                                                      Equat1on 8'5
where:
     Kg = 4.320 for metric units.
        = 0.09450 for English units.

                            1-18

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     6.8  Acceptable Results.  If 90 percent <. I <. 110 percent,
the results are acceptable.  If the results are low in comparison
to the standards and I is beyond the acceptable range, the
Administrator may opt to accept the results.  Use Citation 4 in
the Bibliography of Method 5 to make judgments.  Otherwise, reject
the results and repeat the test.
7.  Bibliography
     1.  Atmospheric Emissions from Sulfuric Acid Manufacturing
Processes.  U. S. DHEW, PHS, Division of Air Pollution.  Public
Health Service Publication No. 999-AP-13.  Cincinnati, Ohio.  1965.
     2.  Corbett, P. F.  The Determination of S02 and SO., in Flue
Gases.  Journal of the Institute of Fuel.  24_:237-243.  1961.
     3.  Martin, Robert M.  Construction Details of Isokinetic
Source Sampling Equipment.  Environmental Protection Agency.  Research
Triangle Park, M. C.  Air Pollution Control Office Publication No.
APTD-0581.  April, 1971.
     4.  Patton, W. F. and J. A. Brink, Jr.  New Equipment and
Techniques for Sampling Chemical Process Gases.  Journal of Air
Pollution Control Association.  1_3:162.  1963.
     5.  Rom, J. J.  Maintenance, Calibration, and Operation of
Isokinetic Source-Sampling Equipment.  Office of Air Programs,
Environmental Protection Agency.  Research Triangle Park, N. C.
APTD-0576.  March, 1972.
     6.  Hamil, H. F. and D. E. Camann.  Collaborative Study of
Method for Determination of Sulfur Dioxide Emissions from Stationary
                                   1-19

-------
Sources (Fossil Fuel-Fired Steam Generators).  Environmental Protection
Agency.  Research Triangle Park, N. C.  EPA-650/4-74-024.  December,
1973.
     7.  Annual Book of ASTK Standards.  Part 31; Water, Atmospheric
Analysis,   pp. 40-42.  American Society for Testing and Materials.
Philadelphia, Pa.   1974.
                           1-20

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SLIDE 109-0

         METHOD — 8

Determination of Sulfuric Acid Mist
  and Sulfur Dioxide Emissions
     from Stationary Sources
                                                          NOTES
 SLIDE 109-1
                 PRINCIPLE
  A gas sample is extracted isokinetically  from the
 stack.
  Sulfuric  acid mist and sulfur dioxide are separated
 and measured using the barium-thorin titration method.
              APPLICABILITY

  This method is applicable for the determination of
 sulfuric acid mist emissions from stationary sources.
 SLIDE  109-2

        METHOD 8 SAMPLING TRAIN
          TEMPERATURE
            SENSOR
     PROBE
           PITOT TUBE

       TEMPERATURE SENSOR
THERMOMETER
    PROBE (r=l
REVERSE TYPE
 PITOT TUBE
      ORIFICE-INCLINED
       MANOMETER
                                       1-21

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 SLIDE  109-3                                         NOTES

               REAGENTS
  Isopropanol which contains peroxide impuri-
ties will cause erroneously high sulfuric acid mist
results.
  Test each lot of isopropanol and reject if
absorbance exceeds 0.1.
 SLIDE  109-4

              CALIBRATION
  All components are calibrated using procedures
outlined in Method 5.
 SLIDE  109-5

             ON SITE SAMPLING
 1. Preliminary measurement and set up.
 2. Collect stack  parameters for setting isokinetic
  sampling rate.
 3. Set up nomograph and select proper nozzle size.

                                    1-23

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SLIDE  109-6                                           NOTES

          MAXIMUM AH CALCULATION
MAX.MUM  AH
                                    M
 SLIDE  109-7

(cont.)          ON SITE SAMPLING
          4. Prepare and assemble sampling train.
          5. Leak-check sampling train.
          6. Run test.
          7. Conduct post test leak-check.
          8. Purge sampling train.
  SLIDE 109-8
             SAMPLE RECOVERY
 1. Weigh impingers to nearest 0.5  g  for moisture
   determination.
 2. Transfer  contents of first  impinger  to a 250 ml
   cylinder;  add filter and dilute to  mark with 80%
   isopropanol. Transfer to container No. 1.
 3. Transfer contents from second and third impingers
   to a 1000 ml graduated cylinder dilute to volume
   with distilled water. Tansfer to container No. 2.
                                        1-25

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 SLIDE 109-9                                              NQTES

                  ANALYSIS
1. Confirm that no leakage occured during transport
  of samples.
2. Shake container No. 1 and allow filter fragments to
  settle.
3. Pipette a 100 ml aliquot into a 250 ml flask.
4. Add thorin indicator and titrate to a pink end point.
5. Repeat titration. Replicate titrant volumes should
  be within 1% or 0.2 ml.
 SLIDE  109-10

(cont.)                ANALYSIS
     6. Thoroughly mix solution in container No. 2.
     7. Pipette a 10 ml aliquot into a 250 ml flask.
     8. Add 40 ml of isopropanol and two to four drops of
       thorin indicator.
     9. Titrate to a pink end point.
    10. Repeat titration. Replicate titrant volumes should
       be within 1% or 0.2 ml.
    11. Prepare and titrate blanks in the same manner as
       samples.
                                          1-27

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                  SECTION J.  HIGHLIGHTS OF EPA METHODS 1-5

This section is under development and will be included in the manual  as  soon
as it is available.
                                     J-l

-------
                      SECTION K.  SUMMARY OF EQUATIONS

Subject                                                               Page

1.  Source sampling calculations (taken from the APTI Course 450
    manual)                                                           K-3

2.  Slides                                                            K-19
                                     K-l

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         Source Sampling  Calculations
This section presents the equations used for source sampling calculations. These
equations are divided into two parts —equipment calibration, and source test
calculations.  Gaseous source test equations are included to aid the source sampler
performing both paniculate and gaseous emissions tests. The purpose of the section
is to give the reader a quick reference to necessary mathematical expressions used
in source testing experiments.
EQUIPMENT CALIBRATION EQUATIONS
Stausscheibe (Type S) Pitot Tube Calibration
Calibration Coefficient (Cp)
Deviation from Average Cp (Leg A or B of Type S tube)
(Eq. 6-2)                  Deviation = Cp^st(^ - Cp

Average deviation from the mean b (Leg A or B)

(Eq. 6-3)                  t  J,  '     ~
Sampling Probe Calibration Developed by Experiment and Graphed  for Each
Probe Length
Test Meter Calibration Using Spirometer
Spirometer volume (temperature and pressure correction not necessary for ambient
conditions)
(Eq. 6-4)   [Spirometer displacement (cm)] x [liters/cm] = liters volume

Convert liters to cubic feet (ft 3)

Test Meter Correction Factor
             Spirometer Standard ft ^
(Eq. 6-5)    —	= Test meter correction factor
                 Test meter ft 3
                                    K-3

-------
                                      1l?m
                                      I/  T^
Correct Volume



(Eq. 6-6)      [Test meter volume] X [Test meter correction factor] —  correct volume



Orifice Meter Calibration Using Test Meter


Test meter volumetric flowrate (Qjn) in cubic feet per minute


(Eq. 6-7)    Qm ~ [Test meter (Vf)— Test Meter Vj] X [Test meter correction factor]





Proportionality Factor (Km)





(Eq. 6-8)                   Km~-





Orifice meter A//@ Flow Rate

                                                0  9244
(Eq. 6-9)               1.  English units AH@ =     ^




where             AH@ = 0.75 cfm at 68°F and 29.92 in. Hg


                                               0.3306
(Eq. 6-9)               2-  Metric units AH@ =	—




where           AH@ = 0.021  m3/min at 760 mm Hg and 20°C




Sampling Meter Console Calibration


Ratio of the accuracy of Console Gas Meter Calibration Test Meter (7).

Tolerance 1± 0.02



(Eq. 6-10)                  7 =
                                Vm Tt
                                       \     13. 6/


Meter Console Orifice Meter Calibration (AH@)
                                         m
                                               V
                                                T
where                      K = 0 . 03 1 7 English units

                             = 0.0012 metric units


                                              0 9244
(Eq. 6-12)               2.
                             K-4

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Source Sampling Nomograph Calibration

Isokinetic AH Equation
     isokinetic
6-13)
                      846.72 D< Af/@ C/
                                                           pm
Sampling Nozzle Equation
                      °-0358
Adjusted C-Factor (Cp)
(Eq. 6-15)             C'factor adjusted^ Cfactor   Q

Adjusted C-Factor
                                         l-B7/,,+ 18B7,,,/29
(Eq. 6-15)       C-factor adjusted ~ C factor Y^T]
SOURCE SAMPLING CALCULATIONS
Method 1 — Site Selection

Equal Area Equation (circular ducts)
(Eq.6-16)                    =

Equivalent Diameter for a Rectangular Duct

                           D     2(length) (width)
(Eq. 6-17)                   E     length
Method 2—Gas Velocity and Volumetric Flow Rate
Average Stack Gas Velocity
(Eq. 6-18)         Vs^KfiC* \^—^~ V"P  ave
Average Dry Stack Gas Volumetric Flow Rate at Standard Conditions
                                                [T
                                                1T~
                                                Pstd,
                                   K-5

-------
 Method 3— Orsat Analysis

 Stack Gas Dry Molecular Weight

 (Eq. 6-20)   Md = LMXBX = QA4(%CO2) + 0.32(%02) + Q.2S(%N2 + %CO)

 Stack Gas Wet Molecular Weight

 (Eq. 6-21)                  Ms = Md(l - Bws) + 1 8 Bws

 Percent Excess Air (%EA)
     6-22)           %EA= - —  - — - — - - xlOO
    . o-^>                   Q 264 (%N^ _ (%()2) + Q5(%co)


Method 4 — Reference Moisture Content of a Stack Gas

Volume Water Vapor Condensed at Standard Conditions (Vwc)


(Eq. 6-23)         Vwc = <" "f «° R T»*  = K, (Vf- Vd
where               Kj = 0.001333 m3/ml for metric units
                       = 0.04707 ft.3/ml for English units

Silica Gel
(Eq. 6-24)                  K2 = (wf~ wi) = Vw
   •                                          SG

where               #2 = 0.001335 m3/gmfor metric units
                       = 0.04715 ft.3 /gm for English units


Gas Volume at Standard Conditions
                                            m(std)
Moisture Content

                                  V   + I
(Eq. 6-26)               ^5= y——y	
                                       SG


Method 5—Particulate Emissions Testing


Dry Gas Volume Metered at Standard Conditions


Leak Rate Adjustment

                                   N
(Eq. 6-27)      Vm =[Vm - (L2 - LJO- E   (L,— L^ty- (Lp
                                   i=2

                                    K-6

-------
Standard Dry Volume at Sampling Meter


(Eq. 6-28)           V


Isokinetic Variation

Raw Data


(Eq' 6"29>       %/=                 60 6S VsPsAn

where                      K3 = 0.003454 mm Hg
                                           ml °K


                             = 0.002669-'"
                                          ml °R
                                   \
 Note: This equation includes a correction for the pressure differential across the
 dry gas meter measured by the orifice meter— average sampling run A// readings.

 Intermediate Data
    . 6-30)        %/- 100 -              - =  K4
                                        PS
 where                     K4 = 4.320 for metric units
                              0.09450 for English units


 Method 8 —Sulfuric Acid Mist and Sulfur Dioxide Emissions Testing

 Dry volume metered at standard conditions (see equations in previous sections of
 this outline)

 Sulfur Dioxide concentration
                                                /.,        \
                                                 solution'
  ,„    .                            N(Vt-Vtb)\Vali   ot
  (Eq. 6-31)                                    N        ;
                                           Vm(std)
  where                K} = 0.03203 g/meq for metric units
                          = 7.061 xlO~5 Ib/meq for English units
  i*  c«ov
  (Eq.6-32)
                Sulfuric acid mist (including sulfur trioxide) concentration
                                           Vm(std)
                                           K-7

-------
where


Isokinetic Variation
Raw Data

(Eq. 6-33)

where
                       =0.04904 g/meq for metric units
                       = 1.08X10-4 Ib/meqfor English units
                 %/=100
                                       6Q0AnvsPs
                       = 0.003464 mm Hg-m^/ml- °K
                       = 0.002676 in.Hg-ft^/ml- °R
                                        12
Concentration Correction Equations
Concentration Correction to 12% CO%

(Eq.6-34)                   ^"
Concentration Correction to 50% Excess Air Concentration
/17   ft ,„

-------
Fw Factor
  • When measuring cs and O2 on a wet basis
  * &wa ~ moisture content of ambient air
  • Cannot be used after a wet scrubber
                                          [20 9         1
                                  	:	
                                  20.9(1 -B1oa)-%0Zw\
F0 Factor
  1. Miscellaneous factor for checking Orsatdata

                             20.9  Fd    20.B-O9d    \°'
(Eq. 6-41)               F0=	=	    I     on dry basis     )
Opacity Equations
% Opacity
(Eq. 6-42)             % Opacity =IQQ- % Transmittance

Optical Density

(Eq. 6-43)           Optical Density = logiQ  \——     .   1
                                           L    Opacity J

(Eq. 6-44)           Optical Density = log\n   	
                      ^                    \Transmittance]
Transmittance
 (Eq. 6-45)                  Transmittance = e~na
-------
          Nomenclature

An       —  sampling nozzle cross-sectional area
As        —  stack cross-sectional area
a         —  mean particle-projected area
Bwm      —  percent moisture present in gas at meter
^ws       ~~  percent moisture present in stack gas
Cp       —  pitot tube calibration coefficient
Cp(std)   —  standard pilot-static tube calibration coefficient
cs        —  paniculate concentration in stack gas mass/volume
cws       ~  paniculate concentration on a wet basis mass/wet
             volume
Csi9       ~~  paniculate concentration corrected to 12% CC>2
°S50       ~~  Particulate concentration corrected to 50% excess
             air
D£       —  equivalent diameter
Djj       —  hydraulic diameter
Dn       —  source sampling nozzle diameter
E        —  emission rate mass/heat Btu input
e         —  base of natural logarithms (lnlO = 2.302585)
%EA     —  percent excess air
Fc        —  F-factor using cs and  CO2 on wet or dry basis
Fd       —  F-factor using cs and  O2 on a dry basis
Fw       —  F-factor using cws and O2 on a wet basis
Fo       —  miscellaneous F-factor for checking orsat data
          —  pressure drop across orifice meter for 0.75 CFM
             flow irate at standard  conditions
AH       —  pressure drop across orifice meter
j         —  equal area centroid
Kp       —  pitot tube equation dimensional constant
                                            ri»7j» molr (mini IK)
                                            •
                                            h
                English Uniis=85.49 it./sec.
                              K-10

-------
   L         —   length of duct cross-section at sampling site
   f         —   path length
   LI        —   plume exit diameter
   1-2        —   stack diameter
   m        —  -mass
   M^       —   dry stack gas molecular weight
   Ms       —   wet stack gas molecular weight
   n         —   number of particles
   NRC      —   Reynolds number
   Q\       —   plume opacity at exit
                 in stack plume opacity
                 atmospheric pressure
   Po       —   barometric pressure (Po= ^atm)
   Pm       —   absolute pressure at the meter
   pmr      —   Pollutant mass rate
   Ps        —   absolute pressure in the stack
   Pst(j      —   standard absolute pressure
                    Metric Units = 760 mm  Hg
                    English Units =29.92 in. Hg
   Ap       —   gas velocity pressure
                 standard velocity pressure read by the standard
                 pitot tube
                 gas  velocity pressure read  by the type "S" pitot
                  tube
                 particle extinction  coefficient
                 stack gas volumetric flow  rate corrected to
                 standard conditions
                                           (in.  Hg)(ft.3)
    R         —   Gas law constant, 21.83
                                          (lb-mole)(°R)
    t          —   temperature (°Fahrenheit or °Celsius)
    Tm       —   absolute temperature at the meter
                    Metric Units = °C + 273 = °K
                    English Units = °F + 460= °R
    Ts        ~   absolute temperature of stack gas
    Tst(j          standard absolute tcmju'iniurc
                    Metric Units = °2()°C -I- 273 = 293°K
                    English Units = 68°F + 460 = 528°R
    Vm       —   volume metered at actual conditions
    ^m t(\    ~   volume metered corrected to standard conditions
    v.p.       —   water vapor pressure
    vs         —   stack gas velocity
Volume H£O  — Metric units = 0.00134 m3/ml X ml
                English units =0.0472 ft.Vmlxml
    W        —   width of the duct cross-section at the sampling site
    d         —   time in minutes
                                  K-ll

-------
Company_
Test Team
Test Date
Observer
 SOURCE  SAMPLING  CALCULATION SHEET
	 Address 	
                      Address
(1) WATER VAPOR VOLUME: (Vw_st(j)
      Vw.std - 0.047KV
          w-std
(2) DRY GAS VOLUME:
                      (vm)
                        m
          'm-std
                      Evaluation Date
                      Eva!uator
Run


Run


Run


Run


Run


Run


                                                 scf
                                                                           ml








Run




Vn
\
Pt
A^
i

Run




i
i
>ar
{
r

Run


Run




















scf,
Run









dry
Run












cf
°R
"Hg.
"H20





                                  K-12

-------
(3) MOISTURE CONTENT:  (B )
B  =
                 
           
                                x 100
                                   'w-std
                                   'm-std
Run



Run


-
Run



scf
scf

B =
w
Run



Run



Run



(4)  GAS ANALYSIS:
                                      cc
                                            Run
                                                Run
Run


%C02 x 0.44 =
%02 x 0.32 =
%CO x 0.28 =
%N2 x 0.28 =
Md =
Run






Run






Run






                                                #/#-mole,  dry
(5)  GAS MOLECULAR WEIGHT:  (Mg)
                     B         B
s " v dM
" 100' IOMOO;
Run


Run


Run


                                                 #/#-mole, wet
                                     K-13

-------
 (6) ABSOLUTE STACK PRESSURE (P$)
            ,    .   stat
            bar   13.6
(7) STACK VELOCITY:  (V,.)
Run


Run


Run


                                                                     "Hg.
       s-avg
      s-avg

Run


titTo) |/_
* p'avgf Tf
Vavq

CP
(VEjTjavg =
s-avg
Ps
Hs

Run





Run








Run


Run






Run






fps
°R
"Hg.
#/#-mole
                                  K-14

-------
(8) ISOKINETIC VARIATION:  (I)
           1.667(T..     )[0.00267(V
      I  =
Vs-a,gs
S avQ.
>

'e> I = (9) PARTICULATE CONCENTRATION: (c) Run T — s-avg ~ £ ~ vs-avg Ps 0 A n Y Run = Run Run Run Run % °R ml cf fps "Hg. min. sq. ft A B R M = n V = m-std = A / B = Run Run Run mg. scf c = 35,310(R) = 0.0154(R) -6, = 2.205 x 10 (R) = Run Run Run micrograms/cubic meter, normal grains/std. cubic foot pounds/std. cubic foot K-15


-------
(10) VOLUMETRIC  FLOW  RATE  (Actual ):(Q)
       For circular ducts
       For  rectangular ducts
       Q =  (D(W)(Vs_avg)  x 60







Run




V
s-avg
Ds =
L
W

Run


Run






Run


Run








acfm
Run











fps
ft.
ft.
ft.




(11)  VOLUMETRIC FLOW RATE (Standard Conditions): (Qstd)
                        B
              17.65(1  -   -
       *std
                       s-avg







Run









Run




B
w
Q
Ps -
s-avg

Run











«
Run








;cfm, dry
Run









Run











%
acfm
"Hg.
°R




                                  K-16

-------
(12)  POLLUTANT  MASS RATE:  PMR



       PMRc  = 1.323 x  10"4(R)(Qstd)
Run



Run



Run



                                                                           scfm
           PMR  =
Run


Run


Run


                       Ibs/hr
                  For circular ducts
                  PMRa =
                     a
1.323 x 10~4(Mn)


        e
                  For rectangular ducts



                         1.323 x 10"4(Mn)(L)(W)


                      =          6   A
                                      n
        PMR.  =










Run












Run




M =
n
9 =
Ds =
D =
n
L =
W =
A =
n

Run


F












tun











Ibs/hr
Run












Run














mg.
nrin.
ft.
ft.
ft.
ft.
sq. ft




                                     K-17

-------
(13) ISOKINETIC CHECK:
         I  =  PMRa/PMR  x 100 =
                a    C
Run 	

Run 	

Run 	

(14) "F"  FACTOR CALCULATION



         E  =  2.205  x  10'6(R)(F)(L;20-9
R =
F =
V
Run 	



Run 	



Run 	



                       E  =
lun 	

Run 	

Run 	

Ib/MM Btu
                                   K-18

-------
SLIDE 151-0                                      NOTES


 SUMMARY OF EQUATIONS

EPA REFERENCE METHODS 1-5
SLIDE 151-1



 ABSOLUTE STACK PRESSURE (PJ
        P__
        -
                      stat
 SLIDE 151-2



             STACK VELOCITY (V.)
 V    — RR
 Vs.avg - 8b.
                               K-19

-------
SLIDE 151-3                                     NOTES

        DRY MOLECULAR WEIGHT (MJ
Md = 0.44 (% CO2) + 0.32 (% O2)
  d     .         2     .        2
        0.28 (% N2 + % CO)
SLIDE 151-4

   MOLECULAR WEIGHT OF STACK GAS (MJ
 Ms = Md (1  - Bws) + 18 (Bws)
 SLIDE 151-5
          PERCENT EXCESS AIR (EA)
              %EA =
          % O, - 0.5% CO        1
          N2 - (% 02 -  0.5% CO) J
  0.264% m2

                              K-21

-------
SLIDE 151-6

 VOLUME OF WATER VAPOR CONDENSED (V^^J
                                             NOTES
    w«std>
       (V,-VjlPwRT^
            P^M.
                 std twlw
           K, (V, - Vc)
 SLIDE 151-7

     MOISTURE CONTENT
  B
                V
           *wc(std) ~r ^m(std)
  SLIDE 151-8

           SAMPLE GAS VOLUME (Vmstd)
   V m O+H     V i
mstd
               m
                       PK« +
                         bar
                                    .AH
                                     13.6
            K1VmY
                             1 std

                  Phar + (AH/13.6)
                                m
                               K-23

-------
SLIDE 151-9
                                           NOTES
    LEAK RATE CORRECTION
         CASE NO. 1
 Vm-   [(Lp-La)6]
SLIDE 151-10
            LEAK RATE CORRECTION
                 CASE NO. 2
 Vm - (L, - LJ6, - 2 (L, - La)62 - (Lp - La)0
 SLIDE 151-11

   STACK GAS FLOW RATE (Q5)
  0,  - As x Vs x 60
                            K-25

-------
STTDE 151-12                                  NOTES

 STACK GAS FLOW RATE AT STANDARD CONDITIONS (Q.,fcU1))
                    _Ps_ Jstd f 1 _ g  )
                    3     T  *     "•'ws'
                     std    ' s
SLIDE  151-13
              ISOKINETIC VARIATION (I)
                 FROM RAW DATA
   _ f, [K3 V,c +  (VJTJ (Pbar + AH/13.6)]
                 606VSPSAN
 SLIDE 151-14
            ISOKINETIC VARIATION (I)
          FROM INTERMEDIATE VALUES
               TV      P
 T  _           ' s v m(std) ' std
        Tstd Vs 0 An Ps 60 (1-Bws)
                             K-27

-------
SLIDE 151-15                              NOTES

       PARTICULATE CONCENTRATION^,)
              GRAINS PER SCF
          C. = 0.154  M"
C. = 2.2x10 6
       V
 Ibs per hour

   Mn
Vm(std)
 SLIDE 151-16

 ACETONE BLANK CONCENTRATION (CJ
         Ca~V_P
                 a   a
 SLIDE 151-17

 ACETONE WASH BANK (WA)
  wa = c, v_ P
           a  w aw " a
                          K-29

-------
                   SECTION L.  MISALIGNMENT OF PITOT TUBE
Subject                                                               Page
1.  Pitot tube errors due to misalignment and nonstreamlined flow     L-3
2.  Slides                                                            L_7
                                      L-l

-------
                         Phot  Tube  Errors Due to  Misalignment

                                  and Nonstreamlined flow   *

                                D. JAMES GROVE and WALTER S. SMITH

   Although the pitot tube is the tool most commonly used for measuring velocities in stacks and ducts, it is also the
tool most commonly misused. In order to use the tube properly, the stack sampler  must first gain a better under-
standing of ihe errors which occur when it is misused. This paper will be limited to a discussion of the errors caused by
misaiignment of the pitot tube with  respect to the flowing gases, and errors caused by the non-streamlined flow of the
gases. Although the errors discussed here  are common to all pitot tubes, data will be presented only for "S" type pitot
tubes, since they are  the type most commonly used. The  two basic types of pitot tube misalignment are shown in
Figure 1. From.experimental data taken in a 12" diameter demonstration duct, with velocities on the order of 20 feet
per second, the magituda of the error in the velocity measurement is given in Figures 2 and 3. The error is plotted as a
                    CASE A
CASEB
                                  Flgur» 1. Typw of pitot tub* miMl!gnnwnt.
function of the angle (0 or 0) of misalignment, and it is the error in the velocity, not the velocity pressure lAp). To get
the approximate error in the Ap. the errors from the graph would have to be multiplied by two.
   From Figure 2 we can draw several conclusions. Contrary to popular opinion, the alignment which gives the highest
reading docs not indicate the direction of flow. The direction of flow  is indicated by the inflection point, or by a 90°
rotation from the alignment which yields a zero velocity pressure. Also important is that misalignment of up to 50° will
result in only a 5% error in velocity.
   Figure 3 offers one immediate conclusion, that the error is not symmetrical on either side of the correct alignment.
When the pitot tube is  pointed into the flow, the velocities measured are generally too high, and when the pitot tube.is
pointed away from  the flow, the velocities measured are too low. These errors are also of a much larger magnitude than
those encountered from case A.
   If a  pitot tube is aligned so that neither $ nor $ are zero (case A and B simultaneously), the resulting errors would be
approximately the sum  of tha two individual errors.

*   Taken  from   Stack  Sampling  News,  Vol.   1,  Number  5.  Nov.  1973.
                                               L-3

-------

3
-













•
,d<
30












H
/
'
jgr







/
/
5

1



ee
-(


H
I
1
',








5
30

/
I
J











/
P













\
'-














V
40













fi>















_f















£>—

>0






























\j














+6
7
J

-6

-1

-1

-2

-J

-3

/TV
>--

>0










srr















or



>
+4














a
0s-















K
^














*<

\
I
~\











iO


«l
I
\
\
.















\
\
I

I

•


*£












1


10













                  fiffurt 2. Vilocity trrort from ettt A Miulignmcnt.
  I   I
                                     +12
—r  $,degrees
                            +6  •:
 -80 t
-60
-40
-20
+20
+60
+80
                                z
                                     -6
                                     -12
                      &
     I
                              r
                             •18
                             -I'
                                     -30
                                                            T
                                     -36  %  error  -
                         Vttodty trrort from cue B
                                    L-4

-------
   Now that the errors due to misalignment are apparent, velocity measurements in non-streamlined flow should be
considered. Tho primary use of the pitot tube by the stack sampler is measuring the velocity at several points on the
(tack cross-section which represent the average face velocity of the pases. The normal procedure is to divide the suck
cross-section into equal areas, and make velocity measurements at the centroid of each of these areas.  In order to obiain
an average face velocity, the sampler sums the velocities at each point and divides by the number of points (equal
areas).  Note that in this  procedure, the sampler assumes that the gases are flowing perpendicular to each of these equal
areas. If this is not the case, the sampler should determine the upward (parallel to the stack walls) vector of the velocity
at each area.
   .t should be considered what errors result when the pitot tube is placed properly with respect to the stack, but the
gases are traveling at an angle to the stack wall (an an angle 4> or & with respect to the pitot tube). The curves in Figures
2 and 3 show that when the pitot tube is not aligned properly with the flow, the velocity reading is neither the velocity
vector  in the direction  of  flow, nor the velocity vector perpendicular  to  the tube. The curves do give us the error
between  the velocity readings and the velocity vector in the direction of flow for a given value of 0 or S. Also the
velocity vector parallel  to  the stack  walls will be  cos  i or cos 8 times the  velocity vector in the direction of flow.
Consequently, the error between the velocity readings and the velocity vector parallel to the stack walls will be a
combination of error in  Figures 2 or 3 and the cosine of the angle between the flow and the pitot tube.  This combined
error is shown in Figure 4 for case A and Figure 5 for case B. Keep in mind that these are errors in the velocity, not the
Ap.
   The most important conclusion to draw  from these curves (Figures 4  and 5)  is that if the pitot  tube is aligned
properly with respect to the stack, regardless  of the direction of flow, the resultant velocity readings will be either close
to correct or too high. There will never be a large error on the low side.
                                 Figun 4. Velocity eiron from cut A flow misalignment.

   There are two predominant cases of non-streamlined flow which occur in stacks and ducts that should be discussed
 in more detail. The first of these, which is by far the most common case, is after a bend or an elbow in the duct. Tho
 resulting flow is shown in Figure 6.
   In attempting to measure  the  upward vector of the velocity, the error (with the  pitot tube properly aligned with
 ritpect to the  stack) will depend on  which of the three ports shown (X, Y, and 2) are used. Port Y will give errors
                                                      L-5

-------
 corresponding to Figure 4. Port X will givo errors corresponding to trie left half of Figure 5, while Port Z corresponds to
 the right half of  Figure 5. Ron X is the only port which gives velocity reading} >t all clow to the upward velocity
 vector, regardless of the angle.

























\












\

-60






m
































3^
-60















































-40
^©-f —





















-(•^






























-20
.^Wi


-0

















— -
















X
^*~*


+150






- % error -
+100



+5



-










^


- -25









^









7
^+20

















d
k®





1









/
/














,-
/
1
X
T
/


I/
2
2
1



+40













41




















+60.











































+80
, degrees ^




•i^^—

                                Flgurt & Velocity •iron from CM* B flow mitalignmcnt.

   The second important case of non-streamlined flow is called tangential or cyclonic flow, which normally occurs after
a cyclone or a cyclonic scrubber. The resulting flow is shown in Figure 7. There are only two velocity vectors, axially
and tangentiaily (move radially), so that regardless of which port is used (X1, Y'. or Z'), the error always corresponds to
that in Figure 4. The larger the tangential vector, the larger the error.
                                      6
)  O  (z
                                                          X1
           fiyurt 6. Flow «f t»f a tend or *n elbow.
                                 flgun 7. TengentUI or cyclonic flow.
                                                        1-6

-------
SLIDE 152-0

 PITOT TUBE
MISALIGNMENT
NOTES
 SLIDE 152-1
                              1-7

-------
SLIDE 152-2
NOTES
SLIDE  152-3
                                L-9

-------
SLIDE 152-4
                                             NOTES
SLIDE 152-5

          VELOCITY ERROR
                 VS
PITCH ANGLE FOR AN S-TYPE PITOT TUBE
 6.1 m/sec
 , degrees
 J	I
                               L-ll

-------
SLIDE 152-6
FLOW AFTER BEND OR ELBOW
NOTES
                Y
              xt> o dz
 SLIDE 152-7


TANGENTIAL OR CYCLONIC FLOW
          Y1
   TOP
   VIEW
                               L-13

-------
  SLIDE 152-8
                               NOTES
   VELOCITY ERRORS FROM TYPE A
        FLOW MISALIGNMENT
               + 150 -
               + 100
                + 50
% VELOCITY
 ERROR
-80
     -60
         -40  -20
                      + 20
                          + 40  +60  +80
   SLIDE 152-9

     VELOCITY ERRORS FROM TYPE B
          FLOW MISALIGNMENT
                  + 150
                  + 100
                  + 50
           -40  -20
            J	L
 _ % VELOCITY
    ERROR
  -80   -60
  
-------
   SECTION M.  ISOKINETIC SAMPLING AND BIASES FROM NONISOKINETIC  SAMPLING



Subject                                                               Page



1.  A method of interpreting stack sampling data                      M-3



2.  Slides                                                            M-13
                                     M-l

-------
                      A Method of Interpreting Suck Sampling Data*

                                  W. S. Smith, ft. T. Shigehara. andW. F. Todd

                                                Engineering Section
                                         Institute for Air Pollution Training
                                         Office of Manpower Development
                                     National Air Pollution Control Administration
                                              Public Health Service
                                           Environmental Health Service
                                  U.S. Department of Health. Education and Welfare


                                               INTRODUCTION
    In order to obtain an average pollutant concentration (cj, two basic quantities are required: (1) total quantity of
pollutant (pmit) emitted  from the stack  per time period (0t), and (2)  total quantity or volume of effluent gas (V,t)
emitted from the stack for the same time period (6t). In equation form:




    The objective  of the stack sampler is to obtain these two basic quantities, pmit and Vit. Since they generally cannot
be measured in their entirety, multiple measurements are made in  order to estimate them. The general approach is to
divide the stack cross section into a number of equal areas (N.) and to traverse the cross section by sampling at the
midpoint or centroid  of  each equal area for equal lengths of  time (0,). The sample is extracted at a regulated  rate,
isokinetically for particulates, and proportionally for gaseous pollutants.
    The sampler's  first assumption is that the sample extracted at the midpoint of the elemental area (Ae) is representative
of that area; i.e., the concentration entering the sampling nozzle (cn) is equal to the average concentration of the elemental
area (cc). The second assumption is that the average concentration (cn) obtained from the sampling train, upon traversing,
is equal  to the average stack concentration (c,)  as defined by Equation 1. It has been pointed out that the correctness of
the above assumptions is dependent on  the time and cross-sectional variation of the pollutant concentration [1]. Whether
or not the proper  sampling approach was used in obtaining a representative sample concentration of the source, however,
an evaluation  of the stack sampling data can still be made to determine if proper sampling techniques were employed, i.e.,
isokinetic sampling rates for particulates and proportional rates for gases.
    Hemeon and Haines [2] in 1954 pointed out two methods of calculating dust concentrations, and Badzioch [3, 4]
expounded upon them in 1958 and 1960. For the purpose of this paper, these methods will be referred to as:  (1) the
ratio-of-area and (2) the sample-concentration calculation methods. Both utilize  the inertial properties of the particles. In
essence,  the above authors have said that, when anisokinetic conditions exist, the ratio-of-area calculation method gives
better accuracy for very large or coarse particles, and  the sample-concentration calculation method gives better accuracy
for gases or fume-like (very small) particles. The decision of which method to use is based on prior knowledge of the
particle size distribution.
    The purpose of this paper is to show how the two methods can be used to interpret stack sampling data.

                                           GENERAL PRINCIPLES

                         THEORY OF SAMPLING  PROCEDURE AND CALCULATIONS

    Consider a particulate sampling train with a nozzle of size An extracting a sample from an elemental area (Ae) for a
time period '(0J. whore 00 is the total  sampling time  (dt) divided by the total number of elemental or equal areas (Ne).
When isokinetic conditions exist,  i.e., the stack velocity  at the centroid of the elemental area (v,e) is equal to the nozzle
velocity  (vns), the sampling train automatically integrates the instantaneous pollutant mass emission rate into the probe
nozzle (pmrn.) ovor the time period (0,}. Mathematically:


  *   Taken  from  Stack Sampling  News, Vol.  1,  No.  2, August 1973.


                                                 M-3

-------
mn. = I Pmrn.d0. = / Anvn.cn.d0.
      0,            0t
                                                                                                          (2)
where mna is the pollutant mass collected by the sampling train during 'Jme 09.
    A sample traverse sums the individual mn.'s for all the elemental areas or:
                                                                                                          (3)
where mnt  is the pollutant mass collected by the sampling train during the total sampling time (0t). Hereafter, for
simplicity, the summation sign (S) will denote the summation from e=1 to e=N,.
    The pollutant mass (mnt) is one of the actual data that the sampler receives. This datum (mnt) is used to estimate the
average pollutant mass emission rate (pmr,) from the stack. This can be accomplished in the following manner.
    Dividing Equation 2 through by An yields:
 For isokinetic conditions (vn.  = VM), using the assumption that the sample concentration is representative of the
 elemental area concentration <€„. ** c,.), it follows that the pollutant mass from the elemental area (mM/A.) ;s-
                                   7=- -
                                                                                                          (4)
                                                      A.
                                                     !A7'
     Dividing Equation 4 by 0. yields the average pollutant mass emission rate (pmrt.) from the elemental area (A.) :

                                            _    m«« A. mn.
                                            pmr.. =• ~~~" —~ -----                                           f 5\
                                                     ^  An  0.                                            tb)

The sample traverse yields the average pollutant mass rate from the entire stack:

                                  _   „       •   A-mn.    A.
                                 . pmr, - S pmrM =  S -—•—=-—- Lmnt                                (6)
                                                      An A.   Anfl.


Substituting Equation 3 and using 0, = 0t/N8 and A, = A,N.r Equation 6 can be rewritten as:

                                               _   mnt A,
                                                     8: -                                            (7)
                                                 M-4

-------
Equation 7 is the retio-of-orea method of calculation.

    The second method of estimating prnr, is to use the average sample concentration (cj and the average stack velocity
(v,). Notice how this is effected.
    The sample volume (Vn.) that the sampling train extracts during time (0.) from the elemental area (A.) is also an
integrated volume. Mathematically:
A cample traverse again yields the sum of the volumes defined by Equation 8.


                                        Vn, = SVn.-2/ AnVn.d0.                                     (9)
                                                         e«

By combining Equations 3 and 9, the average sample concentration can be calculated.
                                                       77-                                              (10)
                                                       vnt
It is then assumed that c~n ="c,.
    If velocity measurements  are taken simultaneously with the pollutant sample and it is assumed that the average stack
velocity (v() = \fr v"M/N,, "cn andV, can be used to determine prnF,:
                                                               _
                                                           — -v,A,                                     (11)
Equation 11 is the sample-concentration method of calculation.

    The same analogy can be applied to pollutant concentration instead of the pollutant mass emission rate of Equation 7
and Equation 11. yielding the following:

                          T»nt
                     "c, =* —                                  Sample-Concentration Method               ( 1 2)
                            m,
                             nt
                      *   0«v.Ar
                                                               Ratio-of-Area Method'                      (13)
 Equations 12 and 13 are the equations used by Hemeon and Haines, and by Badzioch. For the sake of brevity, the ensuing
 discussion will be limited to Equations 7 and 11.
    At this point. Equations  7 and 11 will  be  redefined and summarized to distinguish between the two methods as
 follows:

                                                	    mnt A.
                                                pmr  «=	
                                                        fit Afl                                            (7)

                                               	   Tint _
                                               pmre ™	v,A,                                          (11)
                                                      Vnt
                                                  M-5

-------
where:     pmr,       =       pollutant mass emission rate calculated on a
                              ratio-of-area basis
           pmre       =       pollutant mass emission rate calculated on a
                              sample concentration basis
           mnt       =       pollutant mass collected by the sampling train
                              in total sampling time (0t)
           A,         =       area of stack cross section
           An         =       area of sampling nozzle
           Vnt       —       actual metered sample gas volume corrected to
                              stack conditions
           7,         =       average measured stack gas velocity at stack
                              conditions
                               DETERMINATION OF AVERAGE SAMPLING RATE
     The ratio Vn/Vj is the ratio of isokinetic conditions on an average. By taking the ratio of pmr. to pmrc, and noting
                      pmr,                           vnt            vn
                      pnvc        ntav.A,        An0t7.         V,
                                   Vnt


     We see that pmr./pmra is also a measure of the degree of isokinetic conditions on an average. Summarizing in Table 1
 as follows:

                                     Tablt 1. Amngt Sampling Reta
                                        Ratio,               Ayarage
                                     pmr, / pmr0           Condition
                                          1              Isokinetic
                                         < 1              Undarisokinatic
                                         > 1              Overwokinatic
     Equation 14 says: (1) that only when isokinetic conditions exist will pmr, = pmre, (2) that in order to determine the
ratio pmr,/pmrc. it is necessary only to know Vntl 0t, An, and 7,, and (3) that the ratio prn7./pmrc is not a function of
the characteristic of the pollutant collector (an independent evaluation must be made on the efficiency of the collector).


                             DISCUSSION AND CATEGORIES OF SAMPLING RATES
     It must be understood what the possibilities of Table 1 mean. When pmr,/prnrc -=fe 1.  it  means that the results are
definitely questionable. When  pmr,/pmrc = 1, it means that isokinetic conditions were maintained on an average during
the sampling period, but does  not necessarily  mean that the results are valid. The integrated volumes can be obtained by
sampling at the average stack velocity (v,)  while traversing such that7n =7t. But because of variation of velocity over the
cross section, there are times when anisokinetic conditions will exist. The same situation could arise due to fluctuation of
velocity. Since
                                                M-6

-------
when vn =7S, it should be obvious that the criteria of Table 1 are valid only if Vnt and v. are obtained independently; i.e.
Vnt » not calculated using Equation 15. or vice versa.
    Use of Equation 15 is equivalent to the ratio-of-area method  of calculation as this would make pm?c = pmr.. Such
sampling trains using only a rate meter (orifice, rotameter. cyclone, etc.) or only a null-balance nozzle are not amenable to
the criteria of Table 1 as they are not subject to any cross-check at all. For example, errors could be introduced through:

             1.  Miscalculation in the sampling rate leading to an improper meter setting.
             2.  Careless meter of equipment adjustments.
             3.  Improper calibration of meters or of null-balance nozzles.
             4.  Misuse through pure  ignorance  of  the operating principles of the rate meters or null-
                 balance nozzles.

    In the above conditions, isokinetic rates can be claimed without dispute.

             An evaluator can only:
             1.  Rely on reputation of the sampler.
             2.  Critically examine the procedure.
             3.  Check the results using a material balance.
             4.  Rely on past data whose reliability may also be questionable.
   All this points to the fact that a volumetric device such as  a dry gas meter is a must in a sampling train if any
interpretation is to be made. An independent velocity reading (pitot tube), preferably simultaneous with sampling. Is also a
must

   With the understanding that the ratio pmra/pmrc be a function of the independent measurable quantities (Vnt,  0t.
An, and7,. the different sampling conditions can be categorized as shown in Table 2

                                   Table 2, Sampling Rate Cattgoriet
                                   Casol:  pnv,/pmre  m    1 or7n

                                   Casa 2:  pmra/pmrc  *    1
                          ERRORS IN PROPORTIONAL ANISOKINETIC CONDITIONS

    Before any guidelines can be established, it must be understood how anisokinetic conditions affect the results because
the practical situation says that Case 2 is the more .general situation. Going back to Equation 3, it can be seen that this case
(7n T£"V,) could affect the amount of pollutant collected.
                                                                                                            (3)


The general premise is that when vn = v,. then c,, = c.; but when vn ¥= vs. cn =£ c, except when sampling for gases and
small particles. Thus the amount of pollutant collected by the sampling train depends on vn/v. and the variation of c,. The
degree of deviation from the time value (c,) depends on the method of calculation and- the particle size distribution.
    Hemeon and Haines [2]  and Badzioch [3, 4] illustrated the effect under steady state conditions (c, = constant) of
particle sizes depending on the calculation methods when only large particles and only small particles were present Figures
                                                  M-7

-------
1 and 2 illustrate this. Figure 3 is a combination of Figures 1 and 2, and Table 3 summarizes the biases relative to the true
pmr, [5].
                              1.6
                              1.4
                              1.2
                              1.0
                              OJ
                              0.6
                              0.4
                                                                             p.we (SMALL)
                                                                         I
0.4
US
                                                    8.8         LO        1.2
                                                     RATIO OF ISOKINETIC,
1.4
                                   Figun 1. Error* due to anisokiiwtic conditions (•mall partidm).

                             Table 3. Constant Proportion*! Condition
                               Rttia
                            pmra/piTirc
      Condition
                                         Bias relative to
                                            true pmr,

                                      pcnra          ~~
                                              Itokinatic
                                              Underisokinetic
                                              Ov«r iso kinetic
     According  to Figure 1. when only small particles exist (including gaseous pollutants), the sample-concentration
method of calculation  gives accurate  results; according to  Figure 2, when only large particles exist, the ratio-of-area
calculation method gives the most accurate result under anisokinetic conditions. Figure 3 shows the maximum deviation
from the true value [as marked by pmr, (small)  and pmre (large)]  that could possibly occur if constant proportional
conditions are maintained.
     Unfortunately, the  two extremes, all large particles or all small particles, do not often occur. A mixture of large and
small particles is the more general case. The dotted line in Figure 3 shows the case where 50 percent by weight are small
and  50 percent are large particles. A mixture of different size particles, then, only tends to decrease or shrink the outer
                                                     M-8

-------
    L2
g   LO
                T—"I
     0.
      0.4
 O.S
                                            1.4
                   M        LO         L2
                     RATIO OF ISOKINETIC, »,/»$
Figun 2. Errors due to anisokiiwtic conditions (taroe particles).
      0.2
  Figun 3. errors
    ...     Q.S     1A>      1.2     1.4     1-6      **     «
 RELATIVE BOKINETIC CONDITIONS, WT, or pwa/pwe
due to anisokinetic conditions (60% small and 50% U»r8a particlw).
                                    M-9

-------
boundaries. It is impossible to exceed the outer boundaries if exact, constant, proportional conditions are maintained.
    Realizing this, it can be stated that the true pmr, value lies somewhere between pmr, and pmr6. it may be closer or
even equal to one or the other, depending on the particle size distribution. Without this knowledge, the best that can be
said is:
                                       xv   pmr, + pmrc   pmr, — pmre
                                      pmr. = - - - ±- - - -                                  (16)

      x*s.                          _
when pmr, is the estimate of the true pmr,.
    Under the practical situation, it is impossible to maintain isokinetic or proportional conditions without some degree
of fluctuation. We need to understand how this would affect the sampling results.
    Badzioch wrote an equation relating the pollutant mass collected to the actual pollutant mass in the stack as:
                                                         v,.

where a = parameter, depending on the inertia of the particle and the gas flow pattern at the sampling nozzle. Also, it was
reported that a was a constant for vn,/vM » 0.5 to 4. Watson [6] approximated the range as 0.5 to 2.
    Thus for a given particle size distribution, when c., • constant, then the average (a) is a constant, and:
which is a straight-line function. Further, if 7nt =» vj. or7n, * k 7M. the ratio of mn to m» remains fixed but is biased
depending on the value Vn/v(.

                                           PROPOSED PROCEDURE
                                          FACTS AND ASSUMPTIONS

    The bases may now be set for the interpretation procedure.
                1.  There is no knowledge of particle size distribution or how the pollutant  concen-
                    tration is varying with time.
                2.  The following data are provided:
                    a.   "v,, mn „ An, Vnt, and 0t. Vnt must be'obtained independently of "v
                    b.  Vne, 08, and",, for each elemental area.
                3.  Results within ± 10 percent of the true value are desired.
                4.  There is no deliberate attempt to bias the data.
                5.  Fluctuation within the stack of both  velocity and pollutant concentration at any
                    point are random..
                6.  Only  averages can be calculated.

                                       PROCEDURE AND EXPLANATION
    The following steps should ensure valid results within ±  10 percent of the true value. The limit, ± 10 percent, is purely
arbitrary; an understanding of this example should enable you to set your own desired limits.
    With the principles set forth, a method of evaluating source sampling data can now be proposed.
                                               M-10

-------
                 1.  Calculate pmr. and pmre. using independent measurements of Vnt and7..

                 2.  Calculate the ratio pmr./pmre and pmr«~P ± Q.10, reject the results.
                                                     pmr. + pmre
                                 	            •   pmr. — pmrc
                    b.   If 0.82 < pmr./pmre < 1.2 or	< ± 0.10. go to step 3.
                                                     pmr. *• pmrc

                 3.  Calculate—— .1^
                     Vn. is an integrated volume over the sampling period 0,. whereas V,. is a result of
                     the  readers estimation of the average reading of the  inclined manometer. The
                     inclined manometer of the pitot tube does not give V,. directly but,  instead,
                     yields the velocity pressure (Ap,.). This reading, the Ap,., must be within *  10
                     percent of the average value [7]. Therefore, if ApM varies more than this amount
                     during 0., the^rate must be adjusted, and the Ap,. and the time must be recorded
                     so an average v M can be calculated.


                     a.   If any 1.2 <	< 0.82, reject the data.
                                    V..An0.

                     b.   If all 0.82 <	< 1.20. average pmr. and prnF0.
                                    V.. An 0.

                     This value will be within ± 10 percent of the true pmr,.


                                                  SUMMARY

    There are two approaches used to calculate the pollutant mass rate:

                 1.   The ratio of area method  in which the sample collected is weighted according to
                     the ratio of the cross-sectional  areas of the stack and the sample nozzle.
                 2.   The concentration based  method in  which  the sample collected is weighted
                     according to  the ratio of the volumetric flows In the stack and in  the sample
                     nozzle.

    The source tester should be aware of how the two methods for calculating the pollutant mass rate can be biased by
the particle size distribution of the pollutant when isokinetic conditions are not maintained. Although it is shown that the
bias is predictable if either all  large particles or all  small particles are present, the real situation usually lies somewhere
between these predictable limits. A compromise between these two limits then is the best estimate of the true value when
exact knowledge of the particle size distribution is lacking. The procedure recommended is to obtain the average value of
the two methods, which is a model based upon the  concept of Hemeon and  Haines [2] and others  [3, 4, 6] and can be
applied to real sources.
    The two  methods for calculating pollutant mass rate do  not take into account time and cross-sectional variations of
the pollutant mass rate. However the ratio of the methods, pmr./pmrc. can be used to determine the average percent of
isokinetic  or  proportional conditions. With'additional real time data, e.g., velocity and sample volume reading, a more
detailed evaluation can be made. This shows the necessity of having a velocity measuring instrument during sampling and a
volume meter in the sampling train.
                                                    M-ll

-------
                                          REFERENCES
1.  W. C. Achinger, R. T. Shigehara. "A guide for selecting methods for different source conditions." J. APCA
    1S, 605-609 (September 1968).
2.  W. C. L. Hemeon, G,  F. Haines, Jr.,  'The magnitude of errors in stack dust sampling," Air Repair 4.
    159-164 (November 1954).    .           '
3.  S.  Badzioch, "Collection of gas-borne  dust particles by means of an aspirated sampling nozzle," British J.
    of Applied Physics 10. 26-32 (January 1959).
4.  S.  Bediioch, "Correction for anisokinetic sampling of gas-borne dust particles," J. tnst of fuel, 106-11C
    (March 1960).
5.  W. D. Snoxvden,  R. T. Shigehara, "Non-proportional sampling biases on concentration and pollutant mass
    r.-.te." Unpublished paper (1969).
6.  H. H. Watson. "Errors due to anisokinetic sampling of aerosols,"/4m. Ind. Hyg, Ass. Quart.  15-16,21-25
    * March 1954).
7.  R. T. Shigehara.  W. F. Todd, and W. S. Smith, "Significance of errors in stack sampling measurements,"
    Presented at APCA Annual Meeting, St Louis, Missouri (June 1970).
                                             M-12

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 SLIDE 153-0                                         NOTES

 ISOKINETC SAMPUNG AND BIAS
FROM NONISOKINETIC SAMPUNG
 SLIDE 153-1

   ISOKINETIG SAMPLING

 1. The velocity entering the nozzle
  must be the same as the velocity
  in the stack.

 2. The particles must be moving
   parallel to the stack wall and
   directly toward the nozzle.
 SLIDE 153-2

            EXAMPLE

 o — Large particles. These particles
     are greater than 100 microns and
     are not affected by flow pattern
     due to their inertia.

 o — Small particles. These particles
     are less than 0.3 microns and
     move along with the flow pattern
     since they have very little inertia.
                                      M-13

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SLIDE  153-3
           oO
           oO
           oO
FLOW  ^   °o
           oO
           oO
           oO
           oO
                    oO
                    oO
                       NOZZLE
                    00
                    oO
            NOTES
 100% ISOKINETIC

vn = vs
mn = 8 grains/min
Q,, = 1 cf m
cn = 8/1 = 8 grains/cf
SLIDE  153-4
FLOW
           oQ
0
o
_^000 NOZZLE
-»-ooO
— ooo
— ^-0 o O


O
O
200C


W 7=Z
mn =

Q-
n -

c ~~
                                      200% ISOKINETIC
                                          12 grains/min
                                          2cfm
                                         - 12/2 = 6 grains/cf
SLIDE 153-5
           oO
                                       50% ISOKINETIC

                                    vn = 1/2 vs
                                    mn = 6 grains/min
                                    Qn = 0.5 cfm
                                    cn = 6/0.5 = 12 grains/cf
                                   M-15

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SLIDE  153-3



FLOW




oO
00
°O
oO
oO
oO
oO
oO
oO
. oO
oo NOZZLE
oO
oO
oO
oO
oQ
               NOTES
    100% ISOKINETIC

   v = v
   mn = 8 grains/min
   Qn = 1 cf m
   cn = 8/1 = 8 grains/cf
SLIDE 153-4
FLOW
   200% ISOKINETIC

  vn = 2v,
  mn = 12 grains/min
  Qn = 2 cf m
  cn =12/2 = 6 graihs/cf
SLIDE 153-5
           oO
           oO
    50% ISOKINETIC

 vn = 1/2 vs
 m,, = 6 grains/min
 Qn = 0.5 cfm
 cn = 6/0.5 = 12 grains/cf
M-16

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SLIDE 153-6
        RESULTS
                                                            NOTES
100%lsokinetic—  8gr/ft3
200% Isokinetic —  6 gr/ft3
 50% Isokinetic — 12 gr/ft3
 SLIDE  153-7
           POLLUTANT MASS RATE EQUATIONS
PMR
I IVIII
            ..
                    VsstdAs
               mstd
 PMR  =

Whereas
 PMRC — pollutant mass rate calculated on
       the concentration basis
 mn  — mass collected on the filter and
       probe
 Vm  — volume metered by the sample train
   ""  at standard conditions
 v,  — velocity of the stack at standard
   ""'   conditions
 As  — area of the stack
 PMR. — pollutant mass rate calculated on
       the ratio of areas basis
 H   — time tested
 An  — area of the nozzle
                                          M-17

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SLIDE  153-3

FLOW


oQ
°o
. °9 .
oO
oO
oO
o O
oO
oo NOZZLE
oO
oO
oO
oO
              NOTES
  100% ISOKINETIC

  vn = vs
  mn = 8 grains/min
  Qn = 1 cf m
  Cn = 8/1 = 8 grains/cf
SLIDE 153-4
 FLOW
  200% ISOKINETIC

 vn  = 2vs
 mn = 12 grains/min
 Qn  = 2 cf m
 cn  = 12/2 = 6 grains/cf
 SLIDE 153-5
            oO
                   oo O
            oO
   50% ISOKINETIC

vn = 1/2 vs
mn = 6 grains/min
Qn = 0.5 cfm
cn = 6/0.5 = 12 grains/cf
                                   M-18

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SLIDE  153-8
NOTES
          SIMPLIFIED MASS RATE EQUATION


     The equations below have aU constant values removed.
           M
PMRa = Mr
                   vSstd,As,e,
                   and An are all constant
  Note: The pollutant mass rate on the concentration basis (PMRJ is a result
     of both the mass and sample volume collected. The pollutant mass
     rate on the area basis is dependent on only mass.
 SLIDE  153-9
RESULTS OF PMR, FOR SMALL PARTICLES
       100% Isokinetic - C = ^ = 4 gr/ft3

                             8
       200% Isokinetic - C =   = 4 gr/ft3
      50% Isokinetic - C =     = 4 gr/ft3
                                         M-19

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SLIDE



FLOW




153-3
oO
"O
oO
oO
oO
oQ
oO
oO

oO
oO
00 NOZZLE
oO
00
oO
oO
oO
                                                  MOTES
                                      100% ISOKINETIC

                                      vn = vs
                                      mn = 8 grains/min
                                      Q0 = 1 cf m
                                      cn = 8/1 = 8 grains/cf
SLIDE  153-4
                                      200% ISOKINETIC

                                     vn  = 2vs
                                     mn = 12 grains/min
                                     Qn = 2 cf m
                                     cn  = 12/2 = 6 grains/cf
SLIDE 153-5
                                       50% ISOKINETIC

                                    vn = 1/2 vs
                                    mn = 6 grains/min
                                    Qn = 0.5 cfm
                                    cn = 6/0.5 = 12 grains/cf
                                    M-20

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SLIDE  153-10
            NOTES
           PLOT OF % ISOKINETIC
                    VS.
        POLLUTANT CONCENTRATION
 i
    200%
     150%
 n  TRUE
 U  VALUE
 2
     50%
      0%
        0%
                      I
               50%     100%

                   % ISOKINETIC
IPMRJ SMAU
                            150%    200%
SLIDE 153-11

RESULTS OF PMRC FOR LARGE PARTICLES
     100% Isokinetic - C = ~ = 4 gr/ft3
     200% Isokinetic - C = ~ = 2 gr/ft3
     50% Isokinetic - C - — = 8 gr/ft3
                                  M-21

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SLIDE  153-3



FLOW _




oO
oO
oO
oO
oO
oO
oO
oO
oO
oO
oo NOZZLE
oO
oO
oO
oO
oO
                                      100% ISOKINETIC







                                     Vn = Vs




                                     mn = 8 grains/min




                                     Qn = 1 cf m




                                     cn = 8/1 = 8 grains/cf
SLIDE 153-4
 FLOW
                                      200% ISOKINETIC
                                     Vn =
                                     mn = 12 grains/min




                                     Qn = 2 cf m



                                     cn = 12/2 = 6 grains/cf
 SLIDE 153-5
           oQ
           oO
   50% ISOKINETIC






vn = 1/2 vs



mn = 6 grains/min



Qn = 0.5 cfm



cn = 6/0.5 = 12 grains/cf
                                  M-22

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SLIDE  153-12                                         NOTES

              PLOT OF % ISOKINETIC
                     VS.
           POLLUTANT CONCENTRATION
                                   IPMH.I SMALL
                                   IPMRJ LARGE
NOTE:
 Since no stack contains either all large or all small particles, the bias will be
 in the colored area.
 SLIDE  153-13

RESULTS OF PMRa FOR SMALL PARTICLES
            100% Isokinetic — 4 gr


            200% Isokinetic — 8 gr


            50% Isokinetic — 2 gr
                                       M-23

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SLIDE  153-3
           oO
           oO
FLOW
            OQ
            oO
            oO
            oO
            oO
                    oO
                    oO
                    oo
                       NOZZLE
                    oO
                    00
                    oO
                    °0
            NOTES
 100% ISOKINETIC

v = v
mn = 8 grains/min
Qn = 1 cfm
cn = 8/1 = 8 grains/cf
SLIDE  153-4
                                      200% ISOKINETIC

                                     vn  = 2vs
                                     mn = 12 grains/min
                                     Q,, = 2 cfm
                                     cn  = 12/2 = 6 grains/cf
SLIDE  153-5
           oO
                                       50% ISOKINETIC

                                    vn  = 1/2 vs
                                    mn = 6 grains/min
                                    Q0 = 0.5 cfm
                                    cn  = 6/0.5 = 12 grains/cf
                                  M-24

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 SLIDE 153-14
           PLOT OF % ISOKINETIC
                    VS.
       POLLUTANT CONCENTRATION
NOTES
    200%
H   150%
<
oc
t-
1
3   TRUE
8  VALUE


I
     0%
       0%
              50%     100%     150%

                  % ISOKINETIC
                                    (PMRJ SMALL
 SLIDE 153-15
RESULTS OF PMR= FOR LARGE PARTICLES
          100% Isokinetic — 4 gr
          200% Isokinetic — 4 gr
           50% Isokinetic — 4 gr
                                 M-25

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SLIDE  153-16
                                           NOTES
          PLOT OF % ISOKINETIC
                   VS.
       POLLUTANT CONCENTRATION
\
o
   200% —
    150% —
UJ
O
Z  TRUE
8  VALUE
50%
    0%
             50%
                    100%

                 % ISOKINETtC
                          150%
                                  (PMRJ SMALL
                              (PMR.I LARGE
                                 200%
 SLIDE 153-17
            PLOT OF % ISOKINETIC
                     VS.
         POLLUTANT CONCENTRATION
     200%
  O
  i
  a
  i-
  UJ
  u
  O
  o
  s
                                   200%
                                 M-27

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SLIDE 153-18                                     NOTES

  The pollutant concentration can be
calculated by either equation; however,
the EPA chose to use PMRC since most
particles for new sources are small and
PMRG gives the true value for small par-
ticles. The proposed regulations had the
tester calculate the results by both
methods and average the results.
 SLIDE  153-19

                  Conclusion
 PMR  = % Isokinetic      pMR
        a            100
                                     M-29

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             SECTION N.  PRECISION AND ACCURACY OF TEST METHODS

Subject                                                               Page

1.  Information to support data quality acceptance for performance
    audits and routine monitoring (memo from Dr. T. R. Mauser,
    Director, EMSL, EPA, to Dr. Courtney Riordan, Deputy Assistant
    Administrator, Monitoring and Support Branch, EPA)                N-3

2.  Error analyses                                                    N-8

3.  Slides                                                            N-13
                                     N-l

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SUBJECT:
  FROM:
    TO:
                   UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                            Research Triangle Park, N.C. 27711
  DATE:  October  10, 1980
          Information to Support Data Quality Acceptance Criteria for Performance
          Audits and Routine Monitoring
Dr.  Thomas R.  Mauser, D^__,
Environmental  Monitoring Systems Laboratory,  RTP (MD-75)

Dr.  Courtney Riordan
Deputy Assistant Administrator
  for Monitoring and Technical Support (RD-680)
               Your  memo  of  September  22,  1980, has generated a large amount of

          data gathering  and documentation.   I have divided it into two sections,

          ambient and source.   I  hope  it  is  some  help to you.

          Enclosure

          cc:   D.J.  von Lehmden
               M.R.  Midgett
               J.C.  Puzak
               L.J.  Purdue
               T.A.  Clark
               F.J.  Burmann
  EPA Pom 1320-6 (R.». 3-76)
                                         N-3

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                          STATIONARY SOURCE








      Provided here in Table A-3 are the estimates of precision and accuracy



 for those source emission test methods that the Source Branch of the Quality



 Assurance Division has either collaboratively tested or subjected to a multi-



 sample, single-laboratory evaluation.   Because of the great expense involved



 in the collaborative testing of source emission methods, such tests are not



 normally performed unless they are justified by the particular situation.



 For example, a method for a pollutant of critical importance, and that will



 incur widespread usage, might warrant collaborative testing whereas one that



 would be used intermittently for a few industries would not.  Where collaborative



 testing is not justified and/or budgeting restrictions do not allow the expense,



 a multi-sample, single-laboratory evaluation is routinely conducted during the



 development and evaluation of the test method to obtain within-laboratory



 precision estimates.   The estimates in Table A-3 reflect this; there is no



 between-laboratory standard deviation shown for those methods that have not



 been collaboratively tested.








     Because the true pollutant concentration of a stack gas is unknown and



 constantly changing,  estimates of method accuracy are particularly difficult



 to obtain.   These estimates are frequently obtained from analysis of standard



 cylinder gases, analysis of reference materials that test the accuracy of the



 analytical  procedure only, or comparison with another Reference method or



 instrument to establish relative accuracy.








     Table A-4 provides a listing of source emission methods for which precision



and accuracy data are not available.





                                    N-4

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     TABLE A-3.   SOURCE EMISSION METHODS FOR WHICH PRECISION/ACCURACY DATA EXISTS BASED ON COLLABORATIVE TESTS
                 OR SINGLE-LABORATORY EVALUATIONS
 EPA
Method
                                                        Standard Deviation
Description/Appl ication
Condition of test    Within Lab
                                                                             Between Lab
                  Accuracy
        Velocity
        Volumetric Flow

        C0_ (manual)
        0« (manual)
        MSlecular Weight

        Particulate Emission
        Stack Moisture Content
6       SOp-Power Plant
                                       Real sample,
                                       Multi- laboratory
                     3.9% of flow
                     5.5% of flow

                     0.2%
                     0.3%
                     0.35 g/g mole

                    10.4% of cone.
                     0.1%
                                                            4.0% of cone.
 5.0% of flow
 5.6% of flow

 0.4%
 0.6%
 0.048 g/g mole

12.1% of cone.
 0.1%
                                                                     5.8% of cone.
                                                                                      Accurate within limits
                                                                                      of method precision
Not determinable
Within limits of
method precision

Accurate within limits
of method precision
7       NO -Nitric Acid
        N0*-Power Plant

8       S0?-Sulfuric Acid Plant
        H2S04-Sulfuric Acid Plant

9       Stack Gas Opacity
  10 .      CO-Refinery FCC

  11       H2S-Refinery Fuel Gas
  12        Pb
                             Simulated sample,
                             Multi-laboratory

                             Real sample,
                             Single laboratory
                                                           14.9% of cone.
                                                            6.6% of cone.
                                                         13 ppm

                                                           2.1% of cone.


                                                           5% of cone.
                                                                    18.5% of cone.
                                                                     9.5% of cone.
8.0 mg/m~
2.7 mg/m
2.0% of
opac i ty
11.2 mg/m_
3.0 mg/m
2.0% of
opac i ty
n
n
5%
of
                                       25 ppm

                                         4.5% of cone.
                  5% opacity at level
                  of standard

                  < 24 ppm

                  4% at level of standard
                                                                  within limits
                                                         of method precision
                                                                                                r—CONTINUED	

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  TABLE A-3. (continued)
   EPA                                                        	
  Method    Description/Application      Condition of test    Within Lab
                                                        Standard Deviation
                                                                     Between Lab      Accuracy
   13A      F  by SPADNS Analysis
i
o»
   13B

   15


   16

   17

   23

   24
                             Real sample,
                             Mu 11 i-1aboratory
F  by SIE Analysis

H.S, COS, CS, Sulfur
Recovery

Total Reduced Sulfur - Kraft

Particulate

Chlorinated Hydrocarbons

Volatile Organics from
Paint
Real sample,
Single laboratory
0.044 mg/m        .064 mg/m


0.037 mg/m3       0.056 mg/m3

8% of cone.           	
                      8% of cone.

                      6% of cone.

                      3% of cone.

                      8% Water Based Paint
                      0.5% Solvent Based
                        Paint
  101/102   Hg/Chlor-Alkali Plants3
                             Real samples,
                             Multi-laboratory
                      1.6 pg/ml
                 1.8 ug/ml
-.08 mg/1


-.10 mg/1

10% at level of standard


10% at level of standard

Not determinable

-3%

Not determined




-0.4 ug/ml
104
105
106
110
111
Be
Hg in Sewage Sludge
Vinyl Chloride
Benzene
Hg in Sludge Incinerator
Stacks
H ii
Real samples,
Single laboratory
Real samples,
Multi -laboratory
Real samples,
Single laboratory
Real samples,
Single laboratory
0.4 pg/in
0.2 ug/g
2.5% of cone.
9% of cone.
3
4.8 ug/m
0.6 ug/m -0.13 ug/m
nCCUraLc WICRIR
of method
6.3% of cone. -2% at level of
•t-1 IV at- IAI/A! i
TO. Jj* at. level 1
	 Unknown
precision
standard
>f standard


  a
   Precision for analytical portion only.

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          TABLE A-4.  SOURCE EMISSION METHODS fOR WHICH PRECISION AND ACCURACY DATA ARE NOT ..
 EPA
Method
         Application
Present Status
Comments on Precision/Accuracy
  1

  4


 14

 18

 19

 20

 21
 25

 26

 27

 28

 29

103


107

108

109
Sampling point selection

Estimate of stack moisture


Design of Al Plant-Roof Monitoring System

NH- NO- emissions from fertilizer plants

Calculation of F factor

NO , SO- from gas turbines
  A    £

Leak test method for valves and pumps
in organic processes

Fugitive emissions estimate by visual
observation

Non-methane organic emissions

Organic emissions from asphalt processing

Reserved

Urea emissions from fertilizer plants

Volatile organic contents of printing ink

Screening method for Be


Vinyl chloride monomer in resin

As emissions from smelters

Visual emissions from coke ovens
Promulgated

Promulgated


Promulgated

Future Proposal

Promulgated

Proposed

Future Proposal


Future Proposal


Proposed

Future Proposal



Proposed

Future Proposal

Promulgated


Promulgated

Future Proposal

Future Proposal
Precision/accuracy not applicable

Expected to be similar to Method 5
moisture determination

Precision/accuracy not applicable

Method under development

Precision/accuracy not applicable
Precision/accuracy not applicable
Method being evaluated

Method under development
Method under development

Precision/accuracy expected to be
similar to Method 104
Method under development

Method under development

-------
                              ERROR  ANALYSIS*

Introduction
     The problem of accuracy in stack  sampling measurements is  considered
and debated in almost every report or  journal article  in  which  stack sampling
data appear.  There exists, however, a great deal  of misunderstanding in the
engineering community on the difference between  error,  precision,  and accuracy.
This misunderstanding often leads  to a misinterpretation  of analytical  studies
of stack sampling methods.  The type of error analysis  often used  applies
only to "randomly distributed error  with a  normal  distribution  about the true
value."
     A discussion of the definitions of terms normally  used in  error analysis
will be given in a course lecture.   The definitions are also included in this
manual for your future reference.  It  is hoped that by  studying this section
the student will realize the limitations of error  analysis procedures and will
be able to more carefully design experiments that  will  yield results close to
the "true" value.

Definitions
Error:  This word is used correctly  with two different  meanings (and frequently
incorrectly to denote what properly  should  be called a  "discrepancy"):
     (1) To denote the difference  between measured value  and the "true" one.
         Except in a few trivial cases (such as  the experimental determination
         of the ratio of the circumference  to the  diameter of a circle), the
         "true" value is unknown and the magnitude of  the error is hypothetical.
         Nevertheless, this is a useful  concept  for the purpose of discussion.
     (2) When a number such as a = +_ 0.000008 x  1010 is given or implied, "error"
         refers to the estimated uncertainty in  an experiment and  is expressed
         in terms of such quantities as standard deviation, average deviation,
         probable error, or precision  index.
*
 Adapted from Y. Beers, Theory of  Errors, Addison-Wesley, Reading, Mass, (1958)
 pp. 1-6.
                                   N-8

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Discrepancy:  This is the difference between two measured values of a quantity,
such as the difference between those obtained by two students, or the difference
between the value found by a student and the one given in a handbook or text-
book.  The word "error" is often used incorrectly to refer to such differences.
     Many beginning students suffer from the false impression that values found
in handbooks or textbooks are "exact" or "true."  All such values are the results
of experiments and contain uncertainties.  Furthermore, in experiments such as
the determination of properties of individual samples of matter, handbook values
may actually be less reliable than the student's because the student's samples
may differ in constitution from the materials which were the basis of the hand-
book values.
Random Errors:  Sometimes when a given measurement is repeated the resulting
values do not agree exactly.  The causes of the disagreement between the
individual values must also be causes of their differing from the "true" value.
Errors resulting from these causes are called random errors.  They are also
sometimes called experimental or accidental errors.
Systematic or Constant Errors:  If, on the other hand, all of the individual
values are in error by the same amount, the errors are called systematic or
constant errors.  For example, all the measurements made with a steel tape that
includes a kink will appear to be too small by an amount equal to the loss in
length resulting from the kink.
     In most experiments, both random and systematic errors are present.  Some-
times both may arise from the same source.
Determinate and Indeterminate Errors:  Errors which may be evaluated by some
logical procedure, either theoretical or experimental, are called determinate,
while others are called indeterminate.
     Random errors are determinate because they may be evaluated by application
of a theory that will be developed later.  In some cases random or systematic
errors may be evaluated by subsidiary experiments.   In other  cases it may be
inherently impossible to evaluate systematic errors, and their presence may be
inferred only indirectly by comparison with other measurements of the same
quantity employing radically different methods.  Systematic errors may  sometimes
be evaluated by calibration of the instruments against standards, and in these
cases whether the errors are determinate or  indeterminate  depends upon  the
availability of the standards.
                                     N-9

-------
Corrections:  Determinate systematic errors and some determinate random errors
may be removed by application of suitable corrections.   For example,  the measure-
ments that were in error due to a kink in a steel  tape  may be eliminated by com-
paring the tape with a standard and subtracting the  difference from all the mea-
sured values.  Some of the random error of this tape may be due to expansion and
contraction of the tape with fluctuations of temperature.   By noting  the tempera-
ture at the time of each measurement and ascertaining the coefficient of linear
expansion of the tape, the individual  values may be  compensated for this effect.
Precision:  If an experiment has small  random errors, it is said to have high
precision.
Accuracy:  If an experiment has small  systematic errors, it is said to have high
accuracy.
Adjustment of Data:  This is the process of determining the "best" or what is
generally called the most probable value from the data.   If the length of a
table is measured a number of times by the same method, by taking the average of
the measurements we can obtain a value more precise  than others, then a weighted
average should be computed.  These are examples of adjustment of data for
directly measured quantities.  For computer quantities  the process may be special-
ized and complicated.
Classification of Errors
Systematic Errors:
     (1) Errors of calibration of instruments.
     (2) Personal errors.  These are errors caused by habits of individual
         observers.  For example, an observer may always introduce an error
         by consistently holding his head too far to the left while reading
         a needle and scale having parallax.
     (3) Experimental conditions.  If an instrument  is  used under constant
         experimental conditions (such as of pressure or temperature) different
         from those for which it was calibrated, and if no correction is made,
         a systematic error results.
     (4) Imperfect technique.  The measurement of viscosity by Poiseuille's
         Law requires the measurement of the amount  of  liquid emerging from
         an apparatus in a given time.   If a small amount of the liquid
         splashes out of the vessel which is used to catch it, a systematic
         error results.

                                    N-10

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Random Errors:

     (1) Errors of judgment.  Most instruments require an estimate of the frac-
         tion of the smallest division, and the observer's estimate may vary from
         time to time for a variety of reasons.

     (2) Fluctuating conditions (such as temperature, pressure, line voltage).

     (3) Small disturbances.  Examples of these are mechanical vibrations or,
         in electrical instruments, the pickup of spurious signals from nearby
         rotating electrical machinery or other apparatus.

     (4) Definition.  Even  is the measuring process were perfect, repeated mea-
         surements of the same quantity might still fail to agree because that
         quantity might not be precisely defined.  For example, the "length" of
         a rectangular table is not an exact quantity.  For a variety of reasons
         the edges are not  smooth (at least if viewed under high magnification)
         nor are the edges  accurately parallel.  Thus even with a perfectly
         accurate device for measuring length, the value is found to vary depend-
         ing upon just where on the cross section the "length" is measured.

Illegitimate Errors:  These errors are almost always present, at least to a
small degree, in the very best of experiments and they should be discussed in

a written report.  However, there are three types of avoidable errors which have
no place in an experiment,  and the trained reader of a report is justified in

assuming that these are not present.

     (1) Blunders.  These are errors caused by outright mistakes in reading
         instruments, adjusting the conditions of the experiment, or performing
         calculations.  These may be largely eliminated by care and by repetition
         of the experiment  and calculations.

     (2) Errors of computation.  The mathematical machinery selected for calcu-
         lating the results of an experiment  (such as slide rules, logarithm
         tables, adding machines) should have  errors small enough to be complete-
         ly negligible in comparison with the  natural errors of the experiment.
         Thus if the data are accurate to five significant figures, it is  highly
         improper to use a  slide rule capable  of being read to only three  figures,
         and  then to state  in the report that  "slide rule error" is a source of
         error.  Such a slide rule should be used for calculating the results
         of an experiment having only three or preferably two significant  figures.
         On the other hand, if the experiment  does give five  significant figures,
         five or six-place  logarithm talbes or some other more accurate means  of
         calculation should be used.

     (2) Chaotic Errors.  If the effects of disturbances  become  unreasonably
         large - that is, large compared with  the natural random errors  -  they
         are  called chaotic errors.  In such  situations are experiment should
         be discontinued until the source of  the disturbance  is  removed.


                                    N-ll

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SLIDE 154-0                                       NOTES


PRECISION AND ACCURACY
            OF
EPA REFERENCE METHODS
 SLIDE 154-1


    PRECISION AND ACCURACY
       METHODS EVACUATION

• REAL SAMPLE (Multi-Laboratory)
• SIMULATED SAMPLE (Multi-Laboratory)
• REAL SAMPLE (Single Laboratory)
 SLIDE 154-2


             REAL SAMPLE
            (Multi-Laboratory)

  Approximately 10 different testing laboratories test
 the same source simultaneously. This is usually referred
 to as a "collaborative test." This testing is expensive
 and testing parameters are not usually varied.


                                   N-13

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SLIDE 154-3

           SIMULATED SAMPLE
             (Multi-Laboratory)

  Approximately 10 different testing laboratories test a
common manifold containing a known concentration
of pollutant. This testing is expensive but the pollutant
concentration is known and can be varied.
NOTES
SLIDE  154-4

               REAL SAMPLE
             (Single Laboratory)

  A single laboratory utilizes a "methods evaluation"
train. This train collects a minimum of four samples for
a single point. This testing is less expensive and any
sampling  parameters can be varied to determine its
effect.
SLIDE  154-5
                                        N-15

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SLIDE  154-6
                                                            NOTES
 SLIDE 154-7
                QUAD TRAIN CONFIGURATION
 IMPINGER CONTENTS
 METHOD 8 BACK HALF

 1 — 50 ml H20
 2.— 100 ml 80% IPA
 3 — 100 ml 10% H,0,
 4 — 100 ml 10% HA
 5 — 300 g SIUCA GEL
           PHOBE2C1I"-
           PROBE1T
           PROBE 4 C"
           PROBE 3 r~
                                           N-17

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SLIDE  154-8
                                       NOTES
EPA
METHOD
2
3
DESCRIPTION
Velocity
Volumetric Flow
CCh (manual)
O2 (manual)
Molecular Weight
STANDARD DEVIATION
Within Lab Between Lab
3.9% 5.0%
5.5% 5.6%
0.2% 0.4%
0.3% 0.6%
0.35 g/g mole 0.48 g/g mole
SLIDE 154-9
  EPA
METHOD

    5
    6
    7
DESCRIPTION

   Particulate
SO2 - Power Plant
NO, - Power Plant
STANDARD DEVIATION
 Within Lab  Between Lab
   10.4%       12.1%
    4.0%        5.8%
    6.6%        9.5%
                                   N-19

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         SECTION 0.  SIGNIFICANCE OF ERROR FOR SOURCE TEST OBSERVERS

Subject                                                               Paqe
1.  Use of significance of error for source test observer's
    decisions                                                         0-3

2.  Slides                                                            0-11
                                     0-1

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      USE OF SIGNIFICANCE OF ERROR FOR SOURCE TEST OBSERVER'S DECISIONS
                                     by
                                 Bill DeWees

     The addition of numerous test methods, requirements, quality assurance
procedures, allowable options by the tester, alternative methods and published
articles, has made the average agency performance tester and/or observer all
ask the same question.  What is really important?  If there were an easy an-
swer, the question would not have to be asked.  The only easy answer is
the standard military or politician's answer:  It varies with the conditions.
Unfortunately, this is the correct answer.
     This paper is designed to provide the necessary information and concepts
to allow the agency staff to determine what is important as the conditions
vary.
     The tester or observer needs to know three things to determine what is
important.
     1)   What is the data to be used for, (i.e., proof of compliance, proof
          of violation or engineering evaluation)?
     2)   What are the direction and magnitude of any biases?
     3)   What is the acceptable bias that will be allowed before rejecting
          the results?
     Let's look at the three uses of the data and explore what biases would
be acceptable.  First, the source is attempting to prove itself in compliance
with the regulation.  If the test results conclusively show compliance with  the
regulation, any magnitude of bias in the data that increased the measured re-
sults  (high bias) could be accepted for proof of compliance.  These results  may
not, however, be valid for future use in emissions trading or banking.  An
acceptable low bias could be any amount that does not change what would be vio-
lation  into compliance.
                                     0-3

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      Since the final results are not known  during  the on-site testing,  the
 observer generally would rather have a  fixed  value to allow or disallow the
 test run while on site.   Past collaborative tests  have shown most of the NSPS
 reference methods to have a reproducibility of about  + 10  percent.   Therefore,
 when the source is trying to demonstrate  compliance,  a good rule  of thumb for
 allowing biases determined on-site  may  be less than 10 percent high bias and
 5 percent low bias.   Setting more stringent criteria  than these for each sample
 run could be costly in time and money for both the  industry and agency.
      The second case is  when the agency is  trying  to  prove that the source is
 in violation with the applicable regulation.  Any  test data that  prove  conclu-
 sively that the source is in violation could contain  any  magnitude  of low bias.
 The  low bias will not be challenged by the industry  unless  the testing  does not
 comply with the legal  requirements  as stated by the reference  method.   When  the
 agency bears the proof of violation, a good rule of thumb for  acceptable bias
 would be up to a 5 percent high  bias and  down to a 10  percent  low bias.   Again,
 let me stress that for proof of  violation, meeting the  requirements  of  the
 reference method is  manadatory.
      The final  example is data  used for engineering evaluation.  Any bias  may
 be acceptable in this  case as long as it  is quantifiable.   The  data  can  then
 be adjusted or a confidence limit will be placed on it.
      Both on-site and  posttest  data analysis will be made  by the agency.   The
 agency observer should be aware  of his authority and acceptable biases  on-site.
 It is the belief of  the  author  that an agency observer  that  is  not  allowed to
 make decisions  on-site,  does  not have the right to observe  the  test  and  later
 reject data based on his  on-site observations.  Rejection of a  testing  series
 is both time and cost  consuming  for the agency and industry.  The agency should
 not compromise  its standards  but should make every effort both  on-site  and in
 posttest analysis  to obtain  test results acceptable for their purpose.
      Error  from the  measurement  of most of the sampling parameters  have  very
 little  effect on  the final  data  results.  Table 1 was designed  to provide  a
 useful  tool  in  estimating  the magnitude and direction of  biases from measure-
ment  errors  of  most  sampling parameters.  The parameters are shown  separately
but can  be  added  together when more than one parameter  has been erroneously
measured.   The  table was developed using the testing values  in  the  expected
average range of  testing.  Also, it was assumed that a  2  percent isokinetic

                                    0-4

-------
error makes a 1 percent error in sample concentration.  These values, although
not always exact, should be good enough to make the required on-site or post-
test decisions.
     To better explain the table, let's use three examples.

EXAMPLE 1
     The NSPS test is on an asphalt plant which has a concentration standard
of 0.04 g/scf.  It has been discovered that the test team incorrectly measured
the stack temperature.  The test team measured value was about 350°F, but the
correct reading should be about 320°F.  The question is how much error is there
from a 30°F high measurement?  Table 1 shows that for ts, a 10°F error will
cause a -0.4 percent bias for a concentration measurement.  Therefore, a +30 F
error would cause a -1.2 percent bias in the concentration measurement.  The
30°F error does not meet the requirements of +1.5 percent of the absolute
temperature, however, the error would have little effect on the final data
results and could therefore be allowed.  The -1.2 percent bias means that the
value that will be shown in the source test report will be 1.2 percent less
than the value that should have been measured.  This bias does aid the source
in trying to show compliance, but the error is so small,  it is almost meaning-
less.

EXAMPLE 2
     The test  is on a dog food fixing tank.  The allowable mass emission rate
standard is about 5 Ib/h.  The calibration factor of  the  dry gas meter has
been checked with two critical orifices  supplied by EPA.  The results of the
check shows the Y factor should be 0.91  but the tester  reports a Y factor  of
0.97.  The error is 0.06, which should be multiplied  by the error  in  the table
for Y at 0.01  which causes a +1 percent.  You  inform  the  tester that  the data
will likely be biased high by 6 percent.  You  decide  at this point to allow
the tester to  proceed as long as he  assures you that  a  good posttest  calibra-
tion will be made for the dry gas meter.
     At the conclusion  of the first  run,  the  posttest leak-check indicated
a  leak rate of 0.15 cfm.  This  is well above  the allowable,  but the  tester
said he will just subtract  the  leak  rate from the  final sample  volume as

                                     0-5

-------
 shown  in  the  reference method.  Since the rate of sampling was only about
 0.6  cfm,  this could  potentially cause a 25 percent high bias.  You should sug-
 gest that the run  be invalidated and that another run be made.  The tester
 informs you he has the right to use the procedures that could cause up to a
 25 percent high bias.  You should then inform him that you have an obligation
 to protect the source as well as the general public and proceed to inform the
 facility  contact of  the consequences that the tester has decided to impose on
 the  source.

 EXAMPLE 3
     The  test is at  a Subpart D power plant.  The concentration standard is
 0.1  lb/10 Btu.  You are familiar with the testing crew and they usually do
 a good job.   This  test happens to be on one of those days when nothing seems
 to go  right.
     You  first spot  that the pi tot tube and nozzle are not the minimum distance
 of 3/4 of an  inch  apart.  This is corrected by simply bending the pitot tube
 away from the nozzle.  Next, you check the stack thermocouple and both dry
 gas  meter thermometer readings against each other at ambient temperature.  The
 stack  thermometer  reads 81°F; the inlet dry gas thermometer reads 79°F; and
 the  outlet thermometer reads 63°F.   You inform the team of the discrepancy
 but  they  have no way of adjusting the thermometer.   You inform them that a
 posttest  calibration must be performed on both thermometers.   To estimate
 what error might occur, you use Table 1 to determine the expected error from
 the  average temperature of the meter (tm), being low by 10°F.  The table shows
 that 5°F  gives an  error of -0.9,  therefore,  a -10°F error would be +1.8 per-
 cent error.   This  means the measured value would 1.8 percent higher than the
 true value.
     After the second run, the orsat results seem wrong.   There must have been
 a leak or  some procedure was in error.   The tester knows that the Op value
 should have been about 4.5 percent;  however, his results were 7.7 percent 02.
 Going back to the  table,  a 1 percent error at 5 percent 02 will cause a +6.7
 percent error, therefore a 3.2 percent error causes a +21.4 percent error.
Since the test team  is a reputable one, the tester requests that the test be
 invalidated since  there was an obvious error.  The observer agrees and another
run is  performed.
                                    0-6

-------
     When the observer receives the final report for review, he notes that the
test team has the static pressure as +6.7 in. H20.  The observer thought that
the value should have been -6.7 in. H20; however, he was not sure.  To see if
this really makes any difference, he refers to Table 1 and finds that for Ps,
a 2 in. H20 error will cause a +0.1 percent change.  His change from +6.7 to
-6.7 in. H20 is -13.2 in. H,,0, which would cause about a -0.6 percent error.
The error is insignificant on the impact of the data, however, the observer
may wish to call the source and determine the actual sign of the static pres-
sure to enhance accuracy of data reporting.

OTHER ERRORS
     In addition to the table, four other potential major errors are listed:
1) two leak check procedures, 2) nozzle-pitot tube spacing, and 3) calibration
at the magnehelic.
     Generally, the most critical period for noting errors by the observer and
creating errors by the tester is during the sample recovery phase.  The ob-
server should be present, if possible, during the sample recovery phase.  Both
the probe rinse and used filter should be observed.  The filter should have
a clear space all around its border to show that no particulates have been
circumvented.  Generally, no particulate should exist that can be easily seen
by the naked eye.  No particles of that size should be able to get through
the control device, but if they do, they would not be a health hazard as they
would immediately fall to the ground after existing in the stack.  Their pres-
ence usually means that foreign debris has been caught by the sample train.
The color and appearance can also give information on process operation and
failure of the sample box to maintain the proper temperature.  A drastic color
change for one of the runs may indicate a process malfunction which should be
checked.  Also, as discussed in the paper on the "Role of the Agency Observer",
the apparent mass of particulate collected should be compared to the visible
emissions during test.
CONCLUSION
     There are numerous errors and nontypical conditions that can occur during
each sample run.  The observer should have a good understanding of the intent
of the test and the magnitude of error that will be tolerated by the agency;

                                     0-7

-------
he should then proceed to make his decision in a logical  manner,  using all
facts available at the time.  When the observer is worried about  not meeting
the requirements of the reference method(s),  usually a little creative think-
ing on the part of the observer and some posttest work by the test team can
solve the problem.  An example would be if the process shuts  down with one
point to go in a sample run, test the last point with the process off pro-
vided the fan is still running.  If the fan shuts down, you have  in fact
sampled the last point at the correct rate (nothing).   The posttest rejection
of a test is costly in both time and money to the source  and  agency.   If a
sample run will likely be rejected, reject it on-site since this  is far less
costly and time consuming.
                                    0-8

-------
                                TABLE 1.   ERROR ANALYSIS OF SAMPLING PARAMETERS
Parameter
Pbar
AH
tm
Ps
ts
AP
Moisture
Md
Md
Md
Mn
Time
Y
CP
Nozzle
diameter
Isokinetic
F factor
F factor
F factor
True value
30 in. Hg
30 in. Hg
528°R
30 In. Hg
600°R
1 in. H20
10%
29
29
29
100 mg
120 min
1.00
0.84
0.250 in.

100%
5% 02
10% 02
15% 02
Error
1 in. Hg
1 in. H20
5°R
2 in. H20
10°F
0.1 in. H20
1%
1% C02
1% 02
1% CO
1 mg
1 min
0.01
0.01
0.005 in.

10%
1% 02
1% 02
1% 02
Erroneous
value
31 in. Hg
30.07 in. Hg
533°R
30.15 in. Hg
610°R
1.1 in. H20
11%
29.15
29.03
29
101 mg
121 min
1.01
0.85
0.255 in.

110%
6% 02
11% 02
16% 02
Concentration
(%r
+ 4.1
+ 0.2
- 0.9
+ 0.1
- 0.4
- 2.5
+ 0.1
+ 0.1
+ 0.1
_
1.0
- 0.4
1.0
- 0.6
- 2.0

- 5.0,
+ 6.73
+10. n
+20.4°
QS
-1.6
_c
_c
-0.2
+0.8
+4.9
-0.2
-0.3
-0,1
-*
-'•
-Cr
_c
+ 1.2
c

_c
N/A*
N/A*
N/Ae

-------
                   TABLE 1 (continued)

                   o    Leak Check of the PItot Tube:

                        A posttest leak check of the pltot tube must be performed at a  minimum of 3 1n.  H20.
                        It 1s not possible to posttest calculate the error from a pltot tube that does  not
                        leak check.   However, 1f only one side of the pltot tube does not leak check, the test
                        or observer may wish to determine the maximum error that could  have occurred by the
                        following procedures.  Place the pltot tube back Into  the stack at a point of average
                        velocity using the same orientation as 1n the test.  Take the Ap reading.   Turn the
                        pltot tube over (180° reortentatlon).   Again take the  Ap reading.   The difference in
                        the two readings 1s the expected error 1n 1n.  H20.   If both  sides of the  pltot  tube
                        leak no error analysis 1s possible.

                   o    Spacing of the Pltot Tube to the Nozzle:

                        A minimum of a 3/4 1n.  spacing 1s required between  the pltot tube and nozzle.   If the
                        nozzle-pltot tube spacing 1s only 1/2  1n.  an error  of  a  7 percent high bias  1n  the flow
                        rate may be  caused.   A lesser  spacing  can cause even greater high bias error.
o                               ..                               -
5                  o    Calibration  of the Magnehellc -vs.  the  Inclined  Manometers;

                        The  error would be the  same  as  reported  for Ap.

                   o     Leak Check of  the Sample  Train:

                        The  train  1s to be posttest  leak  checked  at the maximum  vacuum  operated during  the test.
                        If the maximum leak  exceeds  0.02  cfm,  the leak  (leak rate times  the  sample time) is to
                        be substacted  from the  sample  volume.   It 1s  suggested when  leak  check at  the nozzle
                        exceeds  the allowable leak rate,  the leak check be performed  at  the  nozzle 2 1n. Hg
                        (or  the  static pressure,  whichever  1s  higher).   The train  should  then  be leak checked
                        at the  Inlet to  the  filter.  The  higher of the  two leakage rates  can  then be subtracted
                        from  the sample  volume.   Both  approaches  could  cause a high  bias  for  both concentrations
                        and  pmr  standards.   The percent bias will  be somewhere between  the maximum (assuming
                        there was no leakage during  the test)  and the minimum of  zero (assuming the maximum
                       measured leakage actually occurred during  the test).

-------
SLIDE 155-0                                       NOTES

SOURCE TEST OBSERVER'S USE
  OF SIGNIFICANCE OF ERROR
SLIDE 155-1

 BASIS FOR OBSERVER'S DECISIONS
1. What is the pupose of test?
2. What is direction and magnitude of bias?
3. What is the acceptable allowed bias?
 SLIDE 155-2

       USE OF ERROR ANALYSIS TABLE
                  (From Table 1)
    • Errors are calculated using values shown.
    • It is assumed that a  2% error in  the isokinetic
     sample rate results in a 1% error in concentration.
    • When more than one error occurs, use the sum of
     the errors.
 Note: The true value and erroneous measured value are
     shown to eliminate confusing the terms "measured
     high" and "measured low."

                                    0-11

-------
SLIDE  155-3                                          NOTES

               EXAMPLE 1
       For Concentration Standard
1. ERROR Ts: measQred value is 30°F too high.
2. 10°F causes a -0.4% bias (from Table 1).
3. Therefore. +30° F will cause a -1.2% bias.
 SLIDE 155-4

              EXAMPLE 2
      For Mass Emission Standard
                 PART 1
 1. ERROR Y: reported value is 0.06 too high.
 2. 0.01 causes a ^1% bias (from Table 1).
 3. Therefore, +0.06 will cause a +6% bias.
 SLIDE  155-5

                 PART 2
 1. ERROR: leak rate is 0.15 cfm.
 2. Sample rate is *» 0.6 cfm.
 3. Therefore, if total leak rate is subtracted, bias
   could be as high as +25%.
                                       0-13

-------
SLIDE 155-6                                            NOTES

              EXAMPLE 3
      For Concentration Standard

                 PART1
1. ERROR: pilot tube is < % in. from nozzle.
2. Table 1 shows that a Vf> in. spacing causes a
  7% bias.
3. Therefore, pitot tube  must be  bent until
  correct spacing is obtained.
 SLIDE  155-7

                     PART 2
 1. ERROR: oxygen reading is 3.2% too high.

 2. At 5% O2 a 1.0% Oz error causes a +6.7% bias (from
   Table 1).
 3. Therefore, a +3.2% O* error will cause a +21.4% bias.
 SLIDE  155-8

                     PARTS
 1. ERROR:  Static pressure reading  of +6.7  in.
   may have an incorrect sign.
 2. A 2.0 HaO error causes a 0.1% bias (from Table 1).
 3. Therefore,  sign should have  been negative not
   positive. A -13.4 in. H2O error will cause a -0.6% bias.
                                         0-15

-------
 SLIDE 155-9

       OTHER ERRORS
• Pitot tube leak-check
• Pitot tube/nozzle spacing
• Magneheiic calibration
• Sample train leak-check
NOTES
 SLIDE 155-10

  CRITICAL PHASE FOR OBSERVATION
• Check probe rinse for large particles.
• Check filter for large particles and color.
• Check filter for evidence of particle contamination.
< Check ratio of apparent mass collected to visible
  emission readings.
 SLIDE  155-11

                 CONCLUSIONS
   1. Determine purpose of test.
   2. Determine magnitude and direction of biases.
   3. Know acceptable bias allowed.
   4. Make every effort to meet test requirements
     and to use the data.
Note: Test rejection is costly in time and money for both
     the source and agency. If sample run will Ijkely be
     rejected, reject it on-site.
                                      0-17

-------
                    SECTION P.  STACK SAMPLING NOMOGRAPHS

Subject                                                               Page

1.  Stack sampling nomographs for field validation (prepared by
    Entropy Environmentalists, Inc.)                                  P-3

2.  Slides                                                            P-27
                                     P-l

-------
                        INTRODUCTION








     This publication is composed of nomographs which Entropy



Environmentalists, Inc. has found to be very helpful in est-



imating or checking parameters measured in stack sampling.



The charts are to be used as guides and should not be con-



sidered as accurate to the third significant figure (even



though some of them are that accurate).  The nomographs



are separated into three groups:  Moisture Content, Excess



Air, and Volume and Velocities.



     Two hints about using nomographs.  If you plan to use



the nomographs often, put Scotch "Magic Transparent Tape"



over each line; and when too many marks are made on the



lines, just erase them from the tape.  This saves the printed



markings from being erased or obliterated because of ex-



cess use.  The other hint is that if you plan to copy any



of these nomographs on a copy machine, be sure that the



machine does not shrink or expand the copy in one direction



more than the other.
                           P-3

-------
GROUP I - MOISTURE CONTENT



     The stack sampler is frequently confronted with the

need to estimate the moisture content of the stack gas

prior to sampling.  If he estimates incorrectly, he will

create an isokinetic error of about one percent for every

one percent error in his moisture estimates.  For this

reason, a package of moisture nomographs has been assem-

bled which will assist and hopefully improve the sampler's

estimates.



     A.  Wet.and Dry Bulb Temperatures

         Chart 1 is the most  useful of the psychrometric

     charts for stack samplers,  since it not only corrects

     for pressure,  but it also gives the results in per-

     cent moisture (absolute) on a volume basis.  Many

     stack samplers distrust  the wet and dry bulb method

     because it has given them erroneous data in the past.

     This is often due to lack of pressure corrections,

     although  the following conditions can also cause

     problems:

         Acid  gases (>10  ppm  S03) yield high moisture
         results.
         Low velocity  (<5 ft/sec) yields high moisture
         results.
                           P-4

-------
•a
i
en
25-









26-








27 -








28-







29-






30 -






31 -






32-





33 -
                 u»
                 wi
                                       180
-0





-200
       Ub
       UI
       u.


-400   5





-6OO





-800





-1000





-1200
                                                   CHAUT 1




                                 AIR - WATER VAPOR  PSYCHROMETRIC CHART


                                     (CORRECTS FOR ABSOLUTE PRESSURE CHANGES)
u/ S
y D
Z m
                                                                               « 3
                                                                               s S
                                                                                           — 50
                                                                                           h-40
                                                                                           L-30 "5
                                                                                                f
            H20 g



                 u

                 ui
                 at


                 g


            r-10
                                                                                           -0

-------
         High velocity (>50 ft/sec) yields erratic mois-
         ture results.
         High temperature (>250°F) yields erratic mois-
         ture results.  (HINT:   Put wet bulb in hot water
         instead of cold water.)

     Chart 2 is just a simpler  chart than Chart 1.  It does

not have any pressure corrections and is only good at 29.92

inches of mercury.   It is included because it can give you

approximate answers at a glance.   Use Chart 3 to correct

for pressure in Chart 2 or any  other psychrometric chart.



     B.   Combustion Calculations

         Since most fuels are made of carbon and hydrogen,

     it  is fairly easy to calculate the moisture content

     for combustion sources from the fuel analysis,  the

     free water in  the fuel, the humidity of the combustion

     air,  and Chart 4.   First,  you must know the excess

     air.   Charts 8,  9,  and 10,  later in this document,

     will assist you in this venture.

         Next,  you  need to know  the type of fuel.  This is

     usually known  unless a combination of fuels or refuse

     is  being fired.   For a combination of fuels,  calculate

     from Chart 4-A the answer  for each fuel and estimate

     some  reasonable middle answer.   For refuse,  since

     refuse  is  usually  paper, choose wood.
                           P-6

-------
-o
I
                          100 —,
                           90 —
                                              EXAMPLE:
                                    210
Wet bulb 160°F

Dry bulb 230'F
ANSWER: 30% HO
                             0 -J
                         _ 1000
                         P_ 900
                                                                                 Z_ 800
                                                                                    700
                                                                                         ft.
                                                                                         e
                                                                                         V
                                                                                    600  2
                                                                                         a

                                                                                         0)

                                                                                    500  e
                                                                                         a>
                                                                                 =-  400
                                                                                 =- 300
                                                                                 i_ 200
                                                                                 =- 100
                                                                                 L_ 0
                                  3
                                  03
                                                     CHAET 2

                             Nomograph for  calculating percent moisture in stack using
                                           wet and dry bulb thermometers
                                        Assumes  29.92  in.  Hg Stack Pressure

-------
EXAMPLES  A Psychrometric chart for t. « 200°F
                                     a
          and t  « 130*F, yields 11% moisture;
          however, the absolute stack pressure
          is 25 inches Hg.
          True Moisture - 1.4 x 11%
15.5% moisture
                                      CHART 3
                      CORRECTION FACTOR PRESSURE CORRECTIONS
                           FOR THE PSYCHROMETRIC CHARTS
                                    P-8

-------
*- 50
o
                  g  5

                 ^  §
                  S-«
x
*-«
<
VI
M
U

X
u
— 200


- 300

   400

   50C

   600
   700
   800
   900
   1000
   2:
   15

-  10
_  1
                        _  0.5
                                       Wood


                                       Bark
                                         -  Propan*
                                            Gasoline
                                            12 Fuel Oil
                                          . Bunker  "C" Oil
                                            Bituminous  Coal
                        Subbituminous and
                         Lignite
                                              - Anthracite
    1500

                   Figure A

       FOR DETERMINING MOISTURE III FLOE GAS

            FROM COMBUSTION OF FUEL
                                                                                               — 100
                                                                                  • 200


                                                                                  •300

                                                                                   400

                                                                                   500

                                                                                   600

                                                                                   700
                                                                                   800
                                                                                   900
                                                                                   1000
                                                                                                   * .4   ~
                                                                                                   81   -
                                                                                                                    .5.8
                                           -Coke
~—
L.

-
_ m
•
— '
~
—
™
r
-

1UU
50
40
30

20
10

^

2

1
0.5

ii
£
s

&
*
J
xv

>l

;

— iu
— 90
„

— 80
1. 70
— 60
_ 50
1 40

- 30

- 20
— 10
                                                                                                                   Figure B

                                                                                                     FOR DETERMINING MOISTURE IN FLUE OAC
                                                                                                           FROM FREE HATER IN FUEL
  10 —I
    e __
  o
  X
  »
    0 —
                                     — 0
                                     — 50
                                               x

                                               Id

                                               H
                                            U
                                            rt
                                        100
                                                                                   KJST mo*  t)   y^ of

                                                                                               2)   Free H«tex in Fuel

                                                                                               3)   Hunidity of Aablent Air


                                                                                   EXAMPLE)  Lignite with 40% free w»ter it
                                                                                      burned at 50% ExceM Air, which !• 90  *F
                                                                                      at 40% Relative Humidity.  Add 2.5%
                                                                                      (from fuel - Figure A), 6% (fro* fr««
                                                                                      water - Figure B), and 2% (froa ambient
                                                                                      air - Figure C) to get 10.5% moisture
                                                                                      in the stack gases.
                                                                                           CHART 4

                                                            NOMOGRAPHS FOR ESTIMATING MOISTURE  IN  COMBUSTION  SOURCES
                    Figure C

          MOISTURE FROM THE AMBIENT AIR

-------
    The free moisture in the fuel is not readily



apparent to the casual observer.  Coal and anthra-



cite usually contain from three to fifteen percent,



lignite and bark, ten to forty percent, and wood



and refuse, five to fifty percent.  If it is rain-



ing on the fuel, pick a higher number.  The source



may have some measured data you can use.



    The ambient air moisture is usually known.  The



local radio station usually gives it as percent



relative humidity,  so Chart 4-C corrects that to



percent moisture (absolute).








C.  Condenser and Silica Gel Methods



    If all estimating methods fail,  try measuring



the moisture directly.   Chart 5 is for low volumes



which is associated with silica gel tube methods.



Chart 6 is for larger volumes,  using the EPA Method



4.
                      P-10

-------
                          Ref.  1
           P  , inch H3



            2C  —






            25  —
                              A_ - - ~"
            •5
T3
I
     EXAMPLE:  F  " 30 in. Hg
               ID

              T  « 100»P
              VL - 1 ml HjC


              V  - 1 ft-
               D
     Draw line fron P  to T  to obtain Point 1
                    D    •

     Draw line froB Poir.t A to V,  and read B on Ref. 2.


     Draw line fron Poir.t B to V^ and obtain answer of


      4.9% H.O in Etack cas.

Rel





T , T
m
150 	
-
J-S0---:
-
.
53 	

0 	

-50 	








Ref. 1.
ifif. 2.
ler of

'. 2

Answer
*H20


50 -
40 -
30 -
20 -:
•
10 -i
.
Be
, 	 5- —
"~ ---____ 4 -
2 -

1 -











- 10
: s v nl H2° v,
- 7
- 6
- 5

— 4
*- 3

— 2

lf^


- 1.0
- 0.8
- 0.7
- 0.6
- 0.5

- 0.4

- 0.3


- 0.2

•
- 0.1

.' ft3
- 0.2

-
- 0.3

i- 0.4
- 0.5
>- 0.6
_ 0.7
— 0.8
_ 0.9
- 1.0

.

- 2

— 3

— 4

- 5
- 6
- 7
- 8
- 9
- 10

                                                               CHART  5


                                NOMOGRAPH FOR CALCULATING MOISTURE CONTENT FROM LOW VOLUMES

-------
tJ
I








V., ml H-0
1000 * 2

REF. 1 REF. 2




P , inch Hg
m

20-,
.
25-
•

30-

35-









_ , — """
— -*•








V °F

150 —
—
10.0 r-
— **
A_ _--'""" -
* ~- - -. _ __ 50 ~

-
o—I
-
m
-50 —I

EXAMPLE: P - 30 in. Hg
m
Answer
% HLO
2

50-
40-
30 -
20-.
•
10 ^
.
B - -
... 	 5—
"*""--- 4 -
2 -


1 -

— .
T - 100°F
m


V « 100 ml HO
V - 100 ft3
m




Draw line from P to T to obtain Point A on Ref. 1.
mm
iraw line from Point A to V. and read B on Ref. 2.

1
* 1»KK__B* __»»«! .. ft
- 900
- 800
-700 x/
- 600

- 500
- 400

- 300

- 200




. JOO
_ 90
80
- 70
- 60
- 50
- 40

— 30
•* W

20


- 20 'm'

*
- 30

- 40
- 50
- 60
- 70
- 80
- 90
- 100




- 200
V
- 300
_ 400

- 500
- 600
- 700
- 800
- 900
L 1000

- 10
    4.9% H20 in stack gas.
                                                               CHART 6


                                     NOMOGRAPH FOR CALCULATING MOISTURE CONTENT FROM HIGH VOLUMES

-------
GROUP II - EXCESS AIR







     Knowledge about excess air in a combustion source



is necessary not only for use in nomographs such as



Chart 4, but it is also helpful for interfacing between



stack samplers and combustion experts.







     A.  Excess Air Versus Flue Gas Composition



         Let's say a source is burning a waste oil which



     is like pentane.  If a line is drawn  from pentane



     to 240 percent excess air on Chart 7, the nomograph



     says  the flue gas should have about 15.0 percent



     O2 and 4.2 percent COg.  Conversely,  if a line  is



     drawn from pentane to 15.0 percent O2,  it says  that



     there should be 4.2 percent CO2  and 240 percent excess



     air.  This Chart  is useful for calculating excess air,



     or for validating orsat data, or for  calculating CO2



     from  02 data.







     B.  Low Excess Air Versus Composition



         Chart 8  is the same as Chart 7, except it  is for



     lower excess air  and has a dry molecular weight line



     on it.  Some may  recognize this  as being similar to



     a chart published in "Atmospheric Emissions  from
                             P-13

-------
   1500-1
                 20
01
CO
I
H
    400-
300-
    200-
     100-
      50-
                19
               18
          17
                     —  3
            •10
                             Example:  Known:  240% excess air burning Pentane
                                       Answer:  15% O  & 4% CO  in flue gas
                    4 _ _
                       S
                       Q
                     m^m f
6   CM
   8
8  *

10
                        15
                        20
                                         Refuse, Bark
                                           and Wood
                                —  Methane

                                   Average Natural Gas

                                   Ethane
                                   Propane

                                   Pentane
                                   Gasoline
                                   #2 Fuel Oil
                                                       Bunker "C" Oil
                                                        (#6 Fuel Oil)

                                                     - Bituminous Coal
                                                    " T-Sub-bituminous & Lignite;
                                                     - Anthracite

                                                       Coke
                                CHART 7
            NOMOGRAPH FOR ESTIMATING FLUE GAS COMPOSITION,
                      EXCESS AIR OR TYPE OF FUEL
                                 P-14

-------
-o
i
171
                                                                       Example:  Known:  50% Excess Air
                                                                                 burning No. 6 oil
                                                                                 Answer:  7.2% 0  , 10.8% CO
                                                                                 and a dry molecular weight of 30
                                                                          4 METHANE

                                                                          AVERAGE
                                                                         NATURAL GAS'

                                                                            ETHANE  -
                                                                           PROPANE

                                                                            BUTANE
                                                                           PENTANE  ~
L GASOLINE
- KEROSENE
  NO.  2 FUEL OIL
- NO.  4 FUEL OIL
                                                                                    - NO. 5 FUEL OIL
                                                                        	 NO. 6 FUEL OIL

                                                                                     •BUNKER "C" OIL
                                                                           HIGH
                                                                         VOLATILE
                                                                        BITUMINOUS
                                                                      LOW VOLATILE .
                                                                       BITUMINOUS
                                                                    SEXIANTHRACITE

                                                                       ANTHRACITE
                                                                             COKE
 MEDIUM VOLATILE
    BITUMINOUS
                                                                                    •BARK & WOOD
                                                        CHART 8
                                NOMOGRAPH FOR ESTIMATING MOLECULAR WEIGHT OF DRY FLUE GAS

-------
Coal Combustion - An Inventory Guide", by W. S. Smith
           «-
and C. W. Gruber, P.U.S.  No. 999-AP-24.  Since then

the chart has been improved and the information in-

creased.




C.  Molecular Weight Versus Excess Air

    Chart 9 gives dry molecular weights for different

fuels and amounts of excess air.  Chart 10 can be

used to convert dry molecular weights to wet molecular

weights.
                      P-16

-------
                            EXAMPLE:  Lignite is burned at
                                      50% excess air
                                      Answer:  the dry molecular
                                      weight is 30.25
ai
H
   1500  -,
1000  -

 800
 700

 600
 500

 400  -
U)
S   300
    200  -
    100 -
     50  -
      0  -I
                      -  29.0
                      -  29.5
                   .-  30.0


                   -  30.5

                      31.
                      31.5
Bark,

Wood &

Refuse
 _  Methane

    Average Natural  Gas
    Ethane
    Propane

    Pentane
    Gasoline
    #2 Fuel


  -  Bunker "C Oil
4^   (#6 Fuel Oil)
  •  Bituminous Coal
 "P-Subbituminous &  Lignite
    Anthracite
  -  coke
                             CHART 9

        NOMOGRAPH FOR ESTIMATING DRY MOLECULAR WEIGHT FROM
                   EXCESS AIR AND TYPE OF FUEL
                          P-17

-------
                                EXAMPLE:   a dry molecular weight of
                                          30.25 in 10% moisture gas
                                          stream gives a 29 wet
                                          molecular weight
32  -i
30  -
28  -
26  -
24  ~
22  -
20  -
IB
— 28
                                                   Air

                                                   29
— 30
— 31
                      CHART 10

      NOMOGRAPH FOR ESTIMATING WET MOLECULAR

   HEIGHT FROM DRY MOLECULAR WEIGHT AND MOISTURE

                        P-18

-------
GROUP III - VOLUME AND VELOCITY








     Sizing nozzles, estimating Flow rates, and just chock-



ing data requires a decent handle on stack velocity or total



volumetric flow.








     A.  Characteristics of Coal-Fired Equipment



         Chart 11 is a very handy chart which was included



     in "Atmospheric Emissions from Coal Combustion - An



     Inventory Guide".  The volumes appear to be correct



     except those for stokers with control equipment,



     which reflect  the volume at maximum capacity.  As



     an example, we have a 100,000 pounds of steam per



     hour spreader  stoker fitted with draft-controlled



     (constant volume) multiple cyclones.  The chart



     would tell us  that the boiler input was about 120



     million Btu per hour, burning about 8000 pounds of



     coal per hour, it could generate about 10 megawatts,



     the stack gas  was about 28,000 scfm at 35 percent



     excess air, coal to steam efficiencies in the lower



     80 percent, stack gas temperatures about 500*F, and



     could be used  in a hospital or even as a large  in-



     dustrial boiler.  The important thing to note is



     that if this boiler is running at half load, the
                            P-19

-------
ro
o
CLASSFICATION
OF
BUILDING AND
PLANT
SIZE RANGES


1

| CHOW!- Si»ll IH8STIIU IITI ftOC

.
	 fcM»

1 	 1
	 1 	
ctowm-Niiic uniin STEM IIECIIIC CEIEUIIOI snuoi
B-uitf htUtllin llti Nicest SIf»i |

, 	 	 	 Jawfni-cHTiii tun*
U -UM lUTitiimuL.mw
^^^^^^^Bi 1", '.". ifil1; !'r,Taf?tffffSter^^M
ICmmt-ICMOLS. CMICMES. tULL CHLECIi. ««c 1
6W U- 1 to 4 ASytilu«?TT nm* 	 '

FIRING METHODS
RANGE OF
EQUIPMENT
SIZES
EFFLUENT




riLS.tte. 1











H rMIUEMEt CML FIIEO UllfJ 4 CfCLOIC full
1 Mill 91 TIMELIIC CUIf 1
1 MTCI COOLEO VIIU (1C SMTE 1

l,spif-sni
ilCI AUTMUTIC MCliCfAMl
SlltLE IETOII UIDEIFEEI SIOIEI
CUSSI (CUSSlI CltSSI 1 CLUI4 1
MII FIIEO iHirmr 1
LT 	 1 	
-. , i,
1 MO ISO TOO ISO |5o
COAL TO STEAM

EXCESS AIR,%

STACK GAS EFFLUET
clina16O*Ftlatni
at indicated
EMM Air
EQUIVALENT
UNIT CAPACITY
IM MEGAWATTS
91 I0.50O BTU/KW
BOILER OUTPUT 1
I.OOO Ib STEAM '
ptr HOUR at !
IDOOBTU /*> STEAM
BOILER INPUT
T 	 1 	 1 — '
JJ W U
T — n — n — i —
IN- M 15 H fl n 1
1 	 1 	 I—J—
ro i
•
1 	 1 	 1 	 1 	 ^~
i H » M r«
1 1 III! 1 1 1 1 1 III! 1 1
90 100 500 WOO
f
1 t


jl
1
III! 1 1 1 II Mil 1 till Illl
01 05 I 10 5 ' It
1 1
1 1
Ib. COAL ptr HOUR 1 I I I I Mllll | 1 1 I I I III

TOILER INPUT I
10 so 100 500 um
1 1
MILLION BTU ! | 1 1 1 M III 1 1 1 1 1 1 III
ptr HOUH 0, I}' 1.0 J 10
»«.-- TUmiK CUTE 	 1
i*un 01 OWFW curt
-,„ wr-wur«
CUSS5
	 1 i
SM
	 1 	

5Ti
' i i i
1 ' '
SOO 450 400
	 1 	 '
	 i-] 	 i 	
	 	 j 	 , 	
» >
MM II
1 1 	 .
5- M
1 M 1 1 III
UK IUOO j ' 5400C KKJJXXI
I
	 	
	 .
SM
1 	 1
1
1 — 	 _J
- 1 	 1
a i




IKS
-
	
900
1 	 : 	
I 	
0
1 	
1
1 1 1 1 1 III 1 1 1 Illl
30CJXC JOO>: iJW.MO KLOOO.OOO
1 1 1 1 1 llfl 1 1 1 1 1 Illl 1 1 1 M 1 III 1 1 1 M II
5 U X 100 500 iM SjOOO
(!
II 1 1 1 1 Mill 1 1 1 1 1 Illl 1 1 1 1 1 II
„
1 III
5JOO
m MO !u»o uoc tooo 50000
II Illl ll'lll 1 Mil Till 1 Mill
(MOO UiOOft IOILOOO WOJOO LOOO.OOO &400.000
1 t
1 1
1 1 1 Mill ,1 1 1 1 1 MII 1 Illl Illl 1 1 1 1 Ml
50 100 500 IjOOO SJOO ftjOOO SOMO
SPR'- SPREADER STOKER • •• «"»» • o«u«t«
                                    CHART 11
                                                                     •«LIt» I (KITH
             SUMMARY OF CHARACTERISTICS OF COAL-FIRING EQUIPMENT

-------
volume will be about the same, the excess air about



270 percent, and a gas temperature of about 200°F.



This sort of thing does not happen with pulverized



boilers with electrostatic precipitators.








B.  Volume Versus Heat Input



    Chart 12 is a more exacting chart which can cal-



culate the flow rate up a stack on a combustion sourco



if the heat input is known.  The data for this chart



is in an unpublished paper as of April 1973, called



"A Method of Calculating Power Plant Emission Rates",



by R. T. Shigehara, R. M. Neulicht, and W. S. Smith.



As can be seen from the chart, the heat input need



not be measured if the volumetric flow rate and ex-



cess air is known.








C.  Pitot Velocity Readings



    The novice often finds it difficult to relate



pitot tube readings into actual velocities.  By



using Chart 13, one can quickly relate an "S" type



pitot tube reading into a velocity which is usually



near the actual value.  This chart also has a scale



so one can correct the velocity to standard (STP)



conditions which are 68°F and 29.92 inches of mer-




cury pressure.
                       P-21

-------






Oil -


—




Iw
-o
f\3





Anthracite -









REF
- Gas 100-1
90-4
j
80-j
1
70-]
^""^-^ H 60|
w "SO-H-
W |








x 1
W 40 H
<*> I
30-4
- Bituminous 20 ~"1






— 	 _




and Lignite 11
1
10 -\\

0 -1
r- 200
- 190
- 180 o
m
-170 Q
<
w
>- 160 D
O
-150 z
W
-1^0— ^

w
>- 130 u
fe
- 120 H
DQ
lllO S

- 100
.
- 90

                                       Bituminous
                                       and Lignite
                                               Gas
                                                         i-  Anthracite
                                                         - Oil
                            EXAMPLE:  1 million BTU/hour of oil
                                      is burned at 50% Excess Air.
                                      How much gas volume is produced?

                                      ANSWER: 14,200 cf/hr. 9 70°F  dry
          CHART 12
VOLUME VERSUS HEAT INPUT CHART

-------
EXAMPLE:  Stack temperature 500°F
          AP = 0.5 inches HO

          Answer:  Actual approximate Velocity = 54 ft/sec
                   Approximate velocity at STP* = 30 ft/sec
                                                        100 -t-6000
 fa
 o
> 2000

•o
«1000
o

u  500
o
o


I    0
to
H


|


(0
              _o
                                                         90 -
                                                         80 -
                                                         70 -
                                                     U  60 —
                                                     W
                                                              -5000
             — 1000  O
             -1500  3
                     o
                     *H

             t-2000  fa
                                                              -4000
                                                     IL-
                                                     bT 50 H-3000
                                                         40 -
                                                         30
                                                         20 -
                                                        .° 0
                                                              _2000
                                                              -1000
                                 CHART 13

                      Approximate velocity Nomograph

             Assumes Type "S" pitot tube used at 1 ATM in Air

                           STP » 68°F & 29.92 inches of mercury
z
H


1
U
                                                                      8
                             P-23

-------
    Chart 11 corrects for the errors in Chart. 13, not



only for the actual velocity but also  Tor velocity



that has been corrected to STP.  The example given



is a very extreme case which could exist after a



venturi scrubber, but before a fan (high moisture



gives low molecular weights).  This extreme example



was given in order that you not implicitly trust



Chart 13,  especially under extreme conditions.
                     P-24

-------
H
CO
fa M
05 0
^ P
rt!
64 w
l&
|o
O
u

1.0-
-
0.9—
-
0.8—
0.7—
o.e-
0.5—






^v


                     M
                      w
                              10-,
                              15 -
- -20—
                              25 —
                              30 —
                              35 -
                                    W
                                    X
                                    u
                                    2
                                    QU
                                    to
         O
         WJ
         s
                               — 0.9

                                     IX
                                     o


                               — 1.0 os H
                                                                 (M W

                                                                 z
— 1.5



i- 2.0

^ 2.5
                                                                   u
                                     o
                                     u
EXAMPLE:  From Chart 13


  Approx. Actual Velocity 54 ft./sec.

  Approx. STP Velocity 30 ft./sec.

  Actual Molecular Weight  (MW> =  25

  Actual Stack Pressure = 20 inches  Hg


  ANSWER:  Actual Velocity  1.32 x 54 =  71  ft./sec.

           STP Velocity 0.87 x 30 =  26  ft./sec.
                              CHART  14


                 CORRECTION FACTORS FOR VELOCITY CHART
                                   P-25

-------
                                                                              IN
                                                                       ounce

                                                                      /JL.AMPLINO
    MO -
    120
   100
    80  -
    60
CT)
    40  ~
     0  -

uu
O

f
Ul
13
a
a
5
uu
l~

oe
Ul
H-
Ul
s






TIME ONE CUBIC FOOT WITH 1
ORIFICE MGTSR AH = 2.00 |

en
X
.c

U4
§ ,
W I
Ul t
Of /
°- /
/.
- r
Ite /
ut r~
3
O 1
o- f—
< /
1
                                                  35
                                             20
                                                            O

                                                            CL
                                                                                                       -  2.4
                                                                                                       -  2.2
                                                                                                          2.0   O
                                                                                                                p<
                                                                                                               I
                                                                                                               ©
                                                                                                          1.8   X
                                                                                                               O
                                                                                                       -  1.6
                                                                                                       -  1.4
                                                                                                       - 1.2
                                                                                                               01
                                                                                                               5
                                                                              ce
                                                                              O
                                                                                                       -  1.0
     Date:

     Me toi1  Box
CAI.IRRATION  CMIXK - I-PA TRAIN METER BOX
Given  A H,:
          A
Graph  A Il,:

-------
 SLIDE 156-0
                                                NOTES
STACK SAMPLING NOMOGRAPHS
        FOR FIELD USE
SLIDE  156-1
100 —,
 90 _:
 80 _:
Example:  Wet Bulb - 160°F
         Dry Bulb - 230°F
Answer:   30% H2O
  0 -3
                                _ 1000
                                _ 900
               chart 2
                               P-27

-------
 SLIDE 156-2
                                                        NOTES
          r. i
P , Inch Bg
 20-,
                                                          V ,  ft5
Example:  R. = 30 in. Hg
          Tm = 100°F
           v. = 100 ml H2O
          Vm = 100 ft3
          4.9% H2O
                                                      4OO

                                                      500
                                                      600
                                                      700
                                                      BOO
                                                      900
                                                      1000
Answer
                                      1O
                         chart 6
                                      P-29

-------
SLIDE  156-3
                                                 NOTES
  Example:  Known: 50% Excess Air

           Burning No. 6 Oil

  Answer   7.2% O>, 10.8% Ca2
                    I
ai w*«zijjui wi ou
/ '?9-4 METHANE -
6-;j / AVERAGE
3 1 NATURAL GAS"
y / ETHANE -
'V / '9 c PROPANE -
i
-3 J BUTANE -
« J' / 2 PENTANE -
J / 5
' -j I !
, / / £
loj] A G
i / g
r3ss++*fcf "£"'""""
1 L -° *
^ / /
/ ^ HIGH
/A VOLATILE
BITUMINOUS
LOW VOLATILE .
.., BITUMINOUS
r " SEhtlANTHRACITE
A
t
ANTHRACITE
*i.O COKE






- GASOLINE
- NO. 2 FUEL OIL
- NO. 4 FUEL OIL
- NO. 5 FUEL OIL
•- BO. 6 FUEL OIL
I- BUNKER "C" OIL
]

MEDIUM VOLATILE
> BITUMINOUS

• BARK £ WOOD
•
                                                        a
                                                        H«


                                                        8,
                                                        a
                                                        M


                                                        8
                        charts
                                    P-31

-------