Methods
Methods
 Measured parameters:
           o The purpose of the method is to provide guidance for the selection of sampling
             ports and traverse points at which sampling for air pollutants will be performed.
           o Two procedures are presented: a simplified procedure, and an alternative
             procedure.
           o The magnitude of cyclonic flow of effluent gas in a stack or duct is the only
             parameter quantitatively measured in the simplified procedure.
 Applicability:
           o This method is applicable to gas streams flowing in ducts, stacks and flues.
           o This method cannot be used when:
           o The simplified procedure cannot be used when the measurement site is less than
             two stack or duct diameters downstream or less than a half diameter upstream
             from a flow disturbance.
Summary of Method
      Sampling and/or velocity measurements are performed at a site located at least eight
       stack or duct diameters downstream and two diameters upstream from any flow
       disturbance such as 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.
Determining the Number of Traverse Points
 Particulate Traverses
          o When the eight- and two-diameter criterion can be met, the minimum number of
            traverse points shall be:
                     Twelve (12), for circular or rectangular stacks with diameter (or equivalent
                      diameters) greater than 0.61 m
                     Eight (8), for circular stacks with diameters between 0.30 and 0.61 m
                     Nine (9), for rectangular stacks with equivalent diameters between 0.30
                      and 0.61 m
                     When any of the traverse points fall within 2.5 cm of the stack walls,
                      relocate them away from the stack walls to a distance of 2.5 cm or 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.
                     Any “adjusted” points should be relocated away from the stack walls to a
                      distance of 1.3 cm or a distance equal to the nozzle inside diameter,
                      whichever is larger.
                     DETERMINATION OF STACK GAS VELOCITY
                          AND VOLUMETRIC FLOWRATE
                                  (Method 2)
        This method is applicable for the determination of the average velocity and the
volumetric flow rate of a gas stream using an S type pitot tube. This method is not applicable at
measurement sites that fail to meet the criteria of Method 1. Also, the method cannot be used for
direct measurement in cyclonic or swirling gas streams.
      Made of metal tubing with an external diameter between 0.48 and 0.95 cm.
      There shall be an equal distance from the base of each leg of the pitot to its face-opening
       plane.
      The face openings shall be aligned; however slight misalignments are permissible.
      The pitot shall have a known coefficient. If a baseline coefficient value of 0.84 is
       assigned to the pitot tube and upon inspection does not meet the criteria, that pitot tube
       will not be used.
Procedure
      A pretest leak check of the pitot tube and manometer will be conducted.
      The manometer will be leveled and zeroed prior to use as well as periodically checked
       during the test.
      The velocity head and temperature will be measured at each traverse point specified by
       Method 1.
      The static pressure in the stack will be measured during the test as well as the
       atmospheric pressure.
                     GAS ANALYSIS FOR THE DETERMINATION OF
                            DRY MOLECULAR WEIGHT
                                    (Method 3)
       This method is applicable for the determination of CO2 and O2 concentrations and dry
molecular weight of a sample from an effluent gas stream of a fossil-fuel combustion process
and other process. The sample is taken in a flexible bag and analyzed in an orsat analyzer.
        A gas sample is extracted from a stack by either a single point integrated or multi-point
integrated sampling. The gas sample is analyzed for percent CO2, O2, and if necessary CO.
Apparatus
 Pump
            o A leak free diaphragm-type pump, or its equivalent, to transport the sample to the
              flexible bag.
 Rate Meter
 Flexible Bag
            o Any leak free plastic (Tedlar, Teflon, Mylar, etc.) bag or equivalent having a
              capacity consistent with the selected flow rate and sample time
 Pressure Gauge
            o A water filled U-tube manometer, or equivalent, of about 30 cm for the bag leak
              check.
 Vacuum Gauge
            o The sampling point will be at the centroid of the cross section of the duct.
            o The bag will be leak checked.
            o The train will be leak checked.
            o The sampling system will be purged prior to connecting the sample bag.
            o The sample will be taken at a constant rate simultaneous with, and for the same
              total length of time as, each pollutant emission rate determination.
            o At least 30 L of sample will be taken.
   o Within 8 hours of collection, the sample will be analyzed for percent CO2 and percent O2
     using an orsat analyzer.
   o The orsat analyzer will be leak checked prior to any sample analysis.
   o The analysis and calculations for each sample will be repeated until any three analysis
     differ from their mean by no more than 0.3 g/gmol.
                      DETERMINATION OF MOISTURE CONTENT
                               IN STACK GASES
                                   (Method 4)
Apparatus
 Probe
 Condenser
            o The condenser will consist of four impingers connected in series with ground
              glass, leak-free fittings or any similar non-contaminating fittings.
            o The first, third and fourth impingers will be of the Greenburg-Smith design,
              modified by replacing the tip with a 1.3 cm ID glass tube extending to about 1.3
              cm from the bottom of the flask.
            o The second impinger will be of the Greenburg-Smith design with the standard tip.
            o The first two impingers will contain known volumes of water, the third will be
              empty, and the fourth will contain a known weight of 6 to 16 mesh indicating type
              silica gel, or equivalent desiccant.
 Cooling System
            o An ice bath container and crushed ice, or equivalent, are used to aid in condensing
              moisture.
 Metering System
            o This system will include a vacuum gauge, leak-free pump, thermometers capable
              of measuring temperature to within 3°C and a dry gas meter capable of measuring
              volume to within 2 percent.
      Barometer
            o These items are used to measure the condensed water in the impingers and silica
              gel to within 1 mL or 0.5 g.
            o Graduated cylinders will have subdivisions no greater than 2 mL.
            o The balance will be capable of weighing to the nearest 0.5 g or less.
Procedure
      A minimum total gas volume of 0.60 scm will be collected, at a rate no greater than 0.021
       m3/min.
      The moisture determination will be conducted simultaneous with, and for the same total
       length of time as, the pollutant emission rate run.
      The probe and filter (if applicable) will be heated to about 120 °C, to prevent water
       condensation ahead of the condenser.
      After the train is heated and the impingers iced down, a leak check will be performed
       with an acceptable rate of 4 percent the average sampling rate or 0.02 cfm, whichever is
       less.
      During the run, the sampling rate maintained within 10 percent of constant rate.
      The dry gas meter volume will be recorded at the beginning and end of each sampling
       time increment and whenever sampling is halted.
      More ice will be added, if necessary, to maintain a temperature of less than 20°C at the
       silica gel outlet.
      When the run is completed, a post leak check is performed, with the same acceptance
       criteria as for the pre-test leak check.
      The volume and weight of condensed moisture is measured to the nearest mL and 0.5 g,
       respectively.
    In gas streams that contain water droplets, this method may produce a positive bias.
    If this is suspected for this source, either a wet bulb dry bulb and psychometric chart
     (correcting for stack pressure) or saturation and vapor pressure table determination will
     be conducted simultaneously with the moisture sample train.
             DETERMINATION OF PARTICULATE MATTER EMISSIONS
                       FROM STATIONARY SOURCES
                                (Method 5)
Summary of Method
          Particulate matter is withdrawn isokinetically from the source and collected on a glass
fiber filter maintained at a temperature of 120 ± 14°C or such other temperature as specified by
an applicable subpart of the standards or approved by the Administrator for a particular
application. The PM mass, which includes any material that condenses at or above the filtration
temperature, is determined gravimetrically after the removal of uncombined water.
Sample Collection
      Sampling Train
Pretest Preparation
   o Check the filters visually against light for irregularities, flaws, or pinhole leaks.
   o Label filters of the proper diameter on the back side near the edge using numbering
     machine ink.
   o As an alternative, label the shipping containers (glass, polystyrene or polyethylene petri
     dishes), and keep each filter in its identified container at all times except during sampling.
   o Desiccate the filters at 20 ± 5.6°C and ambient pressure for at least 24 hours.
   o Weigh each filter at intervals of at least 6 hours to a constant weight.
   o Record results to the nearest 0.1 mg.
   o During each weighing, the period for which the filter is exposed to the laboratory
     atmosphere shall be less than 2 minutes.
   o Alternatively, the filters may be oven dried at 105°C for 2 to 3 hours, desiccated for 2
     hours, and weighed.
Preliminary Determination
   o Select the sampling site and the minimum number of sampling points
   o Determine the stack pressure, temperature and the range of velocity heads; it is
     recommended that a leak check of the pitot lines be performed.
   o Determine the moisture content for the purpose of making isokinetic sampling rate
     settings.
   o Determine the stack dry gas molecular weight
   o 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.
   o During the run, do not change the nozzle size.
   o Ensure that the proper differential pressure gauge is chosen for the range of velocity
     heads encountered.
   o Select a suitable probe liner and probe length such that all traverse points can be sampled.
   o For large stacks, consider sampling from opposite sides of the stack to reduce the
     required probe length.
   o 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
                     Sampling time per point is not less than 2 minutes (or some greater time
                      interval as specified by the Administrator)
                     Sample volume taken (corrected to standard conditions) will exceed the
                      required minimum total gas sample volume.
   o The sampling time at each point shall be the same. 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.
   o In some circumstances 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.
      During preparation and assembly of the sampling train, keep all openings where
       contamination can occur covered until just prior to assembly or until assembly 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 pre-weighed silica gel from its container to
       the fourth impinger.
      More silica 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 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 to prevent the
       sample gas stream from circumventing the filter.
      Check the filter for tears after assembly is completed.
      When the glass probe liners are used, install the selected nozzle using a Viton A O-ring
       when stack temperatures are less than 260°C or a heat-resistant string gasket when
       temperatures are higher.
      Other connecting systems using either 316 stainless steel or Teflon ferrules may be used.
      When metal liners are used, install the nozzle as discussed 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.
      Set up the train ensuring that the connections are leak tight.
      A glass cyclone may be used between the probe and filter holder when the total
       particulate catch is expected to exceed 100 mg or when water droplets are present in the
       stack gas.
      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.
      A pretest leak check of the sampling train is recommended, but not required.
      If the pretest leak check is conducted, the following procedure should be used.
   After the sampling train has been assembled, turn on and set the filter and probe heating
    systems to the desired operating temperatures.
   Allow time for the temperatures to stabilize.
   If a Viton A O-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 (15 in.) Hg vacuum.
   If a heat-resistant 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 (15 in.) Hg vacuum.
   Then connect the probe to the train, and leak-check at approximately 25 mm (1 in.) Hg
    vacuum; alternatively, the probe may be leak-checked with the rest of the sampling train,
    in one step, at 380 mm (15 in.) Hg vacuum.
   Leakage rates in excess of 4 percent of the average sampling rate or 0.00057 m3 /min
    (0.020 cfm), whichever is less, are unacceptable.
   Start the pump with the bypass valve fully open and the 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 the direction of the bypass valve, as 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 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 the silica gel from being entrained backward into the third impinger.
      During the sampling run, maintain an isokinetic sampling rate (within 10 percent of true
       isokinetic unless otherwise specified by the Administrator) and a sample gas temperature
       through the filter 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.
      When the stack is under significant negative pressure (i.e., 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, 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 to maintain the sample gas temperature exiting the filter; 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 the 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.
      The total PM weight shall include the summation of the filter assembly catches.
      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.
    At the end of the sample run, close the coarse adjust valve, remove the probe and nozzle
       from the stack, turn off the pump, record the final DGM meter reading, and conduct a
       post-test leak check.
       Calculate percent isokinetic to determine whether the run was valid or another test run
should be made. If there was difficulty in maintaining isokinetic rates because of source
conditions, consult with the Administrator for possible variance on the isokinetic rates.
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 PM near the tip of the probe
       nozzle, and place a cap over it to prevent losing or gaining PM.
      Do not cap off the probe tip tightly while the sampling train is cooling down. This would
       create a vacuum in the filter holder, thereby 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 and cap the open outlet of the probe. Be careful not to lose any condensate that
       might be present. Cap the filter inlet where the probe was fastened.
   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.
   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.
 Inspect the train prior to and during disassembly and note any abnormal conditions.
Container 1
         Carefully remove the filter from the filter holder and place it in its identified petri
            dish container.
           Use a pair of tweezers and/or clean disposable surgical gloves to handle the filter.
           If it is necessary to fold the filter, do so such that the PM cake is inside the fold.
           Using a dry Nylon bristle brush and/or a sharp-edged blade, carefully transfer to
            the petri dish any PM and/or filter fibers that adhere to the filter holder gasket.
           Seal the container.
Container 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 PM 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.
           Deionized distilled water may be used instead of acetone when approved by the
            Administrator and shall be used when specified by the Administrator.
           Perform the acetone rinse as follows:
Container 3
      Note the color of the indicating silica gel to determine whether 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 or other liquids to transfer the silica gel.
Sample Transport
         Whenever possible, containers should be shipped in such a way that they remain upright
at all times.