EPA-650/4-74-005-d
     GUIDELINES  FOR DEVELOPMENT
OF A  QUALITY  ASSURANCE PROGRAM:
     VOLUME  IV - DETERMINATION
      OF  PARTICULATE  EMISSIONS
     FROM STATIONARY  SOURCES
                     by

           Franklin Smith and Denny E. Wagoner

               Research Triangle Institute
             Research Triangle Park, N. C.
                Contract No. 68-02-1234
                 ROAP No. 26BGC
              Program Element No. 1HA327
          EPA Project Officer: Steven M. Bromberg

     Quality Assurance and Environmental Monitoring Laboratory
           National Environmental Research Center
         Research Triangle Park, North Carolina 27711
                   Prepared for

          OFFICE OF RESEARCH AND DEVELOPMENT
         U.S. ENVIRONMENTAL PROTECTION AGENCY
               WASHINGTON, D . C.  20460

                   August 1974

-------
                       EPA REVIEW NOTICE
This report has been reviewed by the Environmental  Monitoring and
Support Laboratory, Research Triangle Park, North Carolina, of the
U. S. Environmental Protection Agency and aoproved for publication.
Approval does not signify that the contents necessarily reflect
the views and policies of the Environmental Protection Agency, nor
does mention of trade names or commercial products constitute en-
dorsement or recommendation for use.
                                11

-------
                           TABLE OF CONTENTS

SECTION                                                             PAGE

   I                         INTRODUCTION                             1

  II                       OPERATIONS WNUAL                          5
        2.0  GENERAL                                                  6
        2.1  EQUIPMENT SELECTION                                     10
        2.2  EQUIPMENT CALIBRATION                                   19
        2.3  PRESAMPLING PREPARATION                                 26
        2.4  ON-SITE MEASUREMENTS                                    40
        2.5  POSTSAMPLING OPERATIONS (Base Laboratory)                56
 III               MANUAL FOR FIELD TEAM SUPERVISOR                  65
        3.0  GENERAL                                                 66
        3.1  ASSESSMENT OF DATA                                      67
        3.2  SUGGESTED PERFORMANCE CRITERIA                          70
        3.3  COLLECTION AND ANALYSIS OF INFORMATION                  70
             TO IDENTIFY TROUBLE
  IV          MANUAL FOR MANAGER OF GROUPS OF FIELD TEAMS            83
        4.0  GENERAL                                                 84
        4.1  FUNCTIONAL ANALYSIS OF TEST METHOD                      88
        4.2  ACTION OPTIONS                                         103
        4.3  PROCEDURES FOR PERFORMING A QUALITY AUDIT               111
        4.4  DATA QUALITY ASSESSMENT                                118
REFERENCES                                                          132
APPENDIX A       METHOD 5 (AS REVISED IN JANUARY 1975)               136
APPENDIX B           ILLUSTRATED USE OF NOFDGRAPHS                  168
APPENDIX C           ILLUSTRATED AUDIT PROCEDURES                   174
APPENDIX D                GLOSSARY OF SYMBOLS                       ] 79
APPENDIX E                 GLOSSARY OF TERMS                        181
APPENDIX F                CONVERSION FACTORS                        182

                                     iii

-------
                           LIST OF ILLUSTRATIONS

FIGURE NO.                                                          PAGE
     1      Operational flow chart of the measurement process.         7
     2      Dry gas meter and orifice meter calibration and          23
            calculation form.
     3      Particulate measurement equipment checklist.             29
     4      Sample data form for particulate emissions               ^2
            determinations.
     5      Sample control chart for the range,  R,  of PMR            ^9
            replicates.
     6      Sample control chart for the range,  R,  of percent        °0
            of isokinetic sampling.
     7      Sample control chart for the average percent of          81
            isokinetic sampling.
     8      Summary of data quality assurance program.               87
     9      Most important variables in the determination of PMR.
    10      Added cost vs. precision for selected action options
            for incinerator sources (m  = 100 mg and %CCL = 6.0).
    11      Sample form for recording audit data.
    12      Example illustrating p < 0.10 and satisfactory data     123
            quality.
    13      Example illustrating p > 0.10 and unsatisfactory data   123
            quality.
    14      Flow chart of the audit level selection process.        128
    15      Average cost vs. audit level (n).                       131
    Al      Nomograph for correction factor, C.                      169
    A2      Use of the nomograph in selecting nozzle size and       171
            setting K factor.
    A3      Nomograph operation to obtain desired orifice meter     173
            settings.
                                      IV

-------
                            LIST OF TABLES
TABLE NO.
PAGE
    1     Suggested performance criteria
    2     Means and variabilities of parameters affecting V
    3     Means and variabilities of parameters in determining
          the sample gas volume
    4     Summary of results of variance analysis
    5     Comparison of action options based on CV{PMR}for
          C  adjusted to 12 percent C0~ (incinerator sources)
    6     Particulate emission determination checklist to be
          used by auditor
    7     Computation of mean difference,  d, and standard
          deviation of differences, s,
                                     d
    8     Sample plan constants, k for P{not detecting a lot
          with proportion p outside limits L and U} ^0.1
 71
 98
101

105
111

113

124

124

-------
                               ABSTRACT

     Guidelines for the quality control of measurements of particulate
emissions from stationary sources by the Federal reference method are
presented.  These include:
     1.   Good operating practices,
     2.   Directions on how to assess performance and qualify data,
     3.   Directions on how to identify trouble and improve data quality,
     4.   Directions to permit design of auditing activities.
     The document is not a research report.  It is designed for use by
operating personnel.
     This work was submitted in partial fulfillment of Contract Durham
68-02-1234 by Research Triangle Institute under the sponsorship of the
Environmental Protection Agency.  Work was completed as of February 1975.
                                      vi

-------
 SECTION I
MRODUCTION

-------
SECTION I                   MRODUCTION

     This document presents guidelines for developing a quality assurance
program for Method 5, Determination of Particulate Emissions from Sta-
tionary Sources.  This method was published by the Environmental Protec-
tion Agency in the Federal Register, December 23, 1971.  The method was
revised in January 1975 and the revised method* is reproduced as Appendix
A of this report for convenience of reference.
     This document is divided into four sections:
     Section I, Introduction,.  The introduction lists the overall objec-
tives of a quality assurance program and delineates the program components
necessary to accomplish the given objectives.
     Section II, Operations Manual.  This manual sets forth recommended
operating procedures to insure the collection of data of high quality
and instructions for performing quality control checks designed to give an
indication or warning that invalid data or data of poor quality are being
collected, allowing for corrective action to be taken before future
measurements are made.
     Section III, Manual for Field Team Supervisor.  This manual contains
directions for assessing data quality on an intralaboratory basis and for
collecting the information necessary to detect and/or identify trouble.
     Section IV, Manual for Manager of Groups of Field Teams.  This manual
presents information relative to the test method (a functional analysis
to identify the important operations variables and factors, and statistical
properties of and procedures for carrying out auditing procedures for an
independent assessment of data quality).
     The objectives of this quality assurance program for Method 5 are to:
     1.  Identify and where possible eliminate systematic errors (biases)
and maintain precision within acceptable limits in the measurement process,
     2.  Provide routine indications for operating purposes of satis-
factory performance of personnel and/or equipment,
     3.  Provide for prompt detection and correction of conditions that
contribute to the collection of poor quality data,
* The revised method became a.vailable just prior to the printing of this
  document.  Consequently, there are numerous duplications of the material
  as given in Appendix A and in the Operations Manual of this document.

-------
     4.  Collect and supply information necessary to describe the quality
of the data.
To accomplish the above objectives, a quality assurance program must con-
tain the following components:
     1.  Recommended operating procedures,
     2.  Routine training of personnel and evaluation of performance of
personnel and equipment,
     3.  Routine monitoring of the variables and parameters that may
have a significant effect on data quality,
     4.  Development of statements and evidence to qualify data and
detect defects,
     5.  Action strategies to increase the level of precision/accuracy
in the reported data.
Component 2 above will be treated for all the methods in the final report
of this contract.  All other components are treated in this document.
     Implementation of a properly designed quality assurance program
should enable measurement teams to achieve and maintain an acceptable
level of precision and accuracy in their stack gas-composition measure-
ments.  It will also allow a team to report an estimate of the precision
of its measurements for each source emissions test.
     Variability in emission data derived from multiple tests conducted
at different times includes components of variation from:
     1.  Process conditions,
     2.  Equipment and personnel variation in field procedures,
     3.  Equipment and personnel variation in the laboratory.
In many instances time variations in source output may be the most signifi-
cant factor in the total variability.  This component of variation is
minimized by knowing the time characteristics of the source output and
maintaining isokinetic sampling conditions.  The sampling period should
span at least one complete output cycle, if an average over the cycle is
desired.  If the cycle is too long and an average value is desired,
either the sample collection should be made during a portion of the cycle
representative of the cycle average, or multiple samples should be col-
lected and averaged.

-------
     Quality assurance guidelines for Method 5 as presented here are
designed to insure the collection of data of acceptable quality by preven-
tion, detection, and quantification of equipment and personnel variations
in both the field and the laboratory through:
     1.  Recommended operating procedures as a preventive measure,
     2.  Quality control checks for rapid detection of undesirable
performance,
     3.  A quality audit to independently verify the quality of the
data.
     The scope of this document has been purposely limited to that of a
field and laboratory document.  Additional background information is
contained in the final report under this contract.

-------
    SECTION II
OPERATIONS MANUAL

-------
SECTION II                OPERATIONS MANUAL
                                        »
2.0  GENERAL

     This manual sets forth recommended procedures for determination of
particulate emissions from stationary sources according to Method 5.
(Method 5 as revised by EPA is included as Appendix A of this document.)
Quality-control procedures and checks are designed to give an indica-
tion or warning as part of the operating procedures and are to be per-
formed by the operator on a routine basis.  In addition, the performance
of special quality control procedures and/or checks as prescribed by
the supervisor for assurance of data quality may be required of the
operator on special occasions.
     The sequence of operations to be performed for each field test is
given in Figure 1.  Each operation or step in the method is identified
by a block.  Quality checkpoints in the measurement process, for which
appropriate quality-control limits are assigned, are represented by
blocks enclosed by heavy lines.  Other quality checkpoints involve go/no-go
checks and/or subjective judgments by the test team members with proper
guidelines for decisionmaking spelled out in the procedures.
     The precision/accuracy of data obtained from this method depends
upon equipment performance and on the proficiency and conscientiousness
with which the operator performs his various tasks.  From equipment checks
through on-site measurements, calculations, and data reporting, this method
is susceptible to a variety of errors.  Detailed instructions are given
for minimizing or controlling equipment error, and procedures are recom-
mended in order to minimize operator error.  Before using this document,
the operator should study Method 5 as reproduced in Appendix A in detail.
In addition, the quality assurance documents of this series for Methods
2, 3, and 4 (refs. 1, 2 and 3) should be read and followed.  Also, these
methods, i.e., methods 2, 3 and 4, have been extensively revised by the
Environmental Protection Agency in an effort to improve the quality of
the data obtained by field teams using these methods.  The methods as

-------
EflJIPMENT SELECTION
1.  SELECT EQUIPMENT ACCORDING TO THE
    GUIDELINES GIVEN IN SUBSECTION 2.1
    FOR THE SOURCE TO BE TESTED.
EQUIPMENT CALIBRATION

2.  CALIBRATE EQUIPMENT ACCORDING TO
    SUBSECTION 2.2.
PRESAMPLING PREPARATION
3.
4.
OBTAIN PROCESS DATA, SELECT/PREPARE
SAMPLING SITE, DETERMINE LOGISTICS
FOR PLACING EQUIPMENT ON-SITE, AND
DETERMINE STACK CONDITIONS Ts, Ps
B  , AND Ms.  (SUBSECTION 2.3.1)
CHECK OUT SAMPLING TRAIN AND RELATED
COMPONENTS. (SUBSECTION 2.3.2)
5.
PACKAGE AND SHIP EQUIPMENT.
(SUBSECTION 2.3.3)
Off SITE MEASUREMENTS

6.  MOVEMENT OF EQUIPMENT TO SAMPLING
    SITE AND SAMPLE RECOVERY AREA.
    (SUBSECTION 2.4.1)
                                                    EQUIPMENT
                                                    SELECTION
                                                    EQUIPMENT
                                                   CALIBRATION
                                                   PRELIMINARY
                                                   SITE VISIT
                                                   (OPTIONAL)
                                                    APPARATUS
                                                      CHECK
                                                     PACKAGE
                                                    EQUIPMENT
                                                       FOR
                                                    SHIPMENT
                                                TRANSPORT
                                                EQUIPMENT
                                                 TO SITE
      Figure 1.   Operational flow chart  of  the  measurement  process,

-------
10.
11
12.
13.
     PRELIMINARY MEASUREMENTS  AND SETUP
     WILL INCLUDE DUCT MEASUREMENT,
     PERCENT H20, MOLECULAR WEIGHT (Ms),
     AND SAMPLE BOX LOGISTICS.
     (SUBSECTION 2.4.2)
     DETERMINATION OF MAXIMUM AND MINIMUM
     AP AND STACK GAS TEMPERATURE.
     (SUBSECTION 2.4.2.5)
                                               PRELIMINARY
                                              MEASUREMENTS
                                                AND SETUP
                                                VELOCITY
                                                TRAVERSE
                                                AND STACK
                                               TEMPERATURE
     SET NOMOGRAPH UTILIZING THE PRELIMINARY
     STACK GAS PARAMETERS  [APPENDIX B].
                                                        SET
                                                     NOMOGRAPH
ASSEMBLE AND LEAK CHECK THE SAMPLING
TRAIN.  (SUBSECTIONS 2.4.3.3 THROUGH
2.4.3.6)
10
COLLECT A MINIMUM SAMPLE VOLUME OF 1.7 m3
60 FT3.  MAINTAIN ISOKINETIC CONDITIONS
DURING SAMPLING.  (SUBSECTION 2.4.3.7)
                                                   ASSEMBLE  AND
                                                    LEAK-CHECK
                                                     SAMPLING
                                                       TRAIN
11
                                                      COLLECT
                                                      SAMPLE
PERFORM FINAL LEAK CHECK OF THE ENTIRE
SAMPLING TRAIN.  (SUBSECTION 2.4.3.7(7))
12
                                                    LEAK-CHECK
                                                     SAMPLING
                                                       TRAIN
OBTAIN SAMPLE FROM FILTER HOLDER, PROBE
AND NOZZLE.  MEASURE TOTAL CONDENSATE
(IMPINGER VOLUME AND SILICA GEL WEIGHT
GAIN).  (SUBSECTION 2.4.4)
13
                                                      SAMPLE
                                                     RECOVERY
 Figure 1.  Operational flow chart of  the measurement process  (continued),

-------
14.
15.
 VALIDATE THE DATA BY CHECKING ALL
 DATA SHEETS FOR COMPLETENESS.  COMPARE
 MEASURED VALUES OF Vs, BWs, AND Ms
 WITH THEORETICAL VALUES.
 (SUBSECTION 2.4.6)
DISASSEMBLE AND INSPECT EQUIPMENT FOR
DAMAGE SUSTAINED BUT NOT DETECTED
DURING SAMPLING (SUBSECTION 2.4.6)
16.
PACKAGE EQUIPMENT FOR RETURN TRIP TO
BASE LABORATORY.
(SUBSECTION 2.4.6)
POSTSAMPLIIfi OPERATIONS
17.
DESICCATE FILTERS AND CONSTANT WEIGH
TO + 0.5 mg.  RECORD WEIGHT GAIN TO
THE NEAREST 0.1 mg.  (SUBSECTION 2.5.2)
18.
19.
20.
TRANSFER ACETONE WASHING TO TARED
BEAKER, EVAPORATE AT AMBIENT
CONDITIONS, DESICCATE TO A CONSTANT
WEIGHT AND RECORD DATA TO THE
NEAREST 0.1 mg.  (SUBSECTION 2.5.2)
PERFORM NECESSARY CALCULATIONS TO
OBTAIN PARTICULATE CONCENTRATION,
VOLUMETRIC FLOW RATE, AND PERCENT
ISOKINETIC VARIATION.
(SUBSECTION 2.5.3)
FORWARD THE DATA FOR FURTHER INTERNAL
REVIEW OR TO THE USER.
14
                                                       DATA
                                                    VALIDATION
15
                                                    DISASSEMBLE
                                                     AND CHECK
                                                     EQUIPMENT
16
                                                      PACKAGE
                                                     EQUIPMENT
                                                   FOR SHIPMENT
17
                                                    EQUILIBRATE
                                                   AND CONSTANT
                                                   WEIGH FILTERS
18
                                                   EVAPORATE AND
                                                    EQUILIBRATE
                                                    PROBE WASH
                                                  CONSTANT WEIGH
19
                                                      PERFORM
                                                   CALCULATIONS
20
                                                      REPORT
                                                       DATA
 Figure 1.   Operational flow chart of  the measurement process  (continued)

-------
revised are contained in the Final Report under this contract (ref 4).
The revised methods should be followed in future field tests.

2.1  EQUIPMENT SELECTION

     Specifications, design features, and acceptance criteria for the
equipment and reagents used in measuring particulate emissions are given
in this section.  A corresponding schematic of an assembled particulate
sampling train with all components identified is shown in Figure 5-1 of
Appendix A.  The schematic will aid in the comprehension of the material
covered in this section which will insure proper selection of equipment
and, finally, the collection of high quality data.  A listing of the
required apparatus and reagents, along with certain miscellaneous equip-
ment and tools to aid in source testing, is given in this section.
     All of the components described in this section should be procured
with the stipulation that they meet the criteria discussed below.  All
new items should be visually inspected for identification and damage
prior to acceptance.  If applicable, new equipment should be calibrated
according to section 2.2 as part of the acceptance check.  Equipment not
meeting the acceptance standards must be rejected or modified to meet
the standards.  The descriptive title, any applicable identification num-
ber, and the results of the acceptance check are recorded in the receiv-
ing record file, dated, arid signed by the individual performing the
check.  Calibration data generated in the acceptance check are recorded
in the calibration log book.
2.1.1  Probe Nozzle
     The nozzle serving as; an interface between the sampling probe and the
flue gas should result in a minimum of disturbance to the flow pattern
and to the particulate concentration.  The nozzle must be inert to the
sample gases at the temperatures encountered in the field.
     The nozzle should be thin-walled with a beveled, sharp leading edge..
The bevel should be on the outside with a continuous, smooth inside
                                 10

-------
surface; i.e., a constant internal diameter must be preserved.  A but-
ton-hook shaped nozzle (see Figure 5-1 of Appendix A) is required to
allow for easy insertion through small ports when sampling a thick-
walled stack.
     A set containing a minimum of three nozzles with 6.4-, 9.5-, and
13- mm (1/4-, 3/8-, and 1/2-in) inside diameters is recommended.  Low
stack gas velocity, high moisture content, or high stack gas temperature
may require 14- or 16- mm (9/16 or 5/8 in) diameter nozzles in order to
achieve isokinetic sampling.  These sizes are not generally stock items,
but are available from the manufacturer upon request.
The following specifications are recommended:
Material:
  Temperatures below 870°C (1600°F)
  Temperatures above 870°C (1600°F)
  Temperatures up to 1370°C (2500°F)
  Wall Thickness:
  Angle of Taper:
  Distance from Tip of Nozzle to
    First Bend:
  Inside Diameter:

  Probe Nozzle Brush:
Seamless stainless steel (316)
  tubing for 2- to 3-hour
  exposures (ref. 5).
Quartz
Nickel-base alloys such as In-
  conel (subject to severe cor-
  rosion in the presence of
  fluorine or chlorine)
1.65 mm (0.065 in.)
1 30°
At least two times the outside
  nozzle diameter
Available in increments of 1.6 mm
  (1/16 in.)
See section 2.1.2.
2.1.2  Sampling Probe
     The sampling probe should be made of stainless steel or of borosili-
cate (Pyrex) glass and encased in a steel sheath.  The probe must be
equipped with a heating system that will maintain an even (preset) temp-
erature along the length of the probe to avoid condensation and reevapor-
ation of the sample gas.  The probe material must be non-reactive with
                                 11

-------
the gas constituents so as not to introduce a bias into the analytical
method.  Because of this, a knowledge of the stack gas composition and
temperature is necessary to select the correct probe.
     A new probe should be visually checked for identification, i.e.,
verify that it is the leng;th and composition ordered.  The probe should
be checked for cracks or breaks and leak-checked on a sampling train as
described in- subsection 2.3.2.1(2).  Also, the probe heating system
should be calibrated according to subsection 2.2.2.  Any probe not satis-
fying the acceptance check should be repaired, if possible or rejected.
     A probe brush of an appropriate size and shape is necessary to
clean the probe liner and nozzle prior to and after sampling.
     The following specifications are suggested for the probe and probe
brush:
     Probe Material:
       Temperature <_ 480°C (900°F)

       Temperature <_ 900°C (1650°F)
     Inside Diameter:
     Heating System:
       Temperature requirements
       at the exit and within
       0.3 m (12 in) of the
       inlet
     Probe Brush:
       Bristles
       Handles
       Extensions
2.1.3  Filter Holder
Thick-walled borosilicate glass or
  quartz glass
Quartz
1.3 cm (.5 in.) approximately

No greater than 120 + 14 °C
  (248 + 25°F) with a gas flow
  of 0.02 in /min (.75 ft3/min)
  at room temperature

Nylon
Stainless steel wire
Inert material and total length
  should be at least as long as
  the probe.
     The filter holder should be durable, easy to load, and leak-free
in normal applications.  The design must be such that the filter material
is not torn as the holder is tightened.  Also, the only flow through the
holder must be through the filter.  New filter holders are checked
                                 12

-------
visually for cracks and sharp edges that could puncture or tear a filter.
The filter holder with a filter installed is placed in a sampling train
and leak-checked at about 380 mm Hg (15 in. Hg) vacuum as directed in sub-
section 2.4.3.5.  Disassemble the holder and check the filter for punc-
tures and cuts.  Reject the holder if any of the checks are negative and
cannot be corrected.
     The glass frit should always be cleaned before sampling'according
to the mnaufacturer's recommendations.  A standard cleaning procedure
is not applicable to all filter supports due to the variation in con-
struction materials, but this construction material should allow the
rinsing of the interior surface of the filter holder and frit with 1:1
(V/V) hydrochloric acid and water.  This wash should be followed with a
final rinse of distilled, deionized water.
     Specifications for the filter holder are:
     Material:                     Borosilicate (Pyrex) glass (other
                                     materials may be used if approved
                                     by the EPA administration)
     Leak Sealant:                   Non-reactive to the stack gases
     Filter Support Media:           Glass frit
2.1.4  Filter Holder Box
     The filter box must be equipped with a heating system and a temper-
ature monitoring device to regulate the temperature around the filter
holder during sampling.  A dial-type thermometer is recommended for moni-
toring the temperature.
     Visually check the filter holder box for damage.  Check the heating
system by calibrating it as directed in subsection 2.2.2.  Reject the
box if it is damaged or if a preset temperature in the range of 120 +
14°C cannot be maintained.  The heating system and thermometer should
meet the following criteria:
     Desired Temperature:          No greater than 120 + 14°C (248 + 25°F)
                                     in ambient temperatures down to 0°C
                                      (32°F)
                                 13

-------
     Thermometer:
       Accuracy                    + 3°C (+ 5°F)
       Range                       16° to 150°C (60° to 300°F)

2.1.5  Impingers/Condenser/Container
     The sample gas, having passed through the filter, must be cooled to
20°C (68°F) or less, and the moisture content of the stack gas measured.
To accomplish this task, four impingers are connected in series.  The
first, third and fourth impingers (see Figure 2) are of the modified
Greenburg-Smith design.  The second impinger is of the Greenburg-Smith
design with the standard tip.  Each impinger is checked visually for
damage, such as breaks or cracks, and manufacturing flaws, such as poorly
shaped connections.  The container should be checked for damage and filled
with water to see if it leaks.  Reject any item that is faulty.
     The fourth impinger is required (charged with 200 g of preweighed
silica gel) to remove moisture and to protect the vacuum pump and dry
gas meter.  The reference method requires that the condensate trap be
used to keep the effluent gas temperature at 20°C (68°F) or less.  Ice
containers are available in commercial trains or can be fabricated from
closed-pore expanded polyethylene.  The efficiency of the ice bath can be
increased by the addition of salt.
     Specifications are as follows:
     Second Impinger:                     Tip must be large enough to
                                            allow an impinger full of
                                            water to drain in at least
                                            6 to 8 seconds (this avoids
                                            an excessive pressure drop
                                            in the sampling system)
     Modified Impingers:                  Replace tip with a 13 mm (1/2 in.)
                                            diameter glass tube extending
                                            to within 13 mm from the bot-
                                            tom of the flask
     Joints:                              Inert, leak-free
     An alternate method for cooling the stack gas is to use a condenser
so designed that the total volume of condensate can be determined.  A
                                 14

-------
drying tube should follow the condenser to remove the remaining mois-
ture for calculation of moisture content and to protect the vacuum
pump and dry gas meter.  Important specifications for the condenser and
drying tube follow:
     Condenser:
        Total capacity                     1500 ml
     Drying Column:
        Diameter                           5 cm (2 in.)
        Length                             25 to 30 cm (10 to 12 in.)

2.1.6  Vacuum Pump
     The vacuum pump must be capable of maintaining a constant flow rate
of the sample gas.  Two types of vacuum pumps are commonly used:  a mod-
ified sliding fiber vane pump and a diaphragm pump.  The pump should be
leak-checked upon placing the pump in a sampling train such as in Figure
5-1 of Appendix A.  With the pump running, adjust the system to 380 mm Hg
(15 in. Hg) with the inlet of the metering system closed.  The dry gas
meter dial should not move after the adjustment has been made.  When us-
ing a diaphragm pump with a by-pass valve, the absence of valve float
must also be verified as directed in section 2.2.3.  Suggested specifica-
tions for the vacuum pump follow:
     Desired Flow Rate:
       At zero vacuum              0.11 m /min (4 ft /min)
                                         O          T
       At 508 mm Hg (20 in. Hg)    0.03 m /min (1 ftj/min)
                                     (with the pump outlet at or near
                                     standard pressure, i.e., 760 mm Hg)
       Vacuum (Inlet Plugged):     380 mm Hg (15 in. Hg)

2.1.7  Dry Gas Meter
     A new dry gas meter must be calibrated according  to  section 2.2.3.
It should meet the following requirement:
     Accuracy:                         +2 percent (compared to a wet
                                         test meter) at flow rates of
                                         .008 to 0.034 m3/min (0.3 to
                                         1.2 ft3/min)
                                  15

-------
2.1.8  Orifice Meter
     Construction details of the orifice meter are given by Martin
(ref. 6).  Significant design criteria are listed below.  After visually
inspecting the orifice meter and the inclined manometer (or equivalent
differential pressure gage) for damage, the instruments are assembled in
a sampling train as shown in Figure 5-1 of Appendix A and calibrated as
directed in subsection 2.2.3.  If AH@ is outside the limits outlined below
(and discussed in subsection 2.2.3), the orifice meter should not be used
with a commercially available sampling nomograph.  It AH@ is greater than
53 mm (2.1 in.) of water, the orifice opening can be made larger (ref. 6)
to lower AH@ to an acceptable value.  Low values of AH@ cannot be cor-
rected.   Values of AH@ outside the limits listed below are acceptable
when actual values are used to calculate the relationship of AH to AP
(i.e., a nomograph is not used) for each field test.  The value of AH@
should be inscribed on or otherwise affixed to the orifice meter box.
     Specifications for this instrumentation include:
     Orifice Diameter:                47 cm (3/16 in.)
     AH@ at 21°C (70°F) and           46.7 + 6.4 mm H20 (1.84 + 0.25 in.
       760 mm Hg (29.92 in. Hg):        H20)
     Inclined Manometer Range:        0 to 200 or 250 mm H20 (0 to 8 or
                                        10 in. H20)
     Inclined Portion of Scale:
       Range                          0 to 25 mm H20 (0 to 1 in. H2O)
       Divisions                      0.25 mm H20 (0.01 in. H20)
     Vertical Portion of Scale:
       Range                          25 to 200 or 250 mm H20 (1 to 8
                                        or 10 in. H20)
       Divisions                      2.5 mm H20 (0.1 in. H20)

2.1.9  Thermometers
     Three dial-type thermometers are suitable for monitoring the inlet
and outlet temperatures of the dry gas meter and the sample gas as it
leaves the last impinger.  All of the above temperatures can be monitored
                                  16

-------
by other means, such as a thermocouple or thermistor, but even then a
dial-type thermometer is recommended as a backup system.
     Dial-type thermometers are easily damaged.  Each new thermometer
should be visually checked for damage, such as a dented or bent stem.
Each thermometer is then calibrated as directed in subsection 2.2.4.
A thermometer should read within + 3°C (+ 5°F) of the true value when
checked in an ice water bath and/or + 4°C (+ 7°F) when checked in boil-
ing water (this represents a + 1 percent accuracy when temperature is
given in absolute units).  Damaged thermometers that cannot be cali-
brated should be rejected.
     Suggested thermometer data includes:
     Range:                             0 to 50°C (30° to 120°F)
     Accuracy:                         + 1% of absolute temperature

2.1.10  Vacuum Gage
     The vacuum gage must be checked visually for damage and calibrated
according to the directions in subsection 2.2.7.  Any gage which is
damaged and/or too erratic to be calibrated should be rejected.
     A vacuum gage with the following specifications is adequate for
monitoring the sampling train vacuum:
     Range:                          0 to 76 cm Hg (0 to 30 in. Hg)
     Divisions:                      25 mm Hg (1 in.  Hg)

2.1.11  Check Valve
     A one-way check valve equipped with convenient-sized fittings is
required in the sampling train (see Figure 5-1 Appendix A).

2.1.12  Valves
     Two metering valves (1 ball and 1 needle) with convenient-sized
fittings are required in the sampling train.  Locate the valves in the
sampling train and check for proper operation.  Reject any valve that
cannot be adjusted over the desired operating range.
                                 17

-------
2.1.13  Stack Gas Velocity Measuring System
     See the Quality Assurance Document of this series for Determination
of Stack Gas Velocity and Volumetric Flow Rate (type-S pitot tube)  (ref. 1)
for a discussion of this system.  Also, see the EPA revised method  as
contained in the Final Report of this contract (ref. 4).

2.1.14  Stack Gas Temperature Measuring System
     This system is treated as a subsystem of the velocity measuring
system and is discussed in the document referenced in the preceding sub-
section (i.e., 2.1.13).  The temperature measuring system must be in-
stalled as shown in Figure 5-1 of Appendix A so that the sensor extends
beyond the probe tip and does not touch metal.  The position should be
about 1.9 to 2.5 cm (0.75 to 1 in.) from the pitot tube and probe noz-
zle to avoid interference with the gas flow (ref. 7).

2.1.15  Stack Gas Pressure Measuring System
     This system is treated as a subsystem of the velocity measuring
system and is discussed in the document referenced in subsection 2.1.13.

2.1.16  Filter Media
     The filter media are not reusable and all new filters must be
visually checked for pinholes and tears.  Any filter with a flaw is
rejected.  It is recommended that the surface alkalinity (pH) be measured
for each lot of filters and that only filters meeting the specifications
below be used.  The pH of a filter can be checked in the following manner:
     1.  Randomly select seven filters out of every box of 100 filters.
     2.  Fold and place one of the filters into a 100 ml beaker.  Add
                                                         2
approximately 1 ml of deionized, distilled water for 4 cm  of filter
material, bring to a boil., and hold for 1 minute.  Make a slurry while
the mixture is boiling by stirring the filter and water with a glass stir-
rer.
                                  18

-------
     3.  Cover the beaker and cool to room temperature.  Measure the pH
with a standardized pH meter.
     4.  Repeat Steps 2 and 3 above for the other six filters.  If all
seven pH values are between 6.0 and 8.0, accept the 93 remaining filters.
If one or more pH values fall outside the above range, it is recommended
that the remaining filters not be used.
     The collection efficiency shall be determined as specified in section
3.1.1 of Appendix A.  Test data from the manufacturer's quality control
program should meet this requirement.   Recommended purchasing criteria
for the filters follow:
     Material:                            Glass-fiber; inert
     Collection Efficiency:               99.95 percent (<_ 0.05% penetra-
                                            tion) for particulates larger
                                            than 0.3 ym in diameter
     Surface Alkalinity:                  pH = 7 + 1

2.2  EQUIPMENT CALIBRATION

2.2.1  Nozzle Diameter
     Upon the purchase of a new nozzle, measure the inside diameter to
the nearest 0.025 mm (0.001 in.) using a micrometer.  Make a minimum of
three individual measurements using different diameters (rotate 60° for
each measurement) each time and calculate an average diameter.  The range
(i.e., difference in smallest and largest values) of the measurements
should not exceed 0.1 mm (0.004 in.).   If it does, the nozzle is out-of-
round and should be repaired or replaced.  Number the nozzle and record
the number and diameter of the nozzle to the nearest 0.025 mm (0.001 in.)
in the laboratory calibration log book.  Etch or permanently fix the aver-
age diameter on the nozzle.  The nozzle should be checked visually for
out-of-roundness and signs of damage before each field test.

2.2.2  Probe Heater and Filter Box Calibration
     Set up the sampling train with the probe connected to the sampling
                                                         3             3
box.  With the nozzle detached and a flow rate of 0.021 m /min (0.75 ft /min),
                                 19

-------
profile the temperature in the probe as the heat is increased.   Determine
the inlet and outlet temperature of the probe at a determined reference
point corresponding to 120°C (248°F).   If the outlet temperature is not
120°C + 14°C (248 + 25°F) and the temperature is reasonably uniform along
the probe, adjustments must be made.  If the probe is not equipped to
monitor its temperature continuously,  the temperature should be plotted
as a function of the percent of the power setting (ref.  9).
     A thermocouple with leads of approximately 3 meters can be used with
a potentiometer readout to profile the probe temperature (draw the thermo-
couple along the length of the probe while maintaining a sample flow rate
          3
of 0.021 m /min).  An alternate approach would be to use a remote reading
thermometer.
     The filter box temperature can be monitored with a thermocouple,
thermister, or with a dial-type thermometer.  Adjust the voltage supply
until the box temperature is 120°C (248°F).  The temperature should not
vary more than + 14°C (+ 25°F) over a 2 hour period.
     In all thermometer or temperature sensor calibrations the reference
points should be an ice bath and boiling water.
     The probe and filter box heating units should be calibrated when
new, after repairs, or any time the presampling check indicates that the
system is not functioning properly.

2.2.3  Dry Gas Meter and Orifice Meter
     An initial check should be made of the sampling train to check for
proper operation of the pump, dry gas meter, vacuum gage, and dry gas
meter thermometer(s).  After the metering system components have been
checked, the vacuum system should be leak-checked.  This is done by plug-
ging the inlet side of the metering system, pulling a vacuum of 380 mm Hg
(15 in. of Hg), and observing the dry gas meter.  If the leakage exceeds
        o             2
.00057 m /min (0.02 ft /min), the leak(s) must be found and eliminated
until the above specification is satisfied.
     The dry gas meter should be calibrated when new, and a three-point
check performed prior to each field trip.  Calibration is performed by
                                  20

-------
making simultaneous total volume measurements with a calibrated wet test
meter (or equivalent volume measuring device) and the dry gas meter in
the meter box.  The wet test meter must be of the proper capacity and
accuracy.  For commercial sampling trains, the wet test meter capacity
                       3          3
must be at least 0.03 m /rev (1 ft /rev) with an accuracy of + 1 percent.
The wet test meter must be of the proper capacity; otherwise, at the higher
flow rates the linkage in the wet test meter will slip, resulting in
erronneous volume measurements as recorded by the wet test meter.  The
recommended calibration procedures are as follows:
     1.  If the sampling train has a diaphragm pump and by-pass valve,
the system must be checked for valve float.  A one point check is speci-
fied in Section 5.3 of the reference method (Appendix A).  A multipoint
check covering the expected operating range is recommended here (ref .  8) .
(The wet test meter is not required while checking for valve float by
this technique) .
                                                    3             3
         a)  Initially, operate the system at 0.02 m /min (0.75 ft /min)
for 10 minutes before taking data.
         b)  Operate the sampling system at orifice readings between 1.3 mm
and 130 mm H20 (0.05 and 5 in. I-LO) .
         c)  Take data through the above range at flow rates of 0.002,
0.008, 0.014, 0.019, and 0.028 m3/min (0.1, 0.3, 0.5, 0.7, and 1.0 ft3/
min) , once with the by-pass valve closed (see Figure 5-1 Appendix A) and
once with the by-pass valve completely open.  Time each setting for 1
minute.  Record the AH setting orifice meter reading and the initial
and final volumes on the dry gas meter for each flow rate setting.
         d)  Calculate AH@ from the two sets of data (see ref. 8).
                               -4  6
            where K = 4.48 x 10   m  in metric units, and
                  K = 0.56 ft  in English units.
Plot two curves (one with the bypass valve opened and the other with it
closed) of AH@ vs, the volume (V) recorded by the dry gas meter.  If
                                  21

-------
the valves are floating, the two curves will not coincide.  Ideally, the
curves should coincide and be horizontal over the whole range; in prac-
tice, the curve will probably have a slight slope.
     This initial check for valve float should be performed (for trains
utilizing a diaphragm pump and by-pass valve) once after building or
purchasing a sampling train and must be repeated whenever a new pump is
installed in the system.  Va.lve float, if present, must be corrected
(ref.8).
     2.  Determination of AH@ and y is as follows:
         a)  The wet test meter is placed upstream of the sampling system
with its outlet connected to the inlet (sample umbilical connection) of
the meter box (ref. 9).  These connections must be leak-free.
                                                        3
         b)  Operate the pump at a flow rate near 0.02 m /min for 15 min-
utes to warm up the pump and wet the surface of the wet test meter.
         c)  Collect and record (as shown in Figure 2) the calibration
data by setting AH on the orifice manometer and letting a given volume
(V ) of air pass through the wet test meter  (the larger the volume, the
greater the accuracy).  Repeat the above procedures until the data are
collected.  Always have the by-pass valve open.  A stop watch or laboratory
timer is used to record the time (8) required for V  to pass through the
                                                   w
wet test meter.
      The symbols in Figure 2 are:
                                                           3    3
      V  = Gas volume passing through the wet test meter,  m  (ft )
                                                          3    3
      V  = Gas volume passing through the dry gas meter,  m  (ft )
      t  = Temperature of the gas in the wet test meter,  °C (°F)
     t^ = Temperature of the inlet gas of the dry gas meter,  °C (°F)
     t,  = Temperature of the outlet gas of the dry gas meter, °C (°F)
      ao
     t,  = Average temperature of the gas in the dry gas  meter,  ob-
           tained by the average of t,  and t, , °C (°F)
                                     di      "o
     6    = Time of calibration run, minutes
     AH  = Orifice manometer setting, with a resultant orifice meter
           pressure drop, mm H~0 (in. H-O)
     Y    = Ratio of volumetric measurement by wet test meter to dry test
           meter.   Tolerance = 4- 0.02
                                   22

-------
Date
Calibration By
Wet Test Meter No.
Barometric Pressure,
Dry Gas Meter No.
                  in.Hg
Wet Test Meter Capacity
Date of Wet Test Meter
 Calibration
Orifice
manometer
setting,
AH,
mm HoO
(in H20)
2.5(0.1)
5.1(0.2)
7.6(0.3)
12.7(0.5)
25.4(1.0)
50.8(2.0)
101.6(3.0)
127.0(5.0)
203.2(8.0)
Gas vol .
wet test
meter
V
m3(ft3)
0.071(2.5)
0.071(2.5)
0.071(2.5)
0.14 (5)
0.14 (5)
0.28 (10)
0.28 (10)
0.28 (10)
0.28 (10)
Gas vol .
dry gas
meter
vd»
m3(ft3)









Temperature
Wet test
Meter
V
°C(°F)









Dry gas meter
Inlet
tdi,
°C(°F)









Outlet
tdo,
OC(OF)









Avg.
*d.
°C(°F)









Time
e,
min









Average
Y










AH(3










Calculations




AH
0.1
0.2
0.3
0.5
1.0
2.0
3.0
4.0
8.0


AH
An
13.6
0.00735
0.0147
0.0221
0.0368
0.0735
0.147
0.221
0.294
0.588
Y
Vw Pb ^d + 273>
, /„ AH I / ~-~\
y In j- u" 1 1+ j_ 97Q1
Vdl'b 13. 6/ fw "'"I









AH?
n nmo AU Rt,, + 273) Ql2
U.UOl,^ AH W
n / 4. _i_O"7O\ \/
Pb (tdo+ 273) L Vw J









 Figure 2.   Dry gas meter and orifice meter calibration and calculation form.
                                      23

-------
     P,   = Barometric pressure, mm Hg (in. Hg)
     AH@ = Orifice meter pressure differential that give  a flow rate of
           0.021 m3/min (0.75 ft3/min) at 21°C and 760 mm Hg, mm H20
           (in. H20).  Tolerance = + 3.8 mm H2
-------
Determination of Stack Gas Velocity and Volumetric Flow Rate (type-S
Pitot Tube) (ref. 1) , with one exception:  the type-S pitot tube should
be calibrated in the same configuration that it is to be used.  For this
method, the pitot tube is attached to the sampling probe.  However, if a
free space is maintained between the sampling nozzle and pitot tube of at
least 1.9 cm (0.75 in.) (see Figure 5-1, Appendix A) during sampling, the
pitot tube can be calibrated as directed in reference 1.  If the sampling
train is designed for sampling at higher than normal flow rates thereby
requiring the use of larger size nozzles, the free space shall be set on
the largest sized nozzle to be used.  Method 2 as revised by EPA is con-
tained in the Final Report of this contract (ref. 4).
     The pitot tube coefficient should not vary more than + 5 percent of
the average over the operating range.  If the average coefficient is out-
side the range of 0.83 to 0.87 and a sampling nomograph is used in main-
taining isokinetic conditions, corrections must be made as directed in
subsection 2.4.3.1.

2.2.6  Stack Gas Temperature Measuring System
     A temperature-measuring device attachable to a pitot tube, as shown
in Figure 5-1 of Appendix A, and capable of measuring the stack gas tem-
perature to within +1.5 percent of the minimum absolute stack gas tem-
perature is required.  A high-quality mercury bulb thermometer calibrated
at ice water and boiling water (corrected for local pressure)  temperatures
and readable to the nearest 0.5°C (1°F) is an acceptable laboratory
standard for calibration of temperature-measuring devices.   The calibra-
tion procedure is contained in section 2.1.2.2 of the Quality Assurance
Document of this series for Method 2, Determination of Stack Gas Velocity
and Volumetric Flow Rate (type-S Pitot Tube)  (ref. 1).

2.2.7  Barometer
     The field barometer should be checked against a mercury barometer
before each field test.  If the two differ by more than + 5.1 mm
(+_ 0.2 in.) of mercury either adjust, calibrate,  or replace the field
                                   25

-------
barometer as applicable.  Record the results in the calibration logbook.
Date and sign the entry.
     In lieu of a field barometer the barometric pressure may be obtained
from a nearby weather station.  The uncorrected weather station pressure
data, however, must be adjusted for elevation.

2.2.8  Analytical Balance
     The balance calibration should be verified when first purchased by
weighing a set of at least five standard weights covering the weight
range from about 0.2 to 2 g.   If any weighing deviates more than + 0.3 mg
from its stated value, the balance should be recalibrated.  Subsequent
checks are made by weighing a standard weight from the above weight range
before each set of weighings of filters.  The balance should be cali-
brated whenever a standard weight cannot be weighed to within + 0.3 mg
of its stated weight.  The manufacturer or a qualified laboratory should
perform the calibration.

2.2.9  Orsat Analyzer (optional)
     A standard Orsat analysser may be used at combustion sources for the
determination of stack gas molecular weight.  See the document of this
series entitled "Gas Analysis for Carbon Dioxide, Excess Air and Dry Mo-
lecular Weight", based on Method 3 (ref.2).

2.3  PRESAMPLING PREPARATION

2.3.1  Preliminary Site Visit (optional)
     The main purpose of a preliminary site visit is to gather informa-
tion to design and implement: an efficient source test.  Prior preparation
will result in the prevention of unwarranted loss of time, expenses, and
injury to test and/or plant personnel.  A test plan conceived from a com-
prehensive set of parameters will result in more precise and accurate
results.  This preliminary investigation (on-site) is optional and not a
requirement.  An experienced test group can, in most cases, obtain suf-
ficient information on the source through communications with the plant
                                  26

-------
engineer.  The information should include pictures (diagrams) of the
facilities.
2.3.1.1  Process (Background data on process and controls).   It is recom-
mended that the tester become familiar with the operation of the plant
before a preliminary site visit is made.   Data from similar operations
that have been tested should be reviewed if they are available and appli-
cable.
2.3.1.2  Sampling Site Preparedness.  The management of each facility tested
should provide an individual who understands the plant process and has
the authority to make decisions concerning plant operation to work with
the test team.  This would include decisions concerning whether the plant
would be operated at normal conditions or at rated capacity.  This indi-
vidual or individuals will supervise installation of ports,  sampling plat-
form, and electrical power.  If the above installations are already in
existence, they should be examined for their suitability for obtaining a
valid test and for overall safety conditions (ref. 10).  If the sampling
platform, port size, and locations are sufficient, the diameter, area of
the stack, and wall thickness should be determined.  If ports have to be
installed, specify at least 8 cm (3 in.)  ports with plugs.  Ten centimeter
(4 in.) ports are preferred.  Port locations should be based upon Method 1
of the Federal Register (ref.. 11).  One electric drop should be available
at the test facility with 120-volt, 20-ampere service.
2.3.1.3  Stack Gas Conditions.  The following can be determined on the
initial site survey, either by measurement or estimation:
     1.           T       Approximate stack gas temperature
                   Savg
     2.              P  = Static pressure (positive or negative)
     3. AP    and AP .  = Maximum and minimum velocity pressure heads
          max       mm
     4.             B   = Approximate moisture content
                     wo    KP
     5.              M  = Molecular weight calculated from approximate
                          gas constituent concentrations.
                                  27

-------
     The above parameters can be roughly determined using an inclined
manometer with a range of 0-127 mm H~0 (0-5 in. H-O) ,  a type-S pitot tube,
and a manual thermometer or thermocouple attached to the pitot tube with
a potentiometric readout device.  The moisture content (approximate) can
be determined by the wet-bulb dry-bulb method where acid gases are not
present and at stack gas temperatures less than 360°K, Method 4 can be
used if the wet-bulb dry-bulb method is not applicable, and the gaseous
constituents by hand-held indicator kits.   Nomographs  are useful in check-
ing and estimating the preliminary required data (ref. 12).
2.3.1.4  Methods and Equipment for Transporting Apparatus to Test Site.
Ropes, block and tackle, and other hoisting equipment  should belong in
the repertoire of any stack sampler.  The initial site visit should include
a preconceived plan between plant personnel and tester on how the equip-
ment can best be transported to the sampling site.   Electric forklifts
should be utilized when at all possible.  In addition to the above, it
is recommended, when permis;sible, that pictures be taken of the hoisting
and sampling areas, so that any further correspondence (either by letter
or telephone) will be clarified.

2.3.2  Apparatus Check
     Each item to be used should be visually checked for damage and/or
excessive wear before each field test.  Items should be repaired or re-
placed if judged to be unsuitable for use by the visual inspection.
     Figure 3 shows a checklist for the three phases of a field test.  It
is meant to serve as an aid to the individuals concerned with procuring
and checking the required equipment, and as a means for readily determin-
ing the equipment status at any point in time.  The completed form should
be dated, signed by the field crew supervisor, and filed in the operational
logbook upon completion of a field test.  This includes initiating the
replacement of worn or damaged items of equipment.   Procedures for per-
forming the checks are given in the appropriate subsections of this oper-
ations manual; a check is placed in the proper row and column of the
checklist as the check/operation is completed.
                                  28

-------
                            PRESAMPLING CHECKLIS'I
TEST SITE
CREW SUPERVISOR
DATE
             Date and Initial Appropriate Block  as Procedure is Completed
ITEM
SAMPLING PREPARATION AND
SAMPLING APPARATUS:
1. Nozzle
2. Probe
3. Filter Holder
4. Filter Holder Box
5. Filters
6. Thermometers
7. Impinqers
8. Vacuum Pump
9. Dry Gas Meter
10. Orifice Meter
11. Inclined Manometer
12. Vacuum Gage
13. Check Valve
14. Metering Val ves
15. By-Pass Valve
16. Type-S Pitot Tube
17. Connecting Lines
18. Barometer
19. Inclined Manometer
20. Stack Temperature Measuring
System
SAMPLE RECOVERY:
21 . Probe Brush
22. Storage Containers
23. Graduated Cylinders
24. Wash Bottles
REAGENTS:
25. Silica Gel
26. Distilled Water
27. Crushed Ice
28. Filters
DOCUMENTATION:
29. Data Sheets
CALCULATIONS & DATA VALIDATION:
30. Sampling Nomograph
31. Combustion Nomographs
32. Pocket Calculator
TOOLS AND EQUIPMENT:
33. Transportation Equipment
34. Safety Equipment
35. Tools and Spare Parts
36. Miscellaneous Supplies
Visual Check j leak Check
for Damage j Sampl n6a !




















$20^^9939$
KXXXXX^Wv-OCt _j
KXXXXXXXXXX><
^^4&s^

s&^S$w$$s£
xxxxxxxxxxx;
0<

X^vsewws^
^99999999999
^9^99Q^A
^^?^^
'vV^ ^wVvyP*
FV-^XfS''>'SX^xAvCX'y\XK'
* ^X^'^X 'Xx>?A;<^OOC
XX?S?99%XXX?<

kxXx>0hXXXX^wvv
^^SS^x"?^






K$s£5&S?$9s8? ~~~ " ^
^$^^W£tf









yv^^9^>
ps8XXXX
-------
TEST
ON-SITE MEASUREMENT CHECKLIST
    CREW SUPERVISOR
               	              	 DATE _
                Date and Initial Appropriate Block as Procedure is Completed
ITEM
SAMPLING PREPARATION AND
SAMPLING APPARATUS:
1. Nozzle
2. Probe
3. Filter Holder
4. Filter Holder Box
5. Filters
6. Thermometers
7. Impinqers
8. Vacuum Pump
9. Dry Gas Meter
10. Orifice Meter
11. Inclined Manometer
12. Vacuum Gaqe
13. Check Valve
14. Metering Valves
15. By-Pass Valve
16. Type-S Pitot Tube
17. Connecti nq Lines
18. Barometer
19. Inclined Manometer
20. Stack Temperature Measuring
System
SAMPLE RECOVERY:
21 . Probe Brush
22. Storage Containers
23. Graduated Cylinders
24. Wash Bottles
REAGENTS:
25. Silica Gel
26. Distilled Water
27. Crushed tee
28. Filters
DOCUMENTATION:
29. Data Sheets-
CALCULATIONS S DATA VALIDATION:
30. Sampling Nomograph
31. Combustion Nomographs
32. Pocket Calculator
TOOLS AND EQUIPMENT:
33. Transportation Equipment
34. Safety Equipment
35. Tools and Spare Parts
36. Miscellaneous Supplies
Unpacked or
Purchased On-Site




































Assembled and
Performance Checked
K SAMPLING TRAIN 	 •
UJ
z
o
•xL
$$X$99oo0066656000><5666666<
Dissasembled and
Packaged for Shipment

























•^xxxxxxxxx*xxx><>
•wwyyyyyyyyyw









         Figure  3.   Particulate measurement  checklist (continued)
                                         30

-------
                            POST-SAMPLING CHECKLIST
TEST SITE
CREW SUPERVISOR
DATE
              Date and Initial Appropriate Block as Procedure is Completed
ITEM
SAMPLING PREPARATION AND
SAMPLING APPARATUS:
1. Nozzle
2. Probe
3. Filter Holder
4. Filter Holder Box
5. Filters
6. Thermometers
7. Impinqers
8. Vacuum Pump
9. Dry Gas Meter
10. Orifice Meter
11 . Inclined Manometer
12. Vacuum Gage
13. Check Valve
14. Metering Valves
15. By-Pass Valve
16. Type-S Pi tot Tube
17. Connecting Lines
18. Barometer
19. Inclined Manometer
20. Stack Temperature Measuring System
SAMPLE RECOVERY:
21 . Probe Brush
22. Storage Containers
23. Graduated Cylinders
24. Wash Bottles
REAGENTS :
25, Silica Gel
26. Distilled Water
27. Crushed Ice
28. Filters
• DOCUMENTATION:
29. Data Sheets
CALCULATIONS AND DATA VALIDATION:
30. Sampling Holograph
31. Combustion Nomoqraohj
32. Pocket Calculator
TOOLS AND EQUIPMENT:
33. Transportation Equipment
34. Safety Equip«nt
35. Tools and Spare Parts
36. Miscellaneous Supplies
Inspect for Damage
and/or Excess Wear

























56
506656656&WW








Accepted for
Future Use


























:xxxxxxxXXXXXX>
x?yW$066&&$$$$








To Be
Replaced

























i^yyywwwww
>g^oc>o
-------
     In addition to a visual check, the following performance and/or cal-
ibration checks are performed before each _f_ield test.
2,3.2.1  Sampling Train.  The design specifications of the particulate
sampling train used by EPA are described in APTD-0581 (ref.  6).  Commer-
cial models of this train are available.  Each individual train must be
examined to see if it is in compliance with the specifications in APTD-
0581 (ref. 6) or its equivalent.  In addition, the Office of Air Programs
Publication No. APTD-Q576 :.s a valuable source of information (ref.  9).
     1.  Nozzle.  The nozzle is visually checked for damage, especially
the sharp leading edge, and the tip opening is checked for out-of-roundness.
If there is any sign of damage or out-of-roundness of the tip, the nozzle
diameter should be calibrated according to subsection 2.2.1.  Clean the
nozzle by scrubbing with tap water, followed with a wash (2 hours) in
1:1 (V/V) hydrochloric acid-water wash and rinsed with distilled, deionized
water.  An alternate cleaning procedure when rust and/or organic materials
are present is to precede the tap water wash by soaking the nozzle in
sulfuric acid.  At all times protect the knife edge from being damaged.
A damaged knife edge must be repaired or the nozzle discarded.  Minor
repairs may be done by the tester with a file and assorted tools.  An
alternate approach, especially with major damage, is to send the nozzle
to a qualified machine shop.
     2.  Probe.  Check the probe in the following manner:
         a)  Disassemble probe and check for breakage of inner liner or
damage to other parts of probe.
         b)  Clean all metal parts with acetone.
         c)  Reassemble probe and clean inner liner with brush, using
tap water and acetone.  In extreme cases, the glass ]iner can be cleaned
with a stronger cleansing agent.  Following the initial wash, the glass
liner  (interior surface) should be soaked for 2 hours in a 1:1 (V/V)
hydrochloric acid-water wash.  The final rinse should be with distilled,
deionized water and acetone  (reagent grade).  The acid wash is easily
accomplished by placing a glass female socket over the end of the male
                                  32

-------
outlet of the probe.  The acid is added to the inlet side, and the probe
is allowed to stand vertically for the duration of the wash period.
         d)  Check to see if probe will heat to the required temperature
of 120°C (248°F) to prevent condensation.  The probe temperature can be
profiled with a remote reading thermometer or with a thermocouple with a
readout device.
         e)  The probe should be sealed on the nozzle side and checked
for leaks at a vacuum of 380 mm Hg (15 in. Hg).
         f)  Cover the open ends of the probe with serum caps or equiva-
lent.
     At temperatures greater than 260°C (500°F) or if asbestos string has
been used as a gasket between the glass probe and the union holding the
nozzle to the probe and probe sheath, the probability of leakage exists.
Most stacks have a negative pressure; therefore, a leak would introduce
diluent air into the system and result in a low bias.  This problem can
be eliminated by:
     a)  Sealing the sheath from the outside air with a rubber stopper
or its equivalent (ref.  6), and
     b)  Drilling a 0.3 mm (1/8 in.)  hole in the sheath on the opposite
side of the pitot tube just behind the nut.
This modification also prevents "out" gases resulting from deterioration
of the probe from contaminating the stack sample (ref.  13).
     3.  Sampling Train Leak-Check.  Assemble the sampling train as shown
in Figure 2.   With all the impingers  empty, leak-check the sampling train
by plugging the probe inlet and pulling a vacuum of 280 mm Hg (15 in.  Hg).
                                                                       3
Leaks greater than 2 percent of the sampling rate (i.e., about 0.0006  m /
              3
min or 0.02 ft /min) as  indicated by  the dry gas meter should be found
and corrected before continuing.
Note l:  The leak-check cannot be made through the probe if asbestos
string is used in the gasket.   In this case, leak-check as described
in 2.4.3.6.   Following this initial leak-check at 280 mm (15 in.) Hg
vacuum, connect the probe and  leak-check at 25 mm (1.0 in.) Hg vacuum.
A leakage rate greater than 0.00057 m^/min (0.02 ft-Vmin) is unaccep-
table.
                                  33

-------
Note 2;  If using stopcock grease, use only the high temperature type.
2.3.2.2  Dry Gas Meter Ca.libration Check.  After the sampling train leak-
check has been satisfactorily completed in the system as directed, follow
the same procedure as used in calibrating the dry gas meter (see subsec.
2.2.3); make runs at AH settings equivalent to flow rates of about 0.01,
0.02, and 0.03 m /rain (0.50, 0.75, and 1.0 ft /min).  Calculate y for
each run (see equation ir Fig. 2) .  If -y at either one of the three
points falls outside the range of 1.0 + 0.02, the dry gas meter should be
(1) adjusted and recalibrated, (2) recalibrated and a calibration curve
constructed, or (3) replaced.  Record the results in the calibration log-
book.  Date and sign the entry.
2.3.2.3  Needle Valve(s) Check.  The needle valve(s) should be disassem-
bled and cleaned or replaced at any sign of erratic flow-rate behavior
attributable to the needle valve as observed during the above checks or
when unable to regulate the flow rate at desired levels.  Document the
adequacy of the needle valve with a check mark in the performance check
column of the presampling checklist (Figure 3).
2.3.2.4  Probe Heater Check.  Connect the probe heating system.  The probe
should become uniformly hot to the touch within a few minutes after being
turned on.   If it does not heat properly, repair or replace as necessary.
Document as part of the sampling probe performance check for the presam-
pling phase (Figure 3).
2.3.2.5  Filter Holder Box Heater.  Check the heating system to verify
that a temperature of 120 + 14°C (248° + 25°F), can be maintained for at
least 1 hour at laboratory conditions.  The maintenance of this tempera-
ture may be required in the field to prevent condensation.
2.3.2.6  Barometer.  The barometer is checked as a part of the stack gas
pressure measuring system in the Quality Assurance Document of this series
applicable to Method 2 (ref. 1).
2.3.2.7  Stack Gas Velocity Measuring System.  Check the velocity measur-
ing system according to tie directions given in the Quality Assurance
                                  34

-------
Document of this series for Method 2 and in the EPA revised Method 2 as
contained in the Final Report of this contract (ref. 4).  Visual and per-
formance checks are documented in Figure 3 under visual check for damage
and performance and/or calibration check for the presampling phase of
the field test.  If a calibration check is made, it should be recorded,
dated, and signed in the calibration logbook.
2.3.2.8  Filter Media.  The filter should be permanently numbered for
identification on its backside and along the outer edge where particulates
will not be collected.  It should then be conditioned 24 hours in a
dessiccator using anhydrous calcium sulfate at 20° + 6°C (68° + 10°F).
Following the drying procedure, the filter is weighed on a calibrated
analytical balance (see below) to the nearest 0.1 rag.  A filter is con-
sidered to be at a constant weight when two consecutive weighings
separated by at least 6 hours of dissication result in a difference in
weight no greater than 0.5 mg.
than 0.5 mg.
     Prior to the filter weighing, the balance calibration should be
checked by weighing a standard weight between 0.2 and 2 g.  Results of
the check are recorded in the laboratory logbook with the filter weights.
If the standard weight cannot be weighed within +_ 0.3 mg of its stated
value, the balance should be scheduled for calibration and a correction
factor determined for the present weighings by weighing a set of stan-
dard weights spanning the range of interest.
     The filter numbers and tare weights are recorded in the laboratory
logbook.  Each filter is placed in an inert container and sealed with
the filter number written on the container.
2.3.3  Package Equipment for Shipment
     An important aspect of any source testing method in terms of logis-
tics, time of sampling, and quality of data is the packing of equipment
with regard to (1) accessibility in the field, (2) ease of movement on
site, and (3) optimum functioning of measurement devices in the field.
Equipment should be packed under the assumption that it will receive
severe treatment during shipping and field operation.
                                  35

-------
2.3.3.1  Type-S Pitot Tube and Probe.  Pack the pitot tube and probe in
a case protected by expanded polyethylene or other suitable packing
material.  An ideal container is a wooden case or equivalent lined with
expanded polyethylene in which separate compartments are cut to hold the
individual devices.  It is also recommended that inserts for the individual
nozzles be provided.  The case should have handles that can withstand
hoisting and .should be rigid enough to prevent bending or twisting of the
devices during shipping and handling.
2.3.3.2  Differential Pressure Gage (Dual Inclined Manometer).  Always
close all valves on the pressure gage.  Pack it in a suitable case for
shipment.  Spare parts, such as 0-rings and gage oil (dual inclined
manometer), should also be packed.
2.3.3.3  Stack Temperature Measuring Device.  The temperature-measuring
device (thermocouple, thermistor, remote reading thermometer, etc.)
should be protected from breakage; i.e., placed in a tube or a suitable
shipping container.  If the device is an integral part of the pitot tube,
it can be shipped  in the type-S pitot tube shipping case.
2.3.3.4  Barometer.  The barometer should be packed in a shock-mounted
(spring system) carrying case.
2.3.3.5  Pitot Tube Lines and Sample Line (Umbilical).  All pitot tube
lines and sample lines should be coiled to utilize the smallest amount of
space.  The ends should be connected together and sealed to prevent dust
and dirt from impairing their operation.  For shipment all lines should
be stored in a case (foot locker) for protection and portability.
2.3.3.6  Glassware  (Impingers, U-Joints, etc.).  A word of caution is
needed in the use of glassware.  It is expensive and fragile, but with
sensible handling and packing its failure rate and resultant costs are
minimal.  Generally, breakage of glassware occurs during packing and move-
ment to the sampling facility.  It is recommended that glass impingers
be packed in a suitable case with approximate dimensions of 50 x 50 x 50 cm
(20 x 20 x 20 in.) with a three-tiered layer of expanded polyethylene
                                  36

-------
in which holes are cut to hold the glass irapingers.  At least 1.3 cm
(1/2 in.) of cushioning material should be placed in both top and bottom
of the shipping case (ref. 14).  A separate case Uned with expanded
polyethylene, with layers of 8 cm (3 in.) polyethylene, can be used to
carry the rest of the individual glass joints, filter holders, and fil-
ters.  One major point to consider in shipping cases is the construction
materials.  Durable containers, although more expensive to build, are the
most cost effective in the long term.  A poorly constructed shipping case
of inferior material will quickly deteriorate.  Special packaging may be
required if shipped by air freight.
2.3.3.7  Metering System (Meter Box Assembly).  A standard (commerical unit)
including pump, vacuum gage,  dry gas meter, inclined manometer, etc.,  are
contained in one meter box.  This meter box should be placed in a ship-
ping container lined with a cushioning material such as polyurethane.
     If the vacuum pump is not integral to the meter box, it should be
packed in a shipping container unless its housing is sufficient for tra-
vel.  Additional pump oil should be packed with the pump if oil is
required for its operation.
2.3.3.8  Sampling and Sample Recovery.  Sampling and sample recovery
equipment include the following:
     1.  Probe brush (commercial unit) or fabricated tube as long as the
probe.
     2.  Glass wash bottles.
     3.  Glass storage containers.  Chemically resistant, borosilicate
narrow mouth glass bottles, 500 ml or 1000 ml for acetone washes.  The
caps for the containers should be lined with Teflon or some other inert
material that is non-reactive to acetone,
     4.  Graduated cylinder (250 mil).
     5.  Silica gel:  indicating type, 6-16 mesh, dried at 175°C (350°F)
for 2 hours in preweighed lots of approximately 200 g  (two/test plus
spares in case of high moisture content in the stack gases).
     6.  Ice chest and water container.
                                  37

-------
     7.  Acetone:  AA (atomic absorption) grade.
     8.  Distilled, deionized water.
     9.  Wash acid:  1:1 (V/V) hydrochloric acid-water solution.
     All glass bottles or glass storage containers should be packed with
cushioning material at the top and bottom of the case with some form of
divider to separate the components.  One shipping case can contain the
acetone, preweighed silica gel, glass wash bottles, graduated cylinders,
and probe brush.  A water container and ice chest can be shipped as is.
It is recommended in certain cases that these two items be purchased
on-site.  A general rule of thumb in source testing is "when possible,
always carry a spare."

2.3.3.9  Source Sampling Tools and Equipment.   The need for specific
tools and equipment will vary from test to test.  A listing of the most
frequently used tools and equipment is given below:
     1.  Equipment Transportation
         a)  A lightweight handtruck that can be used to transport cases
and that can be converted to a four-wheel cart for supporting the meter
box control unit.
         b)  A 1.3 cm (1/2 in.) continuous filament nylon rope with large-
throat snap hook and snatch block for raising and lowering equipment on
stacks and roofs.
         c)  Tarpaulin or plastic to protect equipment in case of rain.
Sash cord, 0.6 cm (1/4 in.) diameter for securing equipment and tarpaulin.
         d)  One canvas bucket, useful for transporting small items up
and down the stack.
     2.  Safety Equipment
         a)  Safety harness with nylon and steel lanyards, large-throat
snap hooks for use with lanyards for hooking over guard rails or safety
line on stack.
         b)  A fail-safe climbing hook for use with climbing harness
when climbing ladders having a safety cable.
         c)  Hard hats with chin straps and winter liners, gas masks,
                                  38

-------
safety glasses or safety goggles, and a first aid kit.
         d)  Protective clothing, including the following:  appropriate
suits for both heat and cold, gloves (both asbestos and cloth), and
steel-toed shoes.
         e)  Steel cable, .5 cm (3/16 in.) diameter, with thimbles, cable
clips, and turn-buckles.  These are required for installing a safety line
or for securing equipment to the stack structure.
     3.  Tools and Spare Parts
         a)  Electrical and Power Equipment
             1)  Circular saw
             2)  Variable voltage transformer
             3)  Variable speed electrical drill and bits
             4)  Ammenter-voltmeter-ohmmeter (VOM)
             5)  Extension cords:  Light (No. 14 AWG), 2 cords x 8 m
                 (25 ft) long
             6)  2-3 wire electrical adapters
             7)  3-wire electrical triple taps
             8)  Thermocouple extension wire
             9)  Thermocouple plugs
            10)  Fuses
            11)  Electrical wire
        b)   Tools
             1)  Tool boxes (one large, one small)
             2)  Screwdrivers
                 (a)  One set flat blade
                 (b)  One set Phillips
             3)  C-clamps (2):  15 cm (6 in.), 8 cm (3 in.)
        c)   Wrenches
             1)  Open end set:  0.6 to 2.5 cm (1/4 to 1 in.)
             2)  Adjustables:  30 cm (12 in.), 15 cm (6 in.)
             3)  One chain wrench
             4)  One 30 cm (12 in.) pipe wrench
             5)  One Allen wrench set
                                  39

-------
         d)   Miscellaneous
              1)  Silicone senle.r
              2)  Silicone vacuum grease (high temperature)
              3)  Pump oil
              4)  Manometers (gage oil)
              5)  Ami seize compound
              6)  Pipe fittings
              7)  Dry cell batteries
              8)  Flashlight
              9)  Valves
             10)  Dial thermometers, 150 mm (6 in.) and 915 mm (36 in.)
             11)  Vacuum gage
             12)  SS tubing:  0.6 cm (1/4 in.), 0.9 cm (3/8 in.),
                  1.3 cm (1/2 in.); short lengths
             13)  Heavy-duty wire (telephone type)
             14)  Adjustable packing gland
2.3.3.10  Da ta Re c o r d ing.  Pack one large briefcase with at least the
following:
     1.  Nomograph for maintaining isokinetic conditions,
     2.  Data sheets or data notebook,
     3.  Carbon paper,
     4.  Slide rule or electronic calculator,
     5.  Psychrometric charts,
     6.  Combustion nomographs (ref. 12),
     7.  Pencils, pens, and
     8.  Calibration data, AH@, y, D , and C ,
                                    n       p
2.4  ON-SITE MEASUREMENTS

     The on-site measurement activities include transporting the equip-
ment to the test site, unpacking and assembling the equipment, confirm-
ing duct measurements and traverse points (such preliminary determinations
should be accomplished in a site visit), molecular weight determinations
                                  40

-------
of the stack gas, moisture content, setting of the nomograph, sampling,
sampling recovery, and data recording.  A sample data form is shown in
Figure 4.  Every quantitative stack or measurement data should be recorded
on such a form.

2.4.1  Transport of Equipment to the Sampling Site
     The most efficient means of transporting or moving the equipment
from floor level to the sampling site (as decided during the preliminary
site visit) should be used to place the equipment on-site.  Care should
be exercised against damaging the test equipment during the moving phase.
Utilization of plant personnel or equipment (winches and forklifts),
under close supervision, in moving the sampling gear is recommended.

2.4.2  Preliminary Measurements and Setup
2.4.2.1  Duct Measurement.  Determine the number of traverse points accord-
ing to Method 1 (EPA revised Method 1 in ref.  4).  Measure the duct dimen-
sions following the directions in subsection 2.2.3 of the Quality Assurance
Document of this series for Method 2  (ref. 1).
2.4.2.2  Sample Box Logistics.  Once the sampling points are selected and
the probe has been marked with either a china marker or heat-bonding fiber-
glass tape (<370°C ~ 700°F) the most efficient setup for the sample box
must be determined.  A poor choice will create a backbreaking and time-
consuming sampling experience.  Two rail systems exist for sampling, (mono-
rails and duorails) in which the sampling box moves on a track(s).   Each
individual sampling situation will dictate the system of the sample box
support.   It is recommended that the sampling box be modified to allow at
least two alternate methods of support.
2.4.2.3  Stack Gas Moisture Content.   Determine the approximate moisture
content of the stack gases by Method 4 or its  equivalent (ref.  3).   If
the particular source has been tested before or a good estimate of the
moisture if available,  this should be sufficient.   The reference method
uses the condensate collected during the sampling for the moisture content
used in final calculations.
                                  41

-------
                           TEST IDENTIFICATION
PLANT NAME
LOCATION __
SOURCE
OPERATOR(S)
          TEAM SUPERVISOR
          DATE OF TEST
                           TIME
STACK NUMBER
                      SAMPLING SITE  IDENTIFICATION
STACK DIMENSIONS:
                   m,
STACK AREA
          m,    W
NOZZLE DIAMETER 	
DRY GAS METER NUMBER _
Y  	
SAMPLING PROBE LENGTH
ORIFICE METER AH@ 	
PITOT TUBE NUMBER
PROBE LINER MATERIAL
SAMPLE BOX NUMBER _
FILTER NUMBERS 	
SILICA GEL NUMBERS
                        APPARATUS  IDENTIFICATION
cm
DIFFERENTIAL PRESSURE  GAGE:
    RANGE              mm H,
              DIVISION
                                 mm
          BAROMETER NUMBER
  mm
                             RUN  INFORMATION
          PROBE HEATER SETTING
          FILTER BOX HEATER SETTING
SAMPLING TRAIN LEAKAGE RATE
         m /rain  at
                      mm Hg Vacuum
APavg
Pbar.
pg-
PS = <
                PRELIMINARY  DATA FOR ISOKINETIC  SAMPLING
                  mm  H20
                  mm  Hg
                  mm  Hg
          T
               °K
          rC" FACTOR
                             mm  Hg
  Figure 4:  Sample Data Form for Particulate Emissions  Determinations
                                 42

-------
         uj o;
         GO UJ
      O- UJ
      s: a
         -
      H- o
         O  >— I
      I/I
      eC U-  cr:
      CO O  O
        UJ    CL
        I— x s:<"
        _l O LU C_
        1—I CO !— O
      o:
      UJ UJ
      o; I—
      a
        D- U-fO
        2: 2:  6
        <=c rj —
        i/o
        cC
        CD
UJ
a
a:
o
CJ
UJ
a:
CD UJ
   I— O
>- UJ Z
a: s: >-•
a     a
       -     O

^ „    ^
"-1 °  td
CJ cC
O UJ   p.
_J 3T   P
               Pb
                i—i s:
        =c a =>
        c2 o_ 2:
                                                                                                  UJ
                                                                                                  CD
                                                                                                                     •H
                                                                                                                      J-J

                                                                                                                      8
                                                                                                                      o
                                                                                                                      03
                                                                                                                      a
                                                                                                                      o
                                                                                                                     •H
                                                                                                                      4J
                                                                                                                      tti
                                                                                                                      c
                                                                                                                             (D
                                                                                                                             4-)
                                                                                                                             QJ
 cn

 g
•H
 cn
 CO
•H
 g
 a)

 
-------
                            MEASURED VALUES
(1)   Total  Particulate Weight Collected,   m ,  mg.
CONTAINER
NUMBER
1
2
BLANK*
CORRECTION
TOTAL (ran)
WEIGHT OF PARTICULATE COLLECTED,
mg
FINAL WEIGHT




TARE WEIGHT




WEIGHT GAIN
+ mg
+ mg
mg
mg
         Blank Correction = Residue (Blank) mg x (Vp/VR)
         where   V2 = Volume of acetone wash in container number 2,
                      im, and
                 VD = Volume of acetone blank, usually 100 m£.
                  D

(2)  Volume of gas sample through the dry gas meter at standard conditions
     to three significant digits.
                Vm(std) = °'3855 Vm
                                              AH
                                              3.6
m
(3)  Moisture content of stack gas to two significant digits.

                  (0.00134 m3/mA)V1
      ws
           Vm(std) +
                                                    dimensionless.
 Figure  4.   Sample data form for  particulate anissions  determinations
            (continued).
                                   44

-------

FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED (Vlr)
V*
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME,
ml



SILICA GEL
WEIGHT,
mg


*
m&
        Mass of water in mg = volume of water in ma.

(4)  Particulate concentration at standard conditions on a dry basis,

                                                       .3
           cs = (o.oi54
(5)  Stack gas molecular weight on a wet basis
           Ms =
- Bws) + 18 Bws
                           g/g-mole
where   Md = 0.44(%C02) + 0.32(%62) + 0.28(100 - %C02 - %6"2) .
(6)  Average stack gas velocity
                                           1/2
          avg
•p  (/4P)avg  '    S
                                                         m/sec
(7)  Percent of isokinetic sampling
           4.323 Vm(std)  Ts
                           percent.
Figure 4.  Sample data form for particulate emissions determinations
           (continued).
                                   45

-------
 (8)  Volumetric flow rate,  dry  basis,  standard  conditions
               Qs  =  1388(1  - Bws)  (Vs)ayg A(PS/TS    ) - 	m3/hr-
 (9)  Parti cul ate mass emission  rate calculated  on  a  sample  concentration

      basis



                    PMR  = Cs  x  Qs  = _ g/hr.





                              SUMMARY  OF  RUNS


(10)  Average participate mass emission  rate  for three sample  runs


                          PMR, + PMR9 +  PMR,
                          - ] -- _J - 3  = - 9/hr.
(ll)   PMR" with  90 percent  confidence  limits  (for  3  runs) where FWR° is  the


      grand  mean that would be obtained from a  large  number of  tests



                    PMR -  2.92  sfPMR}//! < PMR <  PMR + 2.92  s{PMR}//3



                      (PMR,  - PMR)^ +  (PMR9  - PMRY +  (PMR.  - PMR)^  1/2

      where s{PMR}         '               ^               J
Figure 4.  Sample data form for particulate  emissions  determinations

           (continued).
                                     46

-------
 2.4.2.4  Molecular Weight of Stack Gas.  Determine the dry molecular weight
 of  the gas stream by Method 3  (ref. 2).  If  the particulate concentration
 is  to be adjusted to 12% C09,  it is recommended that the sample be of the
 integrated type for two reasons:  1) the possibility of a more representa-
 tive sample and, 2) the convenience of taking the sample at the stack and
 being able to  transport the sampling bag to  a more suitable area for Orsat
 analysis.
 2.4.2.5  Stack Temperature and Velocity Heads.  Set up and level the dual
 inclined manometer and determine the minimum and maximum velocity head
 (AP) and the stack temperature (T ).  This is done most efficiently with
                                 s
 a type-S pitot tube, with a temperature-sensing device attached as shown
 in  Figure 5-1  of Appendix A.   The AP's are determined with an inclined
 manometer by drawing the pitot tube across the stack diameter in two
 directions (circular stack with 90° traverses).  This must be done in
 order to pick  the correct nozzle size and to set the nomograph.  Incor-
 rect selection of nozzle size  and/or setting of the nomograph may result
 in  not being able to maintain  the isokinetic sampling rate, thereby void-
 ing the sample.  Determine the static pressure as directed in the Quality
 Assurance Document of this series for Method 2 (ref. 1).

 2.4.3  Sampling
     The on-site sampling includes making a final selection of proper
 nozzle size,  setting the nomograph (if used), loading the filter into the
 filter holder,  preparing and assembling the sampling train, making an ini-
 tial leak-check,  inserting the probe into the stack,  sealing the port,
 sampling isokinetically while traversing,  recording the data,  and making
 a final leak-check of the sampling system.   Sampling is the foundation of
 source testing.  Critical problems in testing result from poor or incor-
 rect sampling more frequently than from any other part of the measurement
 process.   The analytical process  (laboratory) can never correct for errors
made in the field resulting from poor judgment or instrumental failure.
 If the initial  site survey,  apparatus check and calibration,  and prelim-
 inary measurement and setup on-site have been implemented properly,  the
                                   47

-------
testing should go smoothly with a minimal amount of effort and crises.
2.4.3.1  Preliminary Setting of the Nomograph.  The setup of the nomograph
using the parameters obtained in subsection 2.4.2 is given in detail in
Appendix B of this document.  A procedure is included in the appendix for
checking the nomograph for correct design (accuracy).
Note
_3:   If the coefficient,  C ,  of the type-S pitot tube being used is
ide  the range of 0.85 +; 0.02, compute the ratio (C /0.85)2 and mul-
tiply this constant times the correction factor, C, obtained from the
nomograph.  Use this new "C" factor in setting the nomograph for iso-
kinetic sampling (see Appendix B for further discussion).
2.4.3.2  Selection of Nozzle Size.   After the nozzle size and appropriate
probe length have been selected, insert the nozzle in the probe sheath
union and tighten the union.  Do not use wrenches; finger-tight is suf-
ficient in most cases.  Using uncontrolled pressure in tightening the
union will result in a broken or cracked inner-liner.  Keep the ball
joint and nozzle tip protected from dust and dirt with a serum cap or
equivalent.
2.4.3.3  Assembling of Sampling Train.  Assemble the glass impinger train
as follows:
     1.  Measure 200 m£ of distilled water in the graduated cylinder
5-m£ divisions) and place approximately 100 m£ of the water in each of
the first two impingers
     2.  The third impinger is left empty.
     3.  Place approximately 200 g of preweighed indicating silica gel
into the fourth impinger.
     The first, third, and fourth impingers are modified Greenburg-Smith
while the second impinger is of the standard Greenburg-Smith design.
Place the impingers into the sample box and assemble the sampling train
using the appropriate U-joint.s.  A very light coat of silicone grease
(acetone insoluble) should be; applied carefully to the joints, to avoid
leaks in the system.  Depending upon the design of the impinger, apply
the lubricant in a manner that precludes  its contact with  the  sample.
     The loading of the impingers into the sample box can be done in the
                                    48

-------
laboratory by sealing the inlet to the first impinger, the outlet of the
third impinger, and inlet and outlet of the silica gel impinger.  This
is practical only when the sampling site is near and the logistics are
suitable.
     In view of the fact that the reference method does not consider the
analysis of the condensible fraction, the impingers are not needed as
such.  A condenser can be employed consisting of a coiled tube of stain-
less steel or copper and a reservoir that has a capacity of at least
1500 mH,  A good design would incorporate a drain valve in the bottom of
the reservoir to allow the tester to drain and measure the total volume
of condensate for moisture determinations.  In all cases the impingers
or condenser are maintained in an ice bath during sampling to remove the
condensibles and keep the exit gas at or below 20°C (68°F).  When a con-
denser is utilized, a drying tube downstream is used to protect the dry
gas meter and vacuum pump.
2.4.3.4  Load Filter.  Load the filter as follows:
     1.  Preweighed filter (desiccated for 24-hours and weighed to the
nearest 0.1 mg) is removed with teflon covered tweezers from its sealed
container and placed in the filter holder.  The filter should have an
identifying number and the filter holder should be numbered with a semi-
permanent marker to preserve the integrity of the sample.  Make certain
that the filter is centered correctly in the holder with the sample side
toward the probe.   The filter holder should be tightened until the two
halves are secure.  Over-tightening the two halves can break the filter
holder or tear the filter.
     2.  Place the filter holder into the sample box and connect the exit
of the filter holder to the inlet of the first impinger.  Plug the inlet
of the filter holder with a glass ball to check for leaks.  Connect the
meter box (vacuum port) to the sample box with the appropriate umbilical
cord.
2.4.3.5  Perform Leak-Check.   Leak-check the sampling train by plugging
the inlet to the filter holder,  turning on the vacuum pump, and opening
                                  49

-------
the valve system until the vacuum in the system reaches 380 mm Hg (15 in. Hg)
                                        3             3
A leakage rate not in excess of 0.0006 m /min (0.02 ft /min) at 380 mm Hg
vacuum is acceptable.  Release the pressure in the system but do not turn
off the pump until the following sequence has been completed:
     1.  Slowly release the pressure in the system by carefully opening
(twisting) the glass ball in the inlet of the filter holder.
     2.  Shut the coarse valve (main vacuum valve).
     3.  When the vacuum gage reads zero vacuum, remove the glass ball
and shut down the pump.
2.4.3.6  Installation of Probe.  Mount the probe in the sampling box.
Check the configuration of the stack gas temperature measuring system
as shown in Figure 5-1 in Appendix A.   Connect the probe to the inlet of
the filter holder and leak-check in the following manner:
     1.  Seal the inlet of the probe nozzle with a serum cap.
     2.  Turn on vacuum pump.
     3.  Open the valve system and adjust the vacuum to 380 mm Hg (15 in.
Hg).   A lower vacuum may be used provided that the vacuum used here is
not exceeded during the test.
     4.  Check the leakage rate on the dry gas meter.  A leakage rate less
than 0.0006 m3/min (0.02 ft:>/min) at 380 mm Hg (15 in. Hg) vacuum is
acceptable.
Note 4: If an asbestos string is used in the fabrication of the probe
nozzle to the probe liner connection,  leak-check at 25 mm Hg (1 in. Hg)
vacuum only.  If a leak-free connection in the nozzle is employed, the
total  train, filter and probe, can be initially checked at 380 mm Hg
(15 in. Hg) vacuum.
     5.  After completion of the leak check, release the pressure as fol-
lows :
         a)  Slowly release the vacuum by carefully opening  (squeezing)
the serum cap until the system pressure is back to ambient  (monitor with
built-in vacuum gage).
         b)  Turn valve system off (coarse valve).
         c)  Turn off the vacuum pump.
                                  50

-------
     Operations in subsections 2.4.3.5 and 2.4.3.6 can be combined, there-
by requiring only one initial leak-check.  Record leakage rate on the form
in Figure 4.
2.4.3.7  Taking of Sample.  Turn on the sample box and fill the impinger
train container with crushed ice.  The meter box operator should now
recheck the setting of the nomograph while the sample box operator checks
the filter box temperature gage to confirm that it is coming up to operat-
ing temperature; likewise, he can touch the probe to see if it is heating.
It is recommended that a thermocouple be mounted next to the glass liner
so that the probe temperature can be monitored.
     As soon as the filter box temperature and probe temperature are up
to the desired level, the test itself can be performed:
     Remove the plug or cap from the sampling port and remove the dust
(particulates) on the port walls by utilizing a wire brush or its equiva-
lent.  Remove the serum cap from the nozzle tip.  Record the initial
volume of the test meter on the data log sheet of Figure 4.
     2.  If the sample gas is hot, start at the traverse point farthest
from the port and draw the probe out as the test continues.  Asbestos
gloves should be used in handling hot sampling probes and pitot tubes.
     3.  Attach a proper electrical ground to the probe and sampling
system.
     4.  Insert the probe to the farthest traverse point with the nozzle
pointing directly into the gas stream.  Seal the port and immediately
start the pump.  Adjust the coarse and fine control valves until isokinetic
conditions are obtained.  Note the time and record it on the data log
sheet of Figure 4.
     5.  Maintain isokinetic conditions during the entire sampling period.
Sample for an equal amount of time at each traverse point.  The time
period at each traverse point should be long enough to set the sample
rate and record the required data.  The time period at each traverse
point must be long enough to obtain a total sampling period representa-
tive of the process being monitored.  The time at each traverse point must
                                                               3       3
be sufficient to obtain a total sample volume of at least 1.7 m  (60 ft )
                                  51

-------
at standard conditions.   While sampling,  reset the nomograph if:
         a)  The temperature in the stack changes more than + 14°C (25°F) .
         b)  T  (average temperature of meter) varies more than + 6°C
     Adjust the sampling rate for every point and maintain the isokinetic
rate by continuous observation.  Record the meter volume when sampling
has been completed at each individual traverse point.  Take readings at
each sampling point, at least every 5 minutes (or during sampling period
at each traverse point) :  £.11 the readings and adjustments should not be
attempted for time intervals of less than 2 minutes.   When significant
changes in stack conditions are observed, compensating adjustments in
flow rate should be made to maintain isokinetic conditions.  Record on
the data log sheet of Figure 4 the traverse point number, stack tempera-
ture (T ), velocity pressure head (AP, mm H00 or in.  H90) , (orifice pres-
       S                                   jL          L-
sure differential (AH, mm Kg or in. H«0) , gas temperature at dry gas meter
(Tm. )  and Tm    or T   ,  °C or °F) , sample box temperature, condenser
  min       mout     avg
temperature, and the probe temperature if the probe has a thermocouple
and appropriate readout.
     6.  When sampling at one traverse point has been completed, move
the sampler to the next point as quickly as possible.  Close the control
valve only when transferring the sampler from one sample port to the
other.   Exclude the time required to transfer the sampler from one port
to another from the total sampling time.
Note 5  :  Since moving from port to port is time consuming, it is recommended
that longer probes be employed to allow only one move during a test if
a circular stack is involved.  Probes up to 3m (10 ft) long can be managed
without too much difficulty, provided that adequate space is available
on the sampling platform.
     Upon transfer of the sampler to another port, the following proce-
dures should be followed:
         a)  Monitor the vacuum through the system.  An increase of vacuum
is an indication of particulate buildup on the filter.  Loss in vacuum is
an indication of a broken impinger, connector, filter, or a loose con-
nection.
                                   52

-------
         b)  Keep the impingers iced down (i.e., monitor the condenser
temperature) to hold the temperature of the exit gas below 20°C (68°F).
Add salt to the ice bath if necessary.
         c)  Check the line voltage with a voltmeter if a digital temper-
ature system is utilized.
Note 6:  Digital temperature systems may read erroneously with a drop in
line voltage and/or interference from electromagnetic fields.
         d)  Make sure that the dual inclined manometer is level and that
the pitot tube and pitot tube lines are unobstructed.  A signal of trouble
would be AP's that are not representative of the velocity heads obtained
in the velocity traverse made during the preliminary site visit.
         e)  All data should be recorded on a data log sheet as depicted
in Figure 4.
     7.  At the completion of the test, close the coarse control valve on
the meter, remove the probe from the stack, and turn off the pump.  Remove
the probe carefully from the stack, making certain that the nozzle does
not scrape dust from the inside of the port.  Keep the nozzle elevated
to prevent sample loss.  After the probe cools place a serum cap or equi-
valent over the nozzle tip and leak-check the system at 50 mm Hg (2 in. Hg)
vacuum above the operating vacuum during the test.  The vacuum during this
post sampling leak check should be no greater than 380 mm Hg (15 in. Hg).
(Do not boil the water in the impingers.)  Follow the same leak-check pro-
cedures as outlined in subsection 2.4.3.5.  Seal the end of the nozzle.
Disconnect the pitot tube lines and umbilical.  Protect the pitot tube
and the umbilical connections with tape or an appropriate equivalent.
                                                              3        3
Record on the data log sheet of Figure 4 the leakage rate in m /min (ft /min)
and the vacuum at which the leak check was performed.  Check all connectors
such as umbilical connection, pitot tube lines, glass connections, etc.
for evidence of malfunction.  Record all abnormalities on the data log
sheet.  The logging of abnormalities will not necessarily void the sam-
ple, but it may help to improve the quality of sampling performance.
                                  53

-------
2.4.4  Sample Recovery
     Move the sampling train and probe to the sample recovery area.  Care
should be taken to prevent loss or contamination of the sample.  If the
probe must be removed before movement to the recovery area, the probe
should be sealed at both ends (serum caps) and the inlet of the filter
plugged with a glass ball.  The sample recovery area should be a well-
lighted, relatively clean room with enough table-top work space, about
     2       2
4.6 m  (50 ft ), for two crew members to change the filter and wash out
the sampling train.
2.4.4.1  Container No. 1.  Wipe the exterior of the filter holder sur-
face to remove any excess dust or extraneous material.  Remove the fil-
ter from the holder, place the filter in its original container and seal
it.  It is recommended that a piece of paper (inert, smooth surface) be
placed under the filter holder as the filter is being removed to prevent
loss of particulates.  Removal of the filter is more efficient utilizing
a set of tweezers.  Teflon-tipped tweezers and a teflon scalpel should
be used to handle filters.  If a filter is torn, all pieces must be saved,
conditioned, and weighed.  Record date, time of test, location of test,
and the number of run on this container.  This data should also be recorded
on the data log sheet of Figure 4.
2.4.4.2  Container No. 2.  Wash all internal surfaces of the sampling train
from the nozzle tip up to the backside of the filter holder with atomic
absorption grade acetone.  Determine the volume to the nearest ml and
transfer to the container.  A brush with a handle as long or longer than
the probe should be used to loosen the particulate matter.  It is recom-
mended that the probe be washed by attaching a calibrated (125 m& or larger)
cyclone flask to the end of the probe and washing the probe contents into
the container.  This wash may require emptying the flask into container No.
2 several times (the flask should be filled to the mark or to the nearest
major division with acetone each time so that the quantity of wash trans-
ferred is accurately known).  Also, a graduated cylinder should be used to
accurately measure volumes of acetone (10 to 25 m£) to be used for rinsing
                                 54

-------
the residue from the flask.
     Accurately measure in a graduated cylinder an appropriate volume (e.g.,
200 ml) of acetone to serve as a blank.
     The measured volume of acetone wash is quite critical if the acetone
is not residue free.  The total volume of wash obtained by summing the
volumes transferred to container No. 2 is recorded to the nearest m£.
     Record total volume of acetone wash, date, time of test, location and
run number on the container and on the data sheet of figure 4.
2.4.4.3  Container No. 3.  Transfer the silica gel from the fourth itnpinger
into its original preweighed container.  Label container with date, time
of test, location, and any other pertinent data.  This information should
also be recorded on the data log sheet.  All sample containers should be
glass with caps lined with teflon.

2.4.5  Total Volume
     Measure the total volume of condensate by transferring the contents
of the first three impingers into a graduated cylinder with divisions of
2 mH or less.   Record this volume of condensate on the data log sheet of
figure 4 to the nearest m£.

2.4.6  Sample Logistics (Data) and Packing of Equipment
     The above procedures are followed until the required number of tests
are completed.  The following is recommended at the completion of testing.
     1.  Check all sample containers which must be properly labelled.
(Time and date of test, location of testing, number of test, and any other
pertinent documentation.)  This aspect should be performed at the end  of
each individual test or prior to such test if the impingers are to be
utilized in further tests before returning to the laboratory.
     2.  All data recorded during field testing should be recorded in
duplicate (carbon paper).  One set of data should be mailed to the base
laboratory and the other to be hand-carried.  This is a recommendation that
can prevent a very costly mistake.
     3.  All sample containers should be properly packed in a sample box
                                  55

-------
for shipment to the base laboratory.   All boxes should be properly labelled
to prevent loss of the samples.
     4.  The sampling equipment should be inspected as it is disassembled
for packing.  Any signs of damage that could have had an influence on the
precision/accuracy of the measurement should be documented on the data
sheet and that item of equipment checked in the laboratory (if possible) to
determine the magnitude of error that may have resulted from the damaged
equipment.

2.4.7  Data Validation
     Following the directions given in subsection 2.5.3, calculate and/or
determine the following:
     1.  Moisture content of the stack gas, B
                                             ws
     2.  Stack gas molecular weight on a wet basis, M .
                                                     o
     3.  The average stack gas velocity, (V )
     4.  The percent of isokinetic sampling for the sample run, I.
     Compare these measured values to theoretical values derived from
combustion nomographs (ref. 12)  or to values obtained by other measurement
methods, e.g., measuring B   by the wet-bulb/dry-bulb method.
                          ws
     Any large unexplainable differences in measured and theoretical values
should be noted and special care taken to reduce the variability of that
specific parameter for the next run.   If the percent of isokinetic sampling
is outside the range of 0.90 to 1.10, the run should be repeated unless it
is known (must have been approved by the administrator) that the particle
size distribution is below, about 5 urn.
     Values of B   and M  as measured by the first run should be used in
                ws      s              •*
setting isokinetic conditions for subsequent runs unless there is reason
to doubt their validity as compared to the values derived from preliminary
measurements or estimates.

2.5  POSTSAMPLING OPERATIONS (Base Laboratory)
2.5.1  Apparatus Check
     A postsampling check of the equipment can serve to validate the data
                                   56

-------
from the just completed field test.  The least it can do is aid the field
team in making an honest estimate of the accuracy of the field measurements.
     Any malfunctions uncovered during the postsampling check should be
reported immediately and in detail to the supervisor.  It should also be
documented in the laboratory log and/or calibration log as applicable.
     The decision of whether to correct the data, repeat the test, or just
report the error with the data is one that the supervisor must make after
considering 1) the magnitude of the error involved, 2)  the precision/
accuracy of the measurement process, and 3) the ultimate use of the field
data.
2.5.1.1  Type-S Pitot Tube.  The type-S pitot tube is checked according to
the Quality Assurance Document of this series for Method 2 (ref. 1).
2.5.1.2  Dry Gas Meter and Orifice Meter (Sampling Train).  A postcheck (a
postcheck for one test can in some instances serve as the presampling check
for the next test) should be made of the sampling train to check for proper
operation of the pump, dry gas meter, vacuum gage, and dry gas meter
thermometers.  Leak-check the vacuum system.  Determine y and AH@ at three
points in the operating range.  This is a check on the system for future
testing and gives confidence in the data from the previous field test.
This is a recommended procedure to improve the data quality and to prevent
field sampling under assumed conditions.

2.5.2  Analysis (Laboratory)
     The requirements for a precise and accurate analysis are minimal in
the reference method.  The analytical balance should be checked with a set
of calibrated weights before the weighing of the first filter or at any
time a problem is indicated.  Record the actual and measured weights in the
laboratory logbook along with the date and initials.  If the actual and
measured values agree to within + 0.3'mg proceed; otherwise, report it to
the supervisor before proceeding.  Glass wash bottles should be utilized
in transfer and the laboratory area should be free of any grinding or
dust-producing activities.  Blanks are required in the reference method
and are always required in any analytical method striving for data validation.
                                   57

-------
2.5.2.1  Container No. 1.  Transfer the filter and any loose particulate
matter from the sample container to a tared glass weighing dish, desiccate
and dry to a constant weigat.  Weigh and report results to the nearest
0.1 mg.  After opening and closing, the humidity of the air in a desic-
cator may be very different from that of the atmosphere.  Since the rate
of removal of moisture by the desiccant may be quite slow, the initial
period of desiccation should be at least 24 hours.  After the initial
period of desiccation, eacn succeeding period of desiccation should be
at least 6 hours.  Granular or fused anhydrous calcium sulfate is most
frequently used as the drying agent.  It has a good capacity, but is not
a powerful desiccant, although sufficiently satisfactory in this respect
to be usable in this work.
     It is recommended that the sample be considered to be at constant
weight when two successive readings separated by 6 hours vary by <^ 0.5 mg.
An analytical balance which weighs to 0.1 mg should be utilized.
2.5.2.2.  Container No. 2.  Transfer the (AA) acetone washings to a tared
beaker and evaporate to dryness at ambient (laboratory) temperature and
pressure.  The transfer process should include washings (10 m£ volumes
premeasured in a graduated cylinder with 1 m£ divisions) with (AA) acetone
until a complete transferral (no signs of residual matter) is obtained.
The total volume of these washings must be added to the wash volume obtained
in the field (subsection 2.4.4.2).  An accurately measured blank (100 m&
measured in a graduated cylinder) of the acetone taken in the field is
run concurrently with the samples.  This blank will account for any
residue in the acetone or any other laboratory condition that would
tend to affect the final weight of the samples.  After evaporation, the
samples and blanks (one blank for each field site) should be desiccated
until a constant weight is obtained.  The same procedure as outlined in
section 2.3.2.1 should be adhered to.  Report results to the nearest 0.1 mg.
2.5.2.3  Container No. 3.  Weigh the spent silica gel to the nearest 0.5 g.
A top loading (trip) balance is sufficient for this weighing.  It is recom-
mended that the silica gel be weighed in Container No. 3 before the field
test and returned to Container No. 3 following the test.  This negates
                                   58

-------
the error involved in not getting complete transferral of the silica gel
from the original container.
     All data (weights, volume of condensate collected in the first three
impingers) are recorded on permanent data sheets such as depicted in
Figure 4.

2.5.3  Calculations
     Calculation error due to procedure or mathematical mistakes can be a
large component of total system error.  Therefore, it is recommended that
each set of calculations be repeated, starting with the raw field data,
preferably by a team member other than the one that performed the original
calculations.  If a difference greater than the typical round-off error is
observed, the calculations should be checked step by step until the source
of error is found and corrected.  If a computer program is used, the
original data entry should be checked and if differences are observed, a
new computer run made.  A standardized computer program should be written
to treat all raw field data.  A computer program presently being used in
EPA is included in the Final Report of this contract (ref. 4).
2.5.3.1  Weight of Particulate Collected.  Particulate weight is the sum
of the weight gains of container 1 (filter and loose particulate) and con-
tainer 2 (acetone probe wash) minus a correction for the blank as shown
in the table under item (1) of Figure 4.  Record m  in the table of Figure
4 to the nearest 0.5 mg.
2.5.3.2  Dry Gas Volume.  The sample volume measured by the dry gas meter
is corrected to standard conditions by

                             /         \     /-n       AH \
v       -   .„,,/   °K      v    bar" 13.6
        -  '3855            V
                    -
               std) -  '       mmHg     m      T       /
                            \         /    \     m     /
where ^  ,   ,.. = Volume of gas sample through the dry gas meter
                at standard conditions, nH
           V  = Volume of gas sample through the dry gas meter
                                      3
                at meter conditions, m
                                   59

-------
             = Barometric pressure at the orifice meter,

               mm H20.



          AH = Average pressure drop across the orifice meter


               obtained from the table of recorded measurements


               of figure 4, mm H20.


          T  = Average dry gas meter temperature in °C plus 273 obtained


               from the table of recorded measurements of figure 4, °K.


                                          3        3
     Record V  ,   ,N to the nearest 0.003 m  (0.1 ft ) as item  (2) under
             m(std;

measured values on the data sheet in Figure 4.



2.5.3.3  Moisture Content,	B  .  Using the value of V1  from the table under
                          ~"T™" \v S                       -*- r*

item (3) of Figure 4, calculate the moisture content by



                           (0.0013 m3/m2,) Vi
                   B	£c	 .

                    ws
                        V ,   ,.+ (0.0013 nr/m£) Vi
                         m(std)                  x
     Record B   to the nearest 0.001 on the data sheet under item 3 of
             ws

Figure 4.



2.5.3.4  Particulate Concentration at Standard Conditions on a Dry Basis, C_.
         -- -           g


Calculate the particulate concentration as follows:
where   C  = Particulate concentration in grams per standard cubic meter
         s

             on a dry basis.



     Record C  to four significant digits on the data sheet under item  4
             o

of Figure 4.



2.5.3.5  Stack Gas Molecular Weight on a Wet Basis, M.  Calculate the  stack
                                                      g.
gas molecular weight by
                        M  = MH  C1 - Bws> + 18
                         !3
                                  60

-------
 where M, is given by

            Md = 0.44(%C02) + 0.32(%02) + 0.28(100 -

 and %C02 and %6  are  the averages of percent C02 and 02  determinations,
 repsectively, according to the Quality Assurance Document  of  this  series
 for Method 3 and the  EPA revised method as  contained in  the Final  Report
 of this contract (ref. 4).
      Record M  to three significant digits, i.e., —.-,  on the  data  sheet
              s
 under item 5 of Figure 4.
 2.5.3.6  Average Stack Gas Velocity.  Calculate the average stack  gas
 velocity, (V )   ,  in m/sec by
             s avg
                                                          1/2
                 (V  )    =  34.97 C   (/AT)
                  s avg          p      avg
r (T r
    s avg
   P  M
L   s  s
 where   (V )    = Average stack gas velocity, m/sec.
           s avg
              C  = Average pitot tube calibration coefficient over
                   the velocity range being measured, dimensionless.
        (vAP)    = Average of the square roots of the velocity
                   pressure heads, (mm
         (T )    = Average absolute stack gas temperature, °K.
              P  = Absolute stack gas pressure, mm Kg.
               S
              MS = Molecular weight of stack gas on a wet basis,
                   g/g-mole.
      Record (V )    to three significant digits on the data sheet under
                 avg
 item 6 of Figure 4.
     *If Ts varies more than about 10 percent of the "mean from point to
point in the stack, the correct term to use is (/TT)    rather than
ATS).                                               avg
     avg
                                   61

-------
2.5.3.7  Percent of Isokinetic Sampling, I.  Calculate the percent of
isokinetic sampling by
                    4.323 V , „,.  T
                _  	m(std)   s
                    9(Vs)avg Ps "a- -ws'

where         I = Percent of isokinetic sampling.
            Bws = Percent moisture by volume in the stack gas, dimension-
                  less.
        V .,   .  = Volume of gas sample through the dry gas meter
                  at standard conditions,  m .
              0 = Total sampling time, min.
        (V )    = Average stack gas velocity calculated in section 2.5.3.6
                  above, m/sec.
             P  = Absolute stack gas pressure, mm Hg.
              S                                        2
             A  = Cross-sectional area of the nozzle, m .

     Record I to two significant digits on the data sheet under item 7 of
Figure 4.
2.5.3.8  Volumetric Flow Rate at Standard Conditions on a Dry Basis, Q .
Calculate the volumetric flow rate by

                    Q  = 1383(1 - B  ) (V )   A (P /T     )
                    xs             ws    s avg    s  s avg
                                               2
where  A = Cross-sectional area of the stack, m , and the other terms
are as defined in the above calculation of stack gas velocity, subsection
2.5.3.6.  A standard absolute temperature of 293°K and a standard absolute
pressure of 760 mm Hg were used in the calculation of the constant.
     Record Q  to three significant digits on the data sheet under item 8
             S
of Figure 4.
2.5.3.9  Particulate Mass Emission Rate Calculated on a Sample Concentration
Basis, PMR.  Calculate the particulate matter emission rate by

                            PMR = C  x Q
                                   62

-------
where   PMR = Particulate mass emission rate, g/hr.
         C  = Particulate concentration at standard conditions
          S                      3
              on a dry basis, g/m .
         Q  = Volumetric flow rate at standard conditions on a dry
              basis, m /hr.

     Record PMR to three significant digits on the data sheet under item
9. of Figure 4.
2.5.3.10  Calculation Check.  Calculation error due to procedure or mathe-
matical mistakes can be a large component of total system error.  Therefore,
it is recommended that each set of calculations be repeated, starting with
the raw field data, preferably by a team member other than the one that
performed the original calculations.  If a difference greater than the
typical round-off error is observed, the calculations should be checked
step by step until the source of error is found and corrected.  If a com-
puter program is used, the original data entry should be checked and if
differences are observed, a new computer run made.  A standardized com-
puter program should be written to treat all raw field data.
                                  63

-------
          SECTION III
MANUAL FOR FIELD TEAM SUPERVISOR
               65

-------
SECTION III        WNUAL FOR FIELD TEAM SUPERVISOR

3.0  GENERAL
     The term "supervisor" as used in this document applies to the
individual in charge of a field team.  He is directly responsible for the
validity and the quality of the field data collected by his team.  He may
be a member of an organization which performs source sampling under
contract to government or industry, a government agency performing source
sampling, or an industry performing its own source sampling activities.
     It is the responsibility of the supervisor to identify sources of
uncertainty or error in the measurement process for specified situations
and, if possible, eliminate or minimize them by applying appropriate quality
control procedures to assure that the data collected are of acceptable
quality.  Specific actions and operations required of the supervisor for a
viable quality assurance program are summarized in the following listing.
     1.  Monitor/Control Data Quality
         a.  Direct the field team in performing field tests according to
the procedures given in the Operations Manual.
         b.  Perform or qualify results of the quality control checks
(i.e., assure that checks are valid).
         c.  Perform necessary calculations and compare quality control
checks to suggested performance criteria.
         d.  Make corrections or alter operations when suggested per-
formance criteria are exceeded.
         e.  Forward qualified data for additional internal review or  to
user.
     2.  Evaluate Routine Operation
         a.  Obtain from team members immediate reports of suspicious
data or malfunctions.  Initiate corrective action or, if necessary, specify
special checks to determine the trouble; then take corrective action.
Document the corrective action taken.
         b.  Examine the team's log books periodically for completeness
and adherence to operating procedures.
         c.  Approve data sheets,  calibration checks, etc., for  filing.
                                   66

-------
     3.  Evaluate Overall System
         a.  Evaluate available alternative(s) for accomplishing a given
objective in light of experience and needs,
         b.  Evaluate personnel training/instructional needs for specific
operations.
     Consistent with the realization of the objectives of a quality
assurance program as given in section I, this section provides the super-
visor with brief guidelines and directions for:
     1.  Collection of information necessary for assessing data quality
on an intrateam basis;
     2.  The use of performance criteria to insure the collection of data
of acceptable precision/accuracy;
     3.  Isolation, evaluation, and monitoring of major components of
system variability.
     In subsection 3.1, a method of assessing data quality on an intra-
team basis is given.  This method involves calculating a sample standard
deviation using the three replicate runs required in a field test and cal-
culating 90 percent confidence limits for the average of the three repli-
cates.
     Subsection 3.2 presents suggested criteria for judging equipment
performance, frequency of calibration, and isokinetic sampling.
     Directions for the collection and analysis of information to identify
trouble, and subsequently, the control of data quality within acceptable
limits are given in the third subsection.

3.1  ASSESSMENT OF DATA
     The particulate mass emission rate, PMR, for a particular field test
is the average of at least three replicates.  Intrateam assessment of data
quality as discussed herein provides' for an estimate of the precision of
the measurements.  Precision in this case refers to replicability, i.e.,
the variability among replicates and is expressed as a standard deviation.
This precision statement combines variability due to process changes and
to random measurement errors.   This technique does not provide
                                  67

-------
the information necessary for estimating measurement bias (see subsection
4.1'. 2 for a discussion of bias) that could occur, for example, from an
error in determining the pitot tube coefficient, nozzle, cross-sectional
area, or the orifice meter calibration.  However, if the operating
procedures given in the Operations Manual are followed, the bias should be
small in most cases.  An independent performance audit which would make
possible a bias estimate is suggested and discussed in section IV, the
Manual for Manager of Groups of Field Teams.
3.1.1  Calculating Precision of Field Data
       Each field test is comprised of at least three sample runs.  Using
the sample runs as replicates, a standard deviation can be calculated.  This
calculated standard deviation is a combined measure of the measurement and
process variabilities.  The standard deviation is calculated by
            _ f(PMR1
                - PMR)" + (PMR9 - PMR) + (PMR, - PMR)'
s{PMR}
where            s{PMR} = The calculated standard deviation for the
                          three sample runs, g/hr,
       PMR1(PMR2)(PMR3) = Particulate mass emission rate for sample
                          run 1 (2)(3), g/hr,
                    PMR = Average particulate mass emission rate of
                          the three sample runs, i.e., I/3(PMR  + PMR2 +
                          PMR3), g/hr, and
                      2 = The number of replicates minus one (degrees of
                          freedom).

3.1.2  Reporting Data Quality
     The average measured particulate mass  emission rate  (PMR)  serves  as  a
point estimate of the true a.verage particulate mass emission rate  (PMR ).
The spread in the PMR's from the  three runs  can be used to  calculate an
interval estimate of PMR  .  The procedure used here assumes  that  the mea-
sured PMR  is normally distributed about PMR   (i.e., the measurement  method
                                   68

-------
                                             2
is not biased) with a variance estimated by s {PMR}/n.  Since there is no
way of determining or knowing PMR  the internal estimate is actually applic-
able to the measured grand mean value PMR that would result if the number
of runs (n) became very large.  If, in fact, the measurement method is
unbiased then PMR  = PMR as n approaches infinity.
     It is recommended that the average particulate mass emission rate,
PMR, from the three runs be reported along with 90 percent confidence limits
for the grand mean, PMR.  The average measured value and calculated standard
deviation are used to calculate 90 percent confidence limits for PMR by

                       PMR  + 2.92 s{PMR}//n
where    PMR = The average of three replicates, g/hr.
      s{PMR} = Estimated standard deviation of PMR based on three
               replicates, g/hr.
        2.92 = 95— percentile of the Student t-distribution with
               2 degrees of freedom which yields a 90 percent
               confidence interval.
           n = The number of replicates, i.e., n = 3 for this case.
For example, if for a given field test PMR = 22.86 g/hr and s{PMR} is cal-
culated to be 1.32 g/hr, the reported value with 90 percent confidence
limits would be
                   22.86 g/hr. + (2.92)  (1.32 g/hr.)//3
or the grand mean particulate mass emission rate, PMR,  would be assumed
(with 90% confidence) to be in the interval.
                    20.6 g/hr. £ PMR £ 25.1 g/hr.

     The utility of the above statement follows from the fact that if this
procedure for computing confidence limits is followed for several field
tests, then 90 percent of the time the grand mean PMR value will be con-
tained within the given limits.   It is recommended that the 90 percent
                                 69

-------
confidence limits be reported with the Field Data Form in the Operations
Manual.

3.2  SUGGESTED PERFORMANCE CRITERIA
     Data assessment as discussed in the previous subsection is based on
the premise that all variables are controlled within a given level, thereby
guarding against large undetected biases in the measurement process.  These
levels of suggested performance criteria are the values given in the Oper-
ations Manual for determining when equipment and/or personnel variability
is out of control.  Criteria for judging performance are summarized in
Table 1.
     The following section discusses important sources of error in Method 5
and provides information on techniques for monitoring these variables to
determine if the performance criteria given in this section are being ex-
ceeded.

3.3  COLLECTION AND ANALYSIS OF INFORMATION TO IDENTIFY TROUBLE
     In a quality assurance program, one of the most effective means of
preventing trouble is to respond immediately to indications of suspicious
data or equipment malfunctions.  There are certain visual and operational
checks that can be performed while the measurements are being made to
help insure the collection of data of good quality.  These checks are
written as part of the routine operating procedures in section II.  In
order to effectively apply preventive-type maintenance procedures to the
measurement process, the supervisor must know the important variables in
the process, know how to monitor the critical variables, and know how to
interpret the data obtained from monitoring operations.  These subjects are
discussed in the following subsections.
3.3.1  Identification of Important Variables
       Determination of the particulate mass emission rate requires a
sequence of operations and measurements that yields as an end result a
number that serves to represent the average particulate mass emission rate
for that field test.  There is no way of knowing the accuracy, i.e., the
                                  70

-------
                   Table 1.  Suggested performance criteria
1.   Suggested Criteria for Equipment Performance
    (a)  Dry Gas Meter:
    (b)  Barometer:
    (c)  Thermometers:


    (d)  Stack Temperature
         Measuring System:

    (e)  Sampling Train  Leakage:


    (f)  Sample Box Heating
         System:

    (g)  Probe Heating System:
    (h)  Meter Orifice:
4QK
    (i)   Probe Nozzle Diameter:


    (j)   Analytical Balance:


    (k)   Type-S Pitot Tube:
.98 £ y 1 1-02
+ 5.1 mm Hg (+0.2 in. Hg)
+ 2.3°K (+ 5°R) at 273PK (492°R) or
(+ 7°R) at 373°K (672°R)
+ 2.3°K (+ 5°R) at 273°K (492°R) or + 4°K
(+ 7°R) at 373°K (672°R)
                  3             3
Less than 0.0006 m /min (0.02 ft /min) at
380 mm Hg (15 in. Hg) vacuum
Capable of maintaining a temperature of 120°C
(248°F) + 14°C (25°F) at laboratory conditions.

Uniform heating of probe with a
temperature of 120°C (248°F) at the exit
end at a flow rate of  354  cnr/sec (0.75
ft /min) at room temperature.

AH@ should be 46.7 + 6.4 mm H20 (1.84 + 0.25
in. H20) and not vary more than +3.8 mm H2<3
(+0.15 in. H20) over the range of operation
of 13 to 200 mm H20 (0.5 to 8 in. H20) , if a
commercial nomograph is used during sampling
to aid in maintaining an isokinetic sampling
rate.

Range of three different diameter
measurements less than .010 cm (0.004 in.).

Weigh a standard weight within +0.3 mg
of its stated weight.

C  constant within + 5 percent over working
range and each calibration check is within
1.2 percent of the original C .
6.0 < pH < 8.0
    (1)  Filter Media:

    Suggested Criteria  for Performing Equipment Calibration

    (a)  Above items (a)  through (j)  are calibrated when new and checked before
         each field test  and recalibrated any time the check results fall outside
         the prescribed performance limits.

    (b)  Item (k),  the  type-S pitot tube is  calibrated when new, before every
         third field test, or at any  sign of damage.

    (c)  Item (1),  filter media, the  pH's of a random sample of 7 out of 100
         filters are measured for each new order of filters.  The remaining
         93 filters are accepted if all 7 pH's are in the interval of 6.0 to 8.0.

    Suggested Criteria  for Percent Isokinetic

                            0.90 < I  < 1.10
                                    71

-------
agreement between the measured and the true value, for a given field test.
However, a knowledge of the important variables and their characteristics
allows for the application of quality control procedures to control the
effect of each variable at a given level during the field test, thus
providing a certain degree of confidence in the validity of the final
result.
     A functional analysis of this method of measuring the particulate mass
emission rate of a stationary source was made (see subsection 4.1)  to try to
identify important components of system error and show how these errors prop-
agate through the measurement process and influence the final result.  Results
of an evaluation study of Method 5 (ref. 15) for within-run variations
showed an average coefficient of variation of about 6 percent for twelve
runs, six of which had four sampling trains and the other six runs had
three sampling trains.  Also, collaborative tests of the method (refs. 16,
17, and 18) show within laboratory CVs ranging from 10 to 30 percent and
between laboratory CVs of 20 to 40 percent.  These results are used in
the functional analysis as an estimate of overall system error, while the
individual error components are estimated using engineering judgment in a
manner such that their combined variability is consistent with overall
system error.
     Variability in emissions data derived from multiple repetitions
include components of variation from:
     1.  Process conditions,
     2.  Equipment and personnel in field procedures, and
     3.  Equipment and personnel in the laboratory.
     In many instances time variations in source output may be the most
significant factor in the total variability.  In order to judge the rela-
tive magnitudes of measurement variability and process output variability,
process parameters should be monitored throughout the test.  Process infor-
mation is also required if the particulate mass emission rate is to be
given as a function of fuel input.  The exact process data to be obtained
are dependent upon the process being tested.  In general, all factors which
                                  72

-------
have a bearing on the emissions should be recorded on approximately a 15-
minute interval (ref. 19).  These factors include process or fuel weight
rate, production rate, temperature and pressure in the reactor and/or
boiler, control equipment, fan and/or damper settings, pressure drop or
other indicators of particulate collection efficiency and opacity of exit
plume.  Sample forms for combustion, incineration, and process sources
are' given in reference 19.
     It is most important to realize that the larger measurement errors
result from poor operator technique such as loss or gain of collected
particulate mass during sample recovery, (ref. 17), or poor orientation
and positioning of the probe during sample collection.  Such deviations
from recommended procedures cannot be evaluated or corrected for.  It is
important to observe and eliminate such occurrences while the test is in
process.
     Sources of variation due to equipment includes the type-S pitot tube
coefficient, sampling nozzle cross-sectional area, orifice meter, dry gas
meter, probe heater, non-neutral filter media, and sample box heater.
These parameters are all controlled through performance of calibration
checks before each field test, and in the case of the filter media, by
an acceptance check for new batches of filters.  Also, the probe and sample
box heaters are checked periodically during the conduction of the test.
     Important error sources checked immediately before and/or during
sample collection includes sampling train leaks, the sample gas tempera-
ture leaving the last impinger, and isokinetic sampling conditions.
     Assuming good operator technique, the error sources named in the last
two paragraphs are discussed and each one's effect on the determination of
the particulate mass emission rate is derived from a functional analysis
of the measurement process in subsection 4.1.
     A summary of the important parameters is given below.  The parameters
are roughly given in ascending order of importance.  Importance is quali-
tatively derived from the estimated error range of a parameter weighted by
its estimated frequency of occurrence.
                                  73

-------
3.3.1.1  Equipment Calibration.   Equipment calibration is the backbone of
any quality assurance program.   It is important that the calibration
procedure be carried out correctly, that the calibration standards are
properly calibrated and maintained, and that the frequency of calibration
is adequate.
     Important calibration constants and how they influence measurement
accuracy include the following:
     1.  Error in the pitot tube calibration coefficient is directly
reflected in the stack gas velocity determination and is doubled in the
process of determining isokinetic sampling rates.  This error could be very
large if the pitot tube is not calibrated under actual field test condi-
tions, i.e., strapped to the sampling probe and the spacings shown in
Figure 5-1 of Appendix A are not maintained (ref. 7).  Errors as large as
20 percent have been attributed to the pitobe configuration (ref. 7),
     2.  Error in determining the average nozzle diameter is quadrupled
in the process of determining isokinetic sampling rates and is doubled in
the percent of isokinetic sampling calculation.  One source of error here
is the use of an out-of-round nozzle.  The average nozzle diameter is used
to calculate the area of a circle which yields a larger than true cross-
sectional area if the nozzle tip is not round,
     3.  Dry gas meter inaccuracy appears directly in the concentration
and particulate mass emission rate determinations.
     4.  The orifice meter calibration constant is used in determining
isokinetic sampling conditions and any error in the constant is doubled
in setting the sampling rate..  Also, if AH@, the pressure drop across
                                            3             3
the orifice that gives a flow rate of 0.21 m /min (0.75 ft /min) at 21°C
(70°F) and 760 mm Hg (29.92 in.  Hg) differs from 46.7 mm H20 (1.84 in. HO),
and a nomograph is used to set isokinetic sampling conditions, an error
results.  It is recommended that an orifice meter with a AH@ outside the
range of 40.4 to 53.1 mm H^O (1.59 to 2.09 in. ELO) not be used in conjunc-
tion with a nomograph.
                                    74

-------
3.3.1.2  Anisokinetic Sampling.  Anisokinetic sampling can occur from error
in the calibration constants of the pitot tube, orifice meter, and nozzle
diameter.  It can also result to a lesser degree, usually, from measurement
error in the moisture content and molecular weight of the stack gas.
Errors from the above sources will not be directly reflected in the per-
cent of isokinetic sampling calculation.  Therefore, it is important to
determine each parameter as accurately as possible, either through cali-
brations or careful measurements.
     Failure, or in some instances the inability, to make adjustments in
the sampling rate as the stack gas velocity varies or as the deposited
particulate matter plugs the filter can result in anisokinetic sampling.
Use of a nomograph can be a cause of anisokinetic sampling because of
(1) any inaccuracy in the nomograph, (2) use of preset values for C , AH@,
and M, (these errors can be eliminated by using actual values and adjusting
the correction factor on the nomograph), and (3) operator error in setting
the nomograph.  The sum of these errors is quantified to a certain extent
by the percent of isokinetic sampling calculation.
     Deviation from isokinetic sampling cannot be related directly to error
in the measurement process (see subsection 4.1).  However, failure to main-
tain isokinetic sampling conditions under otherwise normal operations
reflects the lack of alertness and, perhaps even the level of competency,
of the field crew.
3.3.1.3  Sample Recovery.  The technique used by, and the attitude of,  the
crew members in sample recovery are of paramount importance to measurement
precision and accuracy (refs.  17 and 18).  Use of an adequate sample
recovery area in terms of space, lighting, or cleanliness will decrease the
probability of error.   Sample recovery procedures as given in Section 4.2
of Appendix A should be followed by the field team.
3.3.1.4  Calculations.  Calculations for this method are known to be a
major source of error (ref.  18).  Some calculations involve several terms and
should only be attempted (for the final report) at a desk or work table and
preferably with the aid of a calculator or at least a good slide rule.   A
computer program using raw data as an input is highly recommended for
                                   75

-------
making the final calculations.
     As a check, it is recommended that all calculations be independently
repeated from raw data.
3.3.1.5  Filter Media.  This is included as a possibility.   It is not known
how important the pH of the filter media is at this time.  However, data
referenced in subsection 4.1 indicates that error due to the conversion of
acid gases to particulate ma.tter by alkaline filters could be significant.
This error would be a positive bias resulting in a measured emission rate
greater than the true rate.

3.3.2  How to Monitor Important Variables
     In general, if the procedures outlined in the Operations Manual are
followed, the major sources of measurement variability will be in control.
It is felt, however, that the supervisor should visually check certain
parameters and operations periodically while measurements are being made
to insure good operator technique and the proper use of equipment.  The
parameters and operations to check are essentially those recommended for
the auditor as listed in table 7 of subsection 4.3.
     Results of the calibration checks for the dry gas meter, orifice
meter, nozzle diameter, and pitot tube should be checked before each field
test.  Any item of equipment not satisfying the suggested performance
criteria of table 2 should be calibrated or replaced.
     There appears to be a need for actual field data on several of the
parameters or variables involved in this measurement method in order to
better judge their influence on measurement variability.  One of the most
effective means of identifying and quantifying important sources of
variability is through the use of quality control charts.  Quality control
charts will provide a basis for action with regard to the measurement
process; namely, whether the process is satisfactory and should be left
alone, or the process is out of control and action should be taken to find
and eliminate the causes of excess variability.  In the case of this method
in which documented precision data are scarce, the quality control charts
can be evaluated after a period of time to determine the range of variation
                                   76

-------
that can be expected under normal operating conditions.  Also, even though
results from individual field tests are within bounds, trends can be identi-
fied and corrective action taken further improving data quality through the
proper use of control charts.
     Discussions of control charts and instructions for constructing and
maintaining them are given in many textbooks in statistics and quality
control, such as in references 20 and 21.  Also, volume 1 of the Quality
Assurance Handbook for Air Pollution Measurement Systems published by EPA
discusses the use of control charts (ref. 22).
     It is good practice to note directly on control charts the reason for
out-of-control conditions, if determined, and the corrective actions taken.
Recommended control charts are discussed below.
3.3.2.1  Pitot Tube Calibration Coefficient.  A sample control chart for
pitot tube calibration checks is given in the quality assurance document
of this series for Method 2 (ref. 1).
3.3.2.2  Determination of %CO? with Orsat Analyzer.  For incinerators
where the particulate concentration or particulate mass emission rate is
corrected to 12 percent CO-, it is recommended that control charts for the
field replications and for calibration checks be maintained as given in
the quality assurance document of this series for Method 3 (ref. 2).
3.3.2.3  Range Chart for Runs.  In compliance testing where it is desired
to determine the source output at a fixed level of operation, a large range
in the three runs (replicates) would suggest process variability and/or
measurement variability.  Expressing the range, R, as a percent of the
average, i.e., the difference in the largest and smallest of the three
replicates divided by the average of the three replicates, all multiplied
by 100; a control chart with limits as given in Figure 5 can be used
initially.  Results from collaborative tests of Method 5 show within labora-
tory CV's of 10, 25, and 31 percent.  Therefore, the CV = 10 percent used
in constructing the control chart is the least of the three values reported
above.  These limits should serve as a starting point.  When a data point
falls out of bounds on this graph, the process data should be checked to
                                   77

-------
see if the process changed between runs and the percent of isokinetic
calculations checked to see if one run was significantly different from
the others in order to identify the cause of the excessive variability.
Note that exceeding the upper control limit does not necessarily invali-
date the test data.
3.3.2.4.  Mean and Range Charts for Percent of Isokinetic Sampling.   Main-
taining isokinetic sampling conditions is important in particulate sampling.
Control charts displaying the range and mean of the calculated percent
isokinetic sampling provide, at a glance, means for evaluating the per-
formance of a team or groups of teams over an extended period of time.  If
deviations from isokinetic greater than + 10 percent are not allowed,
i.e., the run has to be repeated, then in a rough way 10 percent can be
taken as the 3a value giving a standard deviation of about 3.3 percent.
Based on three replicates and the above standard deviation, the range and
mean charts for I are given in Figures 6 and 7, respectively.
     The R values are plotted sequentially as they are obtained and con-
nected to the previously plotted point with a straight line.  Corrective
action, such as instruction in proper operating technique, should be
taken before the next field test any time one of the following criteria
are exceeded:
     1.  One point falls outside the UCL.
     2.  Seven consecutive points fall above the R line (i.e., the range
of I obtained by a given field team is consistently greater than R for
seven or more field tests).  Exceeding the first criteria will usually
indicate poor technique or equipment malfunction between sample runs of
a particular field test.  Exceeding the second criteria indicates a
systematic error due to equipment bias or poor technique.  (Note that the
UCL can be exceeded without violating the I = 100 + 10 interval for any
one run.)
     The I values, i.e., average percent of isokinetic sampling per three
sampling runs, are plotted sequentially as they are obtained from field
tests and connected to the previously plotted point with a straight line.
Corrective action, such as instruction in proper operating technique
                                    78

-------
c
111
o
EC





I

O
O



X


cc
     50
     40
     30
     20
     10
FIELD TEST
NO.
DATE
FIELD TEAM
PROBLEM

AND
CORRECTIVE
ACTION






















1





























2





























3





























4





























5





























6





























7


c

c
8 £
"D 'O
% CO
cu ra
-D t3

O S
C CD

"^ ^
0 01
o —
v> .¥?
1- (—
0) *~
£ cX
CD C
TO E
Q.
C
K) <"
0 I
o S
fL O

8




























9




^
C
*-
O

^$
o
CO
CO
CD


3

o
CD
C
y
O
.i2
•M
C
0)
CD
Q_

C

CD
%
QJ
-C

*
"O
CD
-o
c
CD
trt
O>
c^
'*"' "O
±: CD
-1 »
CD Q
c QJ
0 ^
V o
C
- t/>
^ OJ
a. ?

10




























                     *UCL = D2a = 4.358 X  10 = 44


                     tR = d2a = 1.693 X  10 = 17





       Figure 5.   Sample control for the  range,  R,  of PMR replicates.
                                    79

-------
    c
    0)
     c
     'E
     X
     ra
     E
    en
    C
    cr
18

16

'14
12

10
 8
 6

 4
 2
                                       UCL = 14.4"
FIELD TEST
   NO.
                                                              10
  DATE
FIELD TEAM
 PROBLEM
   AND
CORRECTION
  ACTION
                        *UCL = D2cr = 4.358 X 3.3 = 14.4
                        fR = d20 = 1.693 X 3.3 = 5.6
           Figure  6-   Sample control chart for the range,  R,  of percent
                       isokinetic,  I, sampling for three  test  runs per
                       field test.
                                     80

-------
 u
 CJ
Q_
s-\
IM

 o
 -t-j
 cu
     <
            106
            104
            102
            100
            98
            96
            94
                                      UCL = 105.7*
                                      Warning Limit = 103.6
                                      Warning Limit = 96.2
                                      LCL = 94.3
FIELD TEST NO.
                                                                        10
    DATE
  FIELD TEAM
 PROBLEM AND
  CORRECTIVE
     ACTION
                               *UCL = I + 30{I} = 100 + 3 X 3.3/>/3~'= 105.7


                   Figure 7.   Sample control chart  for the average percent of
                               isokinetic  sampling per field test.
                                            81

-------
and/or performing equipment calibration checks should be taken before
attempting the next field test any time one of the following criteria is
exceeded.
     1.  One point falls outside the UCL or LCL.
     2.  Two out of three consecutive points fall in the warning zone
(between 2a and 3a limits).
     Exceeding the first criteria will usually indicate poor technique
or equipmerit malfunction.  The second criteria when exceeded indicates
an assignable source of variability due either to faulty equipment or a
consistent error in performing the operation procedures.
                                    82

-------
                SECTION IV
MANUAL FOR MANAGER OF GROUPS OF FIELD TEAMS
                      83

-------
SECTION IV     MAI FOR WNAGER OF GROUPS OF FIELD TEW1S

4.0  GENERAL
     The guidelines for managing quality assurance programs for use with
Test Method 5 - Determination of Particulate Emissions from Stationary
Sources are given in this part of the field document.  This information is
written for the manager of several teams for measuring source emissions and
for the appropriate EPA, State,  or Federal Administrators of these programs.
It is emphasized that if the analyst carefully adheres to the operational
procedures and checks of Section II, then the errors and/or variations in
the measured values should be consistent with the performance criteria as
suggested.  Consequently, the auditing routines given in this section
provide a means of determining whether the stack sampling test teams of
several organizations,  agencies, or companies are following the suggested
procedures.  The audit function is primarily one of independently obtaining
measurements and performing calculations where this can be done.  The pur-
pose of these guidelines is to:
     1.  Present information relative to the test method (a functional
analysis) to identify the important operations and factors.
     2.  Present a methodology for comparing action options for improving
the data quality and selecting the preferred action.
     3.  Present a data quality audit procedure for use in checking
adherence to test methods and validating that performance criteria are
being satisfied.
     4.  Present the statistical properties of the auditing procedure in
order that the appropriate pLan of action may be selected to yield an
acceptable level of risk to be associated with the reported results.
     These four purposes will be discussed in the order stated in the
sections which follow.   The first section will contain a functional analy-
sis of the test method with the objectives of identifying the most important
factors which affect the quality of the reported data and estimating the
expected variation and bias in the measurements resulting from equipment
and operator errors.
                                    84

-------
     Section 4.2 contains several actions for improving the quality of the
data; for example, by improved analysis techniques, instrumentation, and/or
training programs.  Each action is analyzed with respect to its potential
improvement in the data quality as measured by its precision.  These
results are then compared on a cost basis to indicate how to select
the preferred action.  The cost estimates are used to illustrate the metho-
dology.  The manager or supervisor should supply his own cost data and his
own actions for consideration.  If it is decided not to conduct a data audit,
sections 4.1 and 4.2 would still be appropriate as they contain a functional
analysis of the reference method and of alternative methods or actions.
     There are no absolute standards with which to compare the routinely
derived measurements.  Furthermore, the taking of completely independent
measurements at the same time that the routine data are being collected (e.g.,
by introducing two sampling probes into the stack and collecting two samples
simultaneously) is not considered practical due to the constrained environ-
mental and space conditions under which the data are being collected.
Hence, a combination of an on-site systems audit, including visual observa-
tion of adherence to operating procedures, and a quantitative performance
audit is recommended as a dual means of independently checking on the
source emissions data.
     The third section contains a description of a data quality audit pro-
cedure.  The most important variables identified in section 4.1 are considered
in the audit.  The procedure involves the random sampling of n stacks from
a lot size of N = 20 stacks (or from the stacks to be tested during a three-
month period, if less than 20) for which one firm is conducting the source
emissions tests.  For each of the stacks selected, independent measure-
ments will be made of the indicated variables.  These measurements will be
used in conjunction with the routinely collected data to estimate the
quality of the data being collected by the field teams.
     The data quality audit procedure is an independent check of data col-
lection and analysis techniques with respect to the important variables.
It provides a means of assessing data collected by several teams and/or firms
with the potential of identifying biases/excessive variation in the data
collection procedures.  A quality audit should not only provide an independent
                                    85

-------
quality check, but also identify the weak points in the measurement
process.  Thus, the auditor, an individual chosen for his background
knowledge of the measurement process, will be able to guide field teams in
using improved techniques.  In addition, the auditor is in a position to
identify procedures employed by some field teams which are improvements
over the current suggested ones, either in terms of data quality and/or
time and cost of performance.  The auditor's role will thus be one of
aiding the quality control function for all field teams for which he is
responsible, utilizing the cross-fertilization of good measurement tech-
niques to improve the quality of the collected and reported data.
     The statistical sampling and test procedure recommended is sampling
by variables.  This procedure is described in section 4.4.  It makes max-
imum use of the data collected, and it is particularly adaptable to the
small lot size and, consequently, the small sample size applications.  The
same sampling plans can be employed in the quality checks performed by a
team or firm in its own operations.  The objectives of the sampling and
test procedure are to characterize data quality for the user and to identify
potential sources of trouble in the data collection process for the purpose
of correcting the deficiencies in data quality.
     Section 4.4.4 describes how the level of auditing, i.e., the sample size
n, may be determined on the basis of relative cost data and prior information
about the data quality.  This methodology is described in further detail in
the Final Report on the Contract.  The cost data and prior information con-
cerning data quality are supplied to illustrate the procedure and these data
must be supplied by the manager of groups of field teams depending upon the
conditions particular to his responsibility.
     Figure 8 provides an overall summary of the several aspects of the data
quality assurance program as described in these documents.  The flow dia-
gram is subdivided into four areas by solid boundary lines.  These areas
correspond to specific sections or subsections of the document as indicated
in the upper right hand corner of each area.  The details are considered
in these respective sections of the document and will not be described here.
                                    86

-------
                                 Pollutant
                                Measurement
                                  Method
                                 Functional
                                  Analysis
                                     I
                                                Subsection 4.1
                               Estimate Ranges
                              and Distributions
                                of Variables
                                      _L
                  Identify and Rank
                     Sources
                   Bias/Variation
                Perform Overall
                   Assessment
        Section III
Develop Standards
    for Q. C.
    Procedure
    Institute
  QC Procedure
  for Critical
    Variables
                                        Subsection 4.2
         Data
        are of
     Satisfactory
        Quality
                                              (Optional)
Evaluate Action Options
  for Improving Data
         Quality
 Continue to Use
Measurement Meth.
   as Specified
Cost of
Implementing
Actions


Select Optimal
Action and
Implement
       Modified
      Measurement
        Method
                                      Subsections 4.3 and 4.4
  Develop Standards
for Audit Procedure
Select Aud .
Procedure
Based on
Statistics
and /or
Cost





Cost Data:
Audit,
CP
cr

G'
p

                                                                Assess Data
                                                               Quality Using
                                                                Audit Data
                                                           No
                                          Data
                                         Quality
                                      Satisfactory
                                                                          Yes
   Continue to Use
 Measurement Method
    as Specified	
                 Figure 8.   Summary  of  data quality assurance
                                          87
                                   prcgran:.

-------
4.1  FUNCTIONAL ANALYSIS OF TEST METHOD

     Test Method 5 - Determination of Particulate Emissions from Stationary
Sources—as described in Appendix A of this document is subjected to a
functional analysis in this section.  This measurement method is used to
determine the concentration of particulate matter in the stack gas.   It
is also used to simultaneously determine the moisture content of the stack
gas and to perform a velocity traverse from which the volumetric flow rate
is calculated.  These results combined with the stack gas composition as
measured by Method 3 yield a particulate mass emission rate for the source
being tested.
     Method 5 as promulgated in the Federal Register, Vol. 36, No. 247 -
Thursday, December 23, 1971 has been subjected to collaborative tests on
a Portland cement plant (ref. 16), a fossil fuel-fired steam generator
(ref. 17), and a municipal incinerator (ref. 18).  These tests showed
within laboratory precisions (expressed as coefficient of variation) rang-
ing from 10 to 30 percent and between laboratory precisions of 20 to 40
percent.  Several recommendations were made for improving the precision of
the method based on the collaborative test results (refs. 16, 17 and 18).
     The method (i.e., Method 5) has been revised by EPA incorporating
the above mentioned recommendations as well as other changes that should
improve the precision of the method.  The revised method is reproduced as
Appendix A of this document.  The functional analysis presented in the
following subsections is based on what can hopefully be achieved using the
revised method.  A within laboratory coefficient of variation of 10 percent
may be achievable by highly motivated, well-trained, stack sampling teams.
     The changes and/or additions made by EPA to the method that should
result in significant improvement in data quality include:
     1.  Minimum free spaces between the pitot tube, sampling nozzle, and
temperature sensor are specified  (see Figure 5-1 in Appendix A).
     2.  Calibration of the 1;ype-S pitot tube is required prior to initial
use and at any sign of damage, plus the calibration standard, facility and
procedures are fully specified.
     3.  Greater detail on sample recovery is provided.
                                    88

-------
     4.  Sampling train leak checks are required before and after a run
         and are recommended between port changes.
     The purposes of the functional analysis as performed here are to:
     1.  To identify operations, variables and factors that can influ-
         ence the quality of the measurement data.
     2.  To illustrate how elements of uncertainty are propagated through
         the measurement process to the resultant particulate measurement.
     3.  To estimate the mean values and ranges of the various error
         sources existing under normal operating conditions and to deter-
         mine the combined probable uncertainty to be associated with
         the reported measurements.
     The results of the functional analysis provide information for the
following:
     1.  Setting acceptable limits on data quality, i.e., precision and
         accuracy.
     2.  Applying quality control procedures to those operations and vari-
         ables  that  would otherwise result in excess variability in the
         measurement data.
     3.  Applying appropriate quality assurance practices (e.g., audits)
         at critical points in the measurement process with acceptable
         limits specified and actions to be taken when limits are exceeded.
     The functional analysis is discussed in two stages.   First the vari-
ables and operations involved in the measurement process are identified
and modeled, i.e., their mean values and variances are estimated.  These
estimates are made using published data if available or engineering
judgment if no quantitative data are available.  Second,  a variance analysis
(sometimes referred to in the literature as a sensitivity analysis or
error analysis) is performed to determine the individual and combined
influence of the variables and operations to the particulate mass emission
rate measurement.
     The variance analysis as presented in this section provides a mathe-
matical means of identifying important variables in the measurement pro-
cess.  The estimates of the mean values and variances of the variables
                                   89

-------
are made as realistic as possible, however, the major purpose of this sec-
tion is to illustrate a method.  Each laboratory should work through the
analysis using experimental data or estimates based on conditions within
that laboratory.  The mathematical basis for the procedures are described
in the Final Report on Contract 68-02-0598 (ref. 4).
     The particulate mass emission rate (PMR) is calculated from the rela-
tionship :
                    PMR = Hf3g/mg (m/V) (V  • A)         (1)
where
       PMR = Rate of particulate emissions, g/hr.
        m  = Total weight of particulate collected, mg.
         n                                                            3
   V ,  ... = Volume of gas sampled corrected to standard conditions, m .
        V  = Stack gas velocity, m/s.
         s                                 2
        A  = Crossectional area of stack, m .
         S
Variability in the measured PMR will have components of variability from
the individual determinations of m , V ,   ,. ,  V  and A .  Variability of
                                  n'  m(std)    s      s             y
each of the four terms is discussed separately below following a short
definition of terms.
     Many different measures of variability are conceivable depending
upon the circumstances under which the measurements are performed.  Three
measures of variability are defined here.  They are repl icability, repeat-
ability and reproducibility defined as follows (ref. 22).
     1.  Replicability.  The precision measuring the variability among
replicates.  Replicates are repeated but independent determinations of the
same sample, by the same analyst, at essentially the same time and same
conditions.  This could apply to the three runs comprising a field test
provided the process variables remained constant.
     2.  Repeatability is a measure of the variability in determinations
made on the same sample (i.e., the same source with source parameters held
as constant as possible) by the same field team using the same equipment
over a short period of time.  The repeatability standard deviation and the
coefficient of variation are symbolized by a  and CV  respectively.  This
                                    90

-------
measure of precision is referred to as the within laboratory standard
deviation in the collaborative test reports.
     3.  Reproducibility is the variability associated with measurements
made of the same sample (i.e., same source with source parameters held as
constant as possible) by field teams from different laboratories.  This
measure of precision is referred to as between laboratory precision in the
collaborative test reports.
     The above definitions are based on a statistical model where each
determination of the rate of emissions is the sum of three components as
follows:
                           PMR = PMR + b + e                         (2)

where
        PMR = the measured rate of particulate emissions, g/hr.
        PMR = the general or true average, rate of particulate emissions,
              g/hr.
          b = an error term representing the differences between field
              teams equipment, sources, etc., g/hr.
          e = a random error occurring in each measurement, g/hr.
In general, b can be considered as the sum:
                             b = b  + b                              (3)
                                  r    s

where
                      b  = random component
                      b  = systematic component
                       S
The term b is considered to be constant during any series of measurements
performed under replicability conditions, e.g., the three runs making up
a field test.  It behaves as a random variate in a series of measurements
during which personnel, equipment or conditions change e.g., between field
tests or laboratories.  Its variance is denoted by

                            var b = a,                                (4)
                                     b
                                    91

-------
       2
where a  is the bias component of variability due to different field teams.
equipment, etc.
     The term e represents a random error occurring in each measurement.
Its variance is denoted by
                                      2
                             var e = a                               (5)
       2
where a  is called the replicability variance.
     The repeatability standard deviation, a , is related to the bias
variance and the replicability variance and the number of replicates r
by
                              V
     Repeatability of particulate mass emission rate determinations will
be discussed in the following, subsections.

4.1.1  Mass of Particulate Collected, m
     The total measured particulate mass, m , is given by
                           m  = m  + e,                              (7)

where m  represents the true particulate mass in the gas volume at stack
conditions equivalent to the volume V ,   ,x as measured by the dry gas
                                     m(.std;
meter and corrected to standard conditions.  The difference between the
true and measured values is the error, e.
     Determination of particulate mass is subject to error from
     1.  Loss or gain of sample during sample recovery (SR),
     2.  Weighing of collected sample (W),
     3.  Conversion of acid gases to particulates by alkaline glass fiber
filters (pH),
     4.  Formation of particulates due to non-uniform or inadequate heating
of the probe and/or sample box (C), and
     5.  Deviation from isokinetic sampling (I).
     These five components of variability are independent  (at least there
                                    92

-------
are no obvious correlations) and with each component's effect an m  given
in mg the variance of m  becomes:

       a2(m } = a2  (m } + 02{m } + a2 {m } + a2{m } + a2{m }.       (8)
           n      SRn     Wn     pHn     en     In

     Magnitudes of each of the five variance components are discussed in
the following subsections.  Using the variances, as estimated in the fol-
lowing subsections, in the above relationship gives a total variance for
m  of
 n
        a2{mn> = 0.0016 x m2 + 0.0016 x m2 + 9 yg2 + 4 yg2 + 0.0034 x m2.

By rearranging and combining terms the variance becomes
                   a2{mn> = 0.0066 m2 + 13 mg2.                      (9)

     Values of cr{m } and CV{m } for different values of true particulate
                  n          n
mass, m , are given in a table in subsection 4.1.1.6.
4.1.1.1  Sample Recovery (SR).  Error due to a loss_or gain of sample dur-
ing sample recovery is mostly a function technique and of the adequacy of
the work area used for sample recovery.  Sample recovery includes any
excess sample due to scraping the probe against the stack wall or sampling
port as well as transferring the filter and collected particulate from the
filter holder to a sample container and removing particulate matter from
the nozzle, probe, filter holder, and connecting glassware.  No quantita-
tive data are available for estimating the magnitude of this error.  How-
ever, it was considered to be a major source of error by those conducting
the collaborative tests (refs. 16, 17, and 18).  For this analysis an error
proportional to the true mass, m , is assumed.  A relative error (coefficient
of variation) of 4 percent given a stand deviation of acr){m } = 0.04 x m  mg
                   2                  22                n
and a variance of ac_{m } = 0.0016 x m  mg .  It is further assumed that
                   I>K  n              t
over a large number of field tests there will be as many positive as
negative errors i.e.,  this error can be modeled as a normally distributed
                                              2
variate having a zero mean and a variance of cr  {m }.  This is symbolized
         ~                 n                  SR  n
as N(y, o ) = N(0, 0.0016 m).
                                    93

-------
4.1.1.2  Weighing Errors (W).   Sample weighing errors are a combination of
four weighings.  The weight of particulate matter collected m  is

                         m  = (W0 - W.) + (W. - W,)                   (10)
                          n     /    1      H    J

where
        m  = The collected mass of particulate matter, mg
        W, = The tare weight of the filter, mg
        W7 = The weight of the exposed filter, mg
        W., = The tare weight of a beaker or drying dish, mg, and
        W, = The gross weight of the beaker and the particulate
             material collected in the probe, mg.
     If the recommended procedures are followed for checking the balance
measurements against measurement standards before each weighing, the
associated weighing errors for each of the weighings, W\., W^, W^, and W^
would most likely result from improper conditioning and handling rather
than from the balance.  Under this assumption the weighings are uncorrelated
and the variances can be combined as follows.

       a2 {m } = a2{W.,} + a2{W.} + a {W-} +  a {W. }                     (11)
        w   n        1        /        3        4

     Weighings W, and W., are ta.re weighings  and should have greater pre-
cision than weighings W, and W., which  involved the particulates recovered
from the probe assembly and the filter, respectively.  These latter weigh-
ings are  sensitive  to the type of particulates i.e.,  if  they are hygro-
scopic (ref 17) or  of high organic content.   Rather  than estimate the
individual weighing errors  the total standard deviation  of m  attributable
to weighing operations  is estimated to be  4  percent  of the true particulate
                                                     2              2
mass,  i. e., a  {m  }  = 0.04 x m  mg or a variance of a  {m  } = 0.0016 m  .
             w n            t                      w n           t
4.1.1.3   Filter Surface Alkalinity  (pH).   The surface of glass fiber  filters
is generally alkaline with  pH's ranging from about 7  to  11.  Acid gases  in
the sample air can  be oxidized and deposited as particulate matter on
these  filters.  The quantity of pseudo-particulates  formed is probably a
                                    94

-------
function of the filter pH, concentration of the acid gases in the sample
gas, residence time, and duration of the sampling period.  Tests dealing
with measuring suspended particulates in ambient air showed a much higher
particulate catch when using filters with a pH of 11 as compared to filters
with a pH of 6.5 (refs. 23 and 24).  One series of nine tests involving
samplers operated side by side, one with a pH-11 filter and the other with
a pH-6.5 filter, showed an average particulate catch 18 percent greater
for the alkaline filters (ref. 23).  A glass fiber filter used as a back-
up to a cloth primary filter in a sampling train showed a weight gain due
to soluble sulfates as large as the total particulate catch of the primary
filter (ref. 25).
     The above data on alkaline fi-ters are not directly applicable to this
application, thus an error limit would be strictly an estimate.  For
this analysis a range of from 0 to 9 rag is assuemd as the potential gain
in particulate matter due to conversion of acid gases on the filter sur-
face.  This error acts as a positive bias and is modeled as the absolute
                                                                      2
value of a normal distribution with a zero mean and a variance of 9 mg  or
a standard deviation of a  {m } = 3 mg, i.e.,  |N(0, 9 gm)|.  Such a distri-
                         pn  n
bution (taking absolute values) has a mean value of approximately + 2.4 mg
and cannot have a negative value.
4.1.1.4  Condensation (C).  Hemeon and Blank (ref. 25) discuss the pos-
sibility of pseudo-particulate matter being formed in the probe prior to
the filter by oxidation of SO^ in the sample gas.  This could occur if the
probe is not uniformly heated and  condensation occurs, followed by heating
and revaporization.  Also, many compounds pass from the gaseous to the solid
phase between 93°C to 148°C (200 to 300°F) (ref. 26); thus, sampling trains
performing at different operating  temperatures could generate biased data.
Insufficient data are available to model this source of error.  Therefore,
just to include it as a significant error, it is treated as a normally
distributed random variable with a 4 mg mean and a standard deviation of
                        2
2 mg, i.e., N(4 mg, 4 mg ).   Under these conditions, it acts generally as
a positive bias but could go negative simulating a probe operating above
120°C (248°F), for example.
                                    95

-------
4.1.1.5" Nonisokinetic Sampling (I) .   Deviation from isokinetic sampling
conditions may result in particulate  measurement error.   The magnitude
of error depends on the degree of departure from isokinetic conditions,
and on the particle size distribution in the sample gas.   Departure from
isokinetic sampling can occur due to  failure to adjust the nozzle velo-
city as the stack gas velocity varies.   This type of departure will be
detected when the percent of isokinetic sampling is calculated.  However,
errors in the pitot tube coefficient  and/or in the nozzle diameter can
cause deviations from isokinetic conditions which are not detectable from
any checks that can be performed while in the field.
     The degree of deviation from isokinetic sampling is not a direct
indication of the error in the final  result.  The error resulting from
nonisokinetic sampling is a function  of the particle size distribution in
the stack.  For gases and small particles (diameters <^ 5 ym) isokinetic
sampling is not necessary (ref. 27).   Sample gases with particle size
distributions extending in the 25 ym  and above sizes are sensitive to
anisokinetic sampling.  Each particle size distribution has to be evaluated,
For this analysis, using a particle size distribution of 80 to 100 ym
particles (ref. 19) a variation of +_ 5 percent from isokinetic sampling
shows a relative variation of approximately + 10 percent in the collected
mass or a ratio of 2 to 1.  For this  analysis a 1 percent deviation from
isokinetic conditions is taken to be  a 2 percent error in the measured
particulate concentration, i.e.,
                          T{iri } = 2 x CV{I} x m .
                          In                 t
     Percent of isokinetic sampling is derived from the ratio of the gas
velocity in the nozzle to the stack gas velocity in the stack by
                               I = V /V .                           (13)
                                    n  s
The component of variability in m  due to nonisokinetic sampling is taken
as
                                    96

-------
                      oT{m } = 2 x CV{V /V } x m .
                       In            n  s     t
                                                              (14)
     The coefficient of variation CV{V /V } is derived in the following
                                      Tl  S
manner.
     The estimated coefficient of variation of V  based on
                                                n
                                                      1/2

—
n
4 K
m
,D2
n
1
1
- B
wm
- B
ws

T AH
m
P M
m m
                                                                     (15)
is given by
CV2{V
                     n
                 ~ CV{K
                               m
4CV2{D
                                          n
            CV{1 - B
                                               CV{1 - B
                                                        wm
                                     ws
                                    0.25(CV{T
                                                     m
                     CV2{P
                                 m
                                      CV2{M
                                           m
                                                          CV2{AH)
                                 (16)
where
 V  = Sample gas velocity in the nozzle.
 D  = Average nozzle diameter.
B   = Water vapor in sample gas at the dry gas meter (taken as
      zero for this analysis).
B   = Water vapor in the sample gas by proportion.
 T  = Absolute temperature at the dry gas meter.
 P  = Ambient pressure at the meter.
 M
         m
             Molecular weight of the sample gas at the meter.
        AH = Pressure drop across the sampling train orifice.
        K  = A constant whose relative error depends on the errors in
         m                                     r
             the individual measured values in the equation.
     Table 2 gives the assumed mean values and the estimated coefficients
of variation of the individual parameters in the above equation.
     Substituting the estimated CV's from Table 2 into the above equation
16 yields a coefficient of variation for V  of

                               CV{V } = 2.04%.
                                   n
                                   97

-------
     Table 2 .   Means and variabilities of parameters affecting V
                                                                n
Parameter
K
m
D
n
1 - B
wm
1 - B
ws
T
m
AH
P
m
M
m
V
s
V
n
Mean
Metric
1.165 x 10~3
.635 cm
0.0
0.90
294°K
102 mm H20
762 mm Hg
30 g/g-mole
15.24 m/sec
15.24 m/sec
Value
(English)
(1.84)
(0.25 in)
(0.0)
(0.90)
(530°R)
(4.0 in H20)
(30.0 in Hg)
(30 Ib/lb-mole)
(50 ft/sec)
(50 ft/sec)
Estimated
CV
CV{K }
m
CV{D }
n
0.0
CV{1 -
CV{T }
m
CV{AH)
CV{P }
m
CV{M }
m
CV{V }
s
CV{V }
n
= 1.0%
= 0.5%

B } = 1.2%
wo
= 0.5%
= 1.0%
= 0.3%
= 1.0%
= 2.07%
= 2.04%
     A functional analysis of Method 2—Determination of Stack Gas Velocity


and Volumetric Flow Rate (Type S pitot tube)—was made and reported in


reference 2.  The results of that analysis is used here without repeating


the analysis.  A coefficient of variation of



                            CV{V } = 2.07%
                                s



was derived for the stack gas velocity determination.


     Using CV{V } and CV{V } the coefficient of variation for the ratio
               ii          s

V /V  becomes
 n  s
                      cv{v /v
                          n  s
n
                             (17)
or
                      CV{V /V } = 2.91%
                          n  s
                                    98

-------
     The average value of V /V  = I = 100, therefore
                           IT  S
                         CV{I} = 2.91%.
     The component of variability of m  due to nonisokinetic sampling as


given by equation 12 becomes




                     o2{m } = 0.0034 x m2 ,
                         n              t



yielding a standard deviation of
                     aT{m } = 0.0582 x m   .
                      In              t
                                                  (18)
4.1.1.6  Summary of Errors in Measured Particulate Mass, m_.  Using  the
                                                 "  ••-'-•—  "   -Q


variance components derived in subsections 4.1.1.1 through 4.1.1.5,  the
variance of m  is
             n
                     o2{mn} = 0.0066 m2. + 13 mg2.
                                                  (19)
     The variance, standard deviation, and coefficient of variation for


different values of m  are given in the following table
m
t
100 mg
200 mg
400 mg
600 mg
Volume of Gas
a {m }
n
79 mg2
277 mg2
1069 mg2
2389 mg2
Measured by
a{m }
n
8.9 mg
16 . 6 mg
32.7 mg
48.9 mg
the Dry Gas Meter
CV{m }
n
8.9%
8.3%
8.2%
8.1%
and Corrected to Standard
Conditions, V , _, .
     The sample volume measured by the dry gas meter and corrected to


standard conditions is given by (equation 5-1 is Appendix A).
                   V
                                      ^
                                      bar
                                          + AH/13.6
 /  l^
m(std)
                                m
                                            m
                                                                     (20)
                                   99

-------
(See definitions of terms in Section 6.1 of Appendix A.)
     Variability in V  is a combination of variability of the dry gas meter,
inaccuracy of the calibration standard  (i.e., wet test meter), and sampling
train leaks, including those leaks undetected because of pump valve float.
Assuming coefficients of variation of 1 percent, 0.4 percent, and 0.5 per-
cent for the dry gas meter, calibration standard, and sampling train leaks,
respectively, results in a CV{V } = 1.2 percent.
                               m
     CV{P   } = 0.3 percent and CV{T } = 0.5 percent are assumed from pre-
         Dei IT                        ID.
vious documents of this series (ref. 2).
     Variability in AH is believed to be primarily due to reading error
(inclined manometer) and calibration error in determining AH@ (AH@ is the
                                                            3
pressure drop across the orifice meter resulting in a 354 cm /sec (0.75
ft /min) flow rate at standard temperature and pressure).  The pressure
drop across the orifice, i.e., AH, relatively constant with no fluctua-
tions and hence, easily read on an inclined manometer.  Also, random
reading error is averaged out because AH as used in the equation is an
average of at least 12 readings.  Therefore, the variability of the average
pressure drop should be adequately characterized by a coefficient of varia-
tion of 1 percent, i.e., CV{AH} = 1 percent.  These assumptions are sum-
marized in table 3.  The estimated variance of V ,  ,, , as given by equa-
tion 20, is

CT^V /  ^ ~ 1-004 a2{V } + 4.02 a2{P,   } + 0.0129 a2{T } + 0.0217 a2{AH}. (21)
    m(std)              m             bar               m

     Using the estimated means and standard deviations of table 4 (in English
                                             2
units) the estimated variance of V  /  n, is a {V /  ,N} - 0.644 and the
                                  m(std)        m(std)
standard deviation a{V  ,   ,.} - 0.8 ft^.  The estimated mean is
                      m(std)

                             Vstd) = 1'7 ^ (6° ft3)

resulting in a coefficient of variation of 1.3 percent (= 0.8 x 100/60).
The most important variable in the determination of V ,  ,,  under the stated
                                                     m(std)
assumptions is clearly V .
                                   100

-------
           Table  3.  Means and variabilities of parameters in
                     determining the sample gas volume
Parameter Mean value
V V = 1.70 m3
mm
(60 ft: )
P,_ P, = 760 mm Hg
bar bar
(29.92 in. Hg)
T T = 294°K
m m
(530°R)
AH AH = 100.6 mm H20
(4 in. H20)
Coefficient of Standard
variation deviation
CV{V } = 1.2% a{V } = 0.02 m3
m m
(0.72 ft
CV{P, } = 0.3% a{P, } = 2.3 mm
bar bar
(0.09 in.
CV{T } = 0.5% a{T } = 1.5°K
m m
(2.65 °R)
CV{AH} =1.0% a{AH} = 1.0 mm H2
(0.04 in.

)
Hg
Hg)

0
H20)
4.1.3  Volumetric Flow Rate, Qs.
     A functional analysis of the method used to measure volumetric flow
rate was made in the quality assurance guidelines document for Method 2
(ref. 1).  Volumetric flow rate is given by the product of the stack gas
velocity, V  , and the cross sectional area of the stack, A .  The results
           s                                              s
of that analysis will be used here without repeating the analysis itself.
A coefficient of variation of 2.33 percent was derived for the volumetric
flow rate.
     That is,
                         CV{Qs> = CV{Vs-As} = 2.33%.
4.1.4  Precision of Particulate Concentration Determinations, C_.
       ——^   ..._ ., ~ ._  „g
                                                                  3
     The concentration of particulate matter in the stack gas, g/m , on a
dry basis corrected to standard conditions, is given by
                      Cs= (10-3g/mg) (mn/Vm(Btd)).

Using previously derived results,  the estimate precision of C  is given by
                                                             S
                      a2{C } = a2{m } + a2{V ,  ,.
                          s        n        m(std)
(22)
                                   101

-------
       2          2
where a {m } and a {V ..   ,N} are given by equations (19) and  (21), respec-
          n          m(.std;

tively.  Substituting these results into (22) and using values of 100, 200,


and 300 mg for m  yields:
m
t
100 mg.
200 mg.
400 mg.
a{C }
s
9.0 mg.
L6.8 mg.
33.2 mg.
CV{C }
s
9.0%
8.4%
8.3%
     Variability in m  is the dominating source of variability in  the



determination of C .
                  s




4.1.5  Precision of Particulate Mass Emission Rate, PMR..




     The particulate mass emission rate is calculated by
and
PMR (g/hr) = Qo (m3/hr) x c  (g/m3)
              S            S






 CV2 {PMR} = CV2 {Qg} + CV2 {Cg}.                   (23)
     CV{Q } was derived in the Quality Assurance Document  for Method  2
         s

 (ref. 1) as 2.33 percent.  Inserting this value and  the  estimated values



 of CV{C  } from the preceding subsection  into  equation  (23),  results  in  the

       s                                  -              3
 following CVs of the PMR measurements for V  ,  ,, =  1.7  m  .






                        mt          CV {PMR}
                      100 mg,.         9.3%

                      200 mg..         8.7%

                      400 mg,,         8.6%




 The concentration factor,  C ,  is the more important of the two variables
                            S


 in equation (23), accounting for about 80 percent of the total variability


 in PMR.





  4.1.6  Summary of Functional  Analysis.




      In summary,  the most  important variables in the determination of PMR
                                    102

-------
are identified in  the diagram of  figure 9.  The coefficient of variation
for each of the important variables is given and a flow diagram  indicat-
ing how each variable influences  the pollutant mass emission rate  is  given
in the figure.  Table 4 summarizes the variance analysis  calculations.
Results for three  levels of collected particulate mass are given for  con-
centration and for particulate mass emission rate.

4.1.7  Bias Analysis
     Two bias terms were identified in the functional analysis of section
4.1.1.  They are the error in the collected mass m  due to (1)  filter sur-
face alkalinity,  and (2) condensation in the probe prior  to the  filter
by oxidation of SO™ in the sample gas.  Combining the estimated biases
of these two effects from sections 4.1.1.3 and 4.1.1.4, respectively,
yields the following overall bias in m  values.

                    t {mn> = t {PH} + t {C}                           (24)

                           = 2.4 mg + 4 mg = 6.4 mg.

     For m  = 100 mg, the bias represents an overall potential relative
bias of +6.4 percent.  However,  for m  = 400 mg, the relative bias is only
+1.8 percent (= 100 x 6.4 mg/400 mg).   Thus, the bias could be significant
for the small values of true particulate mass,  m .

4.2  ACTION OPTIONS
     Suppose it has been determined as a result of the functional analysis
and/or the reported data from the checking and auditing schemes, that
the data quality is not consistent with suggested standards or with the
user requirements.  Poor data quality may result from (1) a lack of
adherence to the control procedures given in section II—Operations
Manual, or (2) the need for an improved method or instrumentation for
taking the measurements.  It is assumed in this section that (2) applies;
that is, the data  quality needs to be improved beyond that attainable by
                                   103

-------
cv{vm} =
1 .2%
1
r
CV{V , ,.}
m(std)
1 .3%
1
r
cv{cs} =
9.0%



1.4%
1

cv{vs} =
2%
f 1
cv{vn}=
2%




r
cv{vn/vs} =
2.9%
\
r
CV{m }
n
8.9%


*-
^
CV{QS} =
2.3%
^
r
CV{PMR} =
9.3%
                       *CV{CS) determined for m  = 100 mg.


Figure 9.  Relationship  of the most important  intermediate measurements
           to  the  determination of PMR.
                                   104

-------
 





















4J
s






































60
g

O
o
-d-









g

o






g°

0
o
rH




O
4-1
CO
•rl
4-1
cfl
4-1
cn



cu
rH
ni
•H
rl
n)




















*


O
vO OO
0 O













rH
CM
,
cr
Ed


a
S
^
CO
e

^
4-1
CO
N^X
S3
>




















6-S
en
en
rH



















^-^
>"
C_>




























*


O
ON en
CO rH
*£>



















C
ca o
S




en
J3_


C





















B-S
^*
O
CM













G
•-I
»
cr
W

^-^
>
U




























*

ON
CM
O
rH 0




















C
05 t>
S





CO
^
•»-^,
pj
>




















B^S
rH

CM













1 —
rH
,
cr
W

/~-N
£5
u














&-S
r^ (N
• •
CSJ OO
O fO
O
*^"









gsO
^o rn
\& oo
0 rH
O
CM



O> ON
• •
O OO OO
o




^
oo
»
cr
Ed

/^"•v
C 5^2
S U




'fcfl
g
^^x

p^
^
en
0 en
<- g
60 ^~
60
oo s~s
i oo en
0 1
rH O OO
rH
r^
X
en ^r
« ON
en
CM rH
en
g en
-- g
60 ^~
60
00 00
1 1 SN!
0 O •*
, 	 | j 	 j .
00
k> ^J
r~~ oo
• ON
rH O
60 60
oo oo o
1 1
O O ON
rH rH
X X
en rH
oo ir>
LA O
CM
CM
.
cr
cu w
CO
03 ^
o rj ^-2
rt D v~'
rl CU >
OS o
c«
rl
cu
C!
o
c
•H CO
C U
o
a





B-S
vO
•
oo











B-S
r*^
oo






rn
•
ON





e^
CM
.
cr
Ed

^-^
cfl & ^
cu >
S o






0
prf
^
rM
                                                                                                                  c
                                                                                                                  o
                                                                                                                  C
                                                                                                                  cu
                                                                                                                  o
                                                                                                                  a
                                                                                                                  CO

                                                                                                                  4-1

                                                                                                                  rH

                                                                                                                  3

                                                                                                                  CO

                                                                                                                  CU
                                                            105

-------
following the operational procedures given for the reference method.
     The selection of possible actions for improving the data quality can
best be made by those familiar with the measurement process and by the
judicious use of the functional analysis as described in section 4.1.  For
each action, the variance analysis can be performed to estimate the vari-
ance, standard deviation, and coefficient of variation of the pertinent
measurement(s).  In some cases it is difficult to estimate the reduction in
specific variances, which are required to estimate the precisions of the
pertinent measurements.   In such cases, an experimental study should be
made of the more promising actions based on preliminary estimates of
precision/bias and costs of implementation of each action.  This preliminary
analysis would follow the methods suggested herein.
     AO:  Reference Method
     Al:  Compute PMR by sample concentration and ratio of area methods
          and average (cost of $200/20 stacks)(ref. 23).
     A2:  Crew training (cost of $1000/20 stacks)
     A3:  Use modified ORSAT (for incinerator)(cost of $200/20 stacks)
     A4:  Use programmable rainicalculator in lieu of nomographs (cost
          of $350/20 stacks).
The costs given for each action are additional costs above that of the
reference method.  The assumptions made concerning the reduction in the
variances (or improved precisions), are given in the following paragraphs
for each action.
     1.  Compute PMR by Sample Concentration and by Ratio of Area Methods
and Average, Al.  It is assumed that the error associated with anisokinetic
sampling is reduced to one-half by this action as  compared to the value
calculated by the reference method i.e., calculating by sample concentra-
tion only (ref. 23).  This assumption results in a reduction in the rela-
tive standard deviation (CV) of PMR from 9.3 percent to 5.0 percent for
m  = 100 mg.
     A nominal cost of $200 per 20 stacks is used as the cost of imple-
menting this action.  Calculations for the particulate mass emission rate
by the method of sample concentration, PMR , and for the percent of iso-
kinetic sampling, I = V /V  , are required by the reference method.  The
                       IT  o
                                   106

-------
product of PMR  and I yields the particulate mass emission rate by the
ratio of areas method, PMR .  Hence, very little additional effort is
                          3
required.
      2.   Crew Training, A2.  It is assumed that the coefficient of varia-
tion of PMR is reduced by 25 percent or,

                        CV{PMR|A2l = 0.75 CV{PMR|AO}.

     The notation CV{PMRJA2} denotes the estimated CV of PMR given that
action A2 is implemented; the vertical line being read given that, and
action following the vertical line denotes the action implemented.  This
results in a  straightforward  computation of the CVs,

              mt             CV {PMR|AO}          CV {PMR|A2}
            100 mg.             9.3%                 7.0%

In estimating a cost for implementing this action it was assumed that one
crew member sent to a source sampling school such as that conducted by the
EPA for 1 week out of a year would constitute special crew training.  The
cost of the school plus subsistence for a week was estimated to be about
1,000 dollars.   This is in excess of salary and benefits.  The cost was
prorated over 20 source tests which was taken as a reasonable number of
tests per team per year.
      3.  Use  Modified  ORSAT  (for  incinerator sources), A3.   It  is assumed
 that  the standard  deviation  of  the measurement  of %C02 is reduced from  0.4
 percent to 0 . 2 percent  (absolute).  For small values of  %C00  the true
                                                            2t
 mean  percent  CO.,,  the  effect of the error  in the determination  of %C02
 on  the correction  or adjustment in the particulate matter concentration
 is  a  dominating factor  in  the overall error in  the determination of PMR
 for low %C00  levels.   Denote C    as the adjusted value of C  , where the
           Z                  S3.                            S
 relationship  is
                              csa = c  -r  t                        (26)
                               sa    s %co2
                                   107

-------
or the relationship in the coefficients of variation is
                       cv2 {<:  } = cv2 {c } + cv2 {%co0}/r,
                             sa          s            L
(27)
where r is the number of replicates used to estimate the mean, %CO«,
assuming a {%C021 = 0.4, then CV{%cio2} = 0.4/(/r x %CC>2) for the standard
ORSAT and CV{%"C02> = Q.2/(/r x 7X0^ for the modified ORSAT.  The following
measures of precision are derived assuming r is taken as suggested in
the Quality Assurance Document for Method 3 (ref. 2) and m  = 100 mg.
%co2
2%
6%
10%
Standard ORSAT
r
12
3
3
CV {Csa}
10.7%
9.8%
9.3%
CV {PMR}
11.0%
10.1%
9.6%
Modified ORSAT
r
6
3
3
CV {C }
sa
9.9%
9.2%
9.1%
CV {PMR}
10.2%
9.5%
9.4%
     An ORSAT with 0.1 ml dimensions as depicted in figure 2 of the Opera-
tions Manual of reference 2 costs very little more than the so called
standard ORSAT.  Over a period of a year the difference in cost should be
negligible.  A cost of 200 dollars per 20 source tests is assumed for
this example.
     4.  Minicalculator in lieu of nomographs, A4.  It is assumed that the
coefficient of variation of V /V  is reduced in accordance with the follow-
                             n  s
ing equation:
                 CV {V /V |A4} = 0.80 CV {V /V |AO} .
                      n  s'                 n  s'

     An increase in precision and accuracy should be realized since
exact values of C , AH@, and M, would be used to determine isokinetic
                 P            d
conditions rather than the mean values of their expected range as are
now built into the nomograph.  Also, routine calculation errors (i.e.,
                                   108

-------
error in setting and reading the nomograph) should be greatly reduced.
The above assumed relationship must be considered in the analysis of the
variation of m , C , and PMR as described in section 4.1.1.  The corre-
              n'  s'
spending coefficients of variation of PMR for the reference method and
for action A4 are estimated as follows:
                             CV {PMRJAQ}             CV {PMR|A4}
         100 mg.                9.3%                    8.6%
         200 mg.                8.7%                    8.0%
         400 mg.                8.6%                    7.9%

A programmable mini-calculator can be purchased for about 300 dollars.
Cost of programming should be more than recovered in sampling time saved
as a result of using the calculator.  The increased cost is taken as 350
dollars per 20 source tests.

4.2.1  Comparison of Actions
     The added cost per 20 stacks is plotted as a function of the precision
of the estimated PMRs as measured by its coefficient of variation, CV{PMR}
in figure 10.  Examination of the plotted results enables one to quickly
identify the action or combination of actions which will yield results of
some desired precision.   In practice it may not be reasonable to insist
that the data be of a specified precision, but that the cost of report-
ing poor quality data is a rapidly increasing function of the data quality
for data of variability exceeding a specified value.  The selection of
the best action option then becomes a trade-off between the overall cost
and the expected precision to be achieved by its implementation.  The
cost of implementing an action plus the cost of reporting poor quality
data are added to obtain an overall cost for the action.  An assumed
function of the cost of reporting poor quality data is shown as the solid
curve in figure 10 as an illustration only.  Its exact shape and location
on the graph would have to be determined from actual cost data.  Table 5
                                  109

-------
                    CN1
                    <
                                                                                                                 Pu
                                                                                                                 ^^
                                                                                                                 >
                                                                                                                                             to
                                                                                                                                             o>
                                                                                                                                             o
                                                                                                                                             )-i

                                                                                                                                             o
                                                                                                                                             CO
                                                                                                                                             O
                                                                                                                                             4-1
                                                                                                                                             cfl
                                                                                                                                             S-i
                                                                                                                                             d)
                                                                                                                                             fi
                                                                                                                                            •H
                                                                                                                                             a
                                                                                                                                             c
                                                                                                                                            •H
                                                                                                                        O
                                                                                                                        14-1

                                                                                                                        co
                                                                                                                        C
                                                                                                                        O
                                                                                                                        •H
                                                                                                                                             c
                                                                                                                                             o
                                                                                                                                             01
                                                                                                                                             4-1
                                                                                                                                             CJ
                                                                                                                                             a;
                                                                                                                                            rH
                                                                                                                                             QJ
                                                                                                                                             CO
                                                                                                                                             C  II
                                                                                                                                             o
                                                                                                                                            •H   rsl
                                                                                                                                             CO  O
                                                                                                                                            •H  U
                                                                                                                                             O  S-5
                                                                                                                                             0)
                                                                                                                                             S-i  T3
                                                                                                                                             cx c
                                                                                                                                                05
                                                                                                                                             CO
                                                                                                                                             >  oo
                                                                                                                                             CO  O
                                                                                                                                             o  o
                                                                                                                                             a  iH

                                                                                                                                            13  II
                                                                                                                                             Q)
                                                                                                                                             0)
                                                                                                                                             M
                                                                                                                                             3
O
O
CM
O
O
O
O
O
OO
O
o
o
o
o
o
CN
                                         03
                                                                                  PSPPV
                                                                   110

-------
summarizes the results of the analyses of this section which are used in
plotting the data in figure 10.  A comparison of the actions indicates
that action Al would he most cost-effective in improving the precision of
PMR.  Both actions Al and A3 cost the same to implement, however, the
larger impr -vement in precision resulting from Al shows (for this hypothe-
tical case in figure 10) a lower overall cost since A3 shows a $400 for
reporting poor quality data.
           Table 5.  Comparison of action options based on
                     CV {PMR} for C  adjusted to 12-percent
                     CO,., (incinerator sources)

Action option
AO (a{%C02}=0.4)
Al
A2
A3 (a{%C02>=0.2)
A4

Cost/
20 stacks
$ 0
$ 200
$1000
$ 200
$ 350
Estimated precision
(CV {PMR} in %)
m = 100 mg
11.0
7.6
9.1
9.5
10.3
4.3  PROCEDURES FOR PERFORMING A QUALITY AUDIT
     "Quality audit" as used here implies a comprehensive system of planned
and periodic audits to verify compliance with all aspects of the quality
assurance program.  Results from the quality audit provide an independent
assessment of data quality,  "independent" means that the individuals
performing, and as much as possible of the equipment used in the audit, are
different from the regular field crew and equipment.  From these data both
bias and precision estimates can be made for the measurement process.
     The auditor,  i.e., the individual performing the audit, should have
extensive background experience in source sampling, specifically with the
characterization technique that he is auditing.   He should be able to
                                   111

-------
establish and maintain good rapport with field crews.
     The functions of the auditor are summarized in the following list:
     1.  Observe procedures and techniques of the field team during on-
site measurements.
     2.  Perform certain independent checks,  and from previous training
and experience, estimate the validity of the field crew's measurements.
     3.  Check/verify applicable records of equipment calibration checks
and quality control charts in the field team's home laboratory.
     4.  Perform calculations using data obtained from the audit.
     5.  Compare the audit value with the field team's test value.
     6.  Inform the field team of the comparison results specifying any
area(s) that need special attention or improvement.
     7.  File the records and forward the comparison results with appro-
priate comments to the manager.

4.3.1  Frequency^ of Audit
     The optimum frequency of audit is a function of certain costs and
desired level of confidence in the data quality assessment.  A methodology
for determining the optimum frequency using relevant costs is presented  in
subsection 4.4.4.  For the costs assumed in this document, an optimum audit
level of n = 5 for a lot siz;e of N = 20 results as shown in Figure 15,
page 131.  However, costs will vary among field teams and types of field
tests.  Therefore, the most cost effective auditing level will have to be
derived using local cost data according to the procedure given in subsec-
tion 4.4.4 and in the final report on this contract.

4.3.2  Collecting Audit Information
     While at the sampling site, the auditor should observe the field
team's overall performance of the field test.  Table 6 is a sample check-
list of the operations to observe.  Each item on the list should be checked
yes or no according to whether it was performed as recommended in the
operations manual and, if applicable, the result was within specified
limits.  Those items checked no should be explained under comments.  No
checklist can cover all situations; the auditor must utilize his good
                                  112

-------
Table 6.   Particulate emission determination checklist to be used by auditor
 YES
NO
OPERATION
                         EQUIPMENT PREPARATION AND CHECK
              1.   Sampling train assembled and leak checked.
              2.  , Probe and filter box heaters checked and set for  proper
                  temparatures.
              3.   Stack gas temperature measuring system assembled  and
                  checked for proper operation by comparing to a  mercury
                  in glass thermometer.
              4.   Stack gas velocity measuring system assembled and checked
                  for proper operation.
              5.   Orsat analyzer assembled and checked.
                            PRELIMINARY MEASUREMENTS
              6.   Selection of traverse points according to Method  1.
              7.   Moisture content by Method 4, or equivalent.
              8.   Molecular weight by Method 3, or equivalent.
              9.   Measurement of stack dimensions.
             10.   Mark probe for sampling at traverse points.
                                SAMPLE COLLECTION
             11.   Equal sampling time at each traverse point.
             12.   Probe temperature satisfactory throughout the test.
             13.   Filter box temperature 120 + 14°C (248 i 25°F)through the test.
             14.   Sample gas temperature at last impinger « 20°C  (68°F) through-
                  out the test.
             15.   Isokinetic sampling checked and adjusted if  necessary
                  at least every 5 minutes.
             16.   Leak check of sampl-ing train at end of test.
                                 SAMPLE RECOVERY
             17.   Satisfactory handling and movement of probe  and filter
                  to sample recovery area.
             18.   Recovery area satisfactory (i.e., space, cleanliness,
                  etc.)
                                  113

-------
Table  6.  Particulate emission determination checklist to be used by auditor
                               (continued)
 YES
NO
OPERATION
             19.   Sample recovery procedure adequate.
             20.   Proper labeling of sample containers.
             21.   Determination of moisture content procedure adequate,
                                    ANALYSIS
             22.   Proper equilibration of (1) filter,  (2) probe wash
                  residue, and (3) acetone blank residue.
             23.   Correct collected particulates for acetone blank.
             24.   Analytical  balance checked before weighings.
                                  DOCUMENTATION
             25.   All information recorded on data sheet as obtained.
             26.   All unusual  conditions recorded.
                                    COMMENTS
                                   114

-------
                          AUDIT MEASUREMENTS

          STACK CROSS-SECTIONAL AREA, AS 	
          DRY GAS METER CALIBRATION, y  *	
                                      a	
          ORIFICE METER CALIBRATION, AH@a	
          SAMPLING NOZZLE DIAMETER, D
                                     na-
          SAMPLING NOZZLE CROSS-SECTIONAL AREA,
          PITOT TUBE CALIBRATION COEFFICIENT, C
                                                       m
                                                       Dimensionless
                                                       mm ^0
                                                       mm
                                                             m
                                                           Dimensionless
1.  V   = V  x v  =
     ma    m   ra
2'   Vma(std) = °'3855 Vma
                             CALCULATIONS
                                 3
                                m
                            >    ,   AH
                             bar   13.6
                                                       m ,  at standard
                                                           conditions.
3.   Csa - 0.001  (mn/Vma(s
4.
        = 2.75 x 10
    'sa
                      m /hr, at standard conditions on a dry basis.
5.
    PMRa = Csa
9/hr.
6.
          4'323 Ts Vma(std)
                   Ana Ps e
                                                       percent.
        PMR - PMR
7.   d =
                    x 100 =
          PMR.
    , percent.
           Figure 11.   Sample form for recording audit data
                                  115

-------
judgment and include other checks as deemed desirable for a specific
situation.
     A completed checklist with all yes checks implies that in the opinion
of the auditor the measurement was made in such a manner that large biases
resulting from poor technique are not likely to be present.
     In addition to the above observations, the auditor should independently
determine the stack dimensions.  This should be carried out with the reali-
zation that the measurement is to be used as an estimate of the average
dimension of the stack.  Therefore, for example, a stack which could be out
of round should have its diameter measured from as many sampling ports as
possible and the average diameter used as the stack diameter in subsequent
calculations.  Record the cross-sectional area, A  ,  on the form of figure 11•
                                                 S3.
     The auditor should obtain from the field team a complete set of test
data, i.e., the data form of figure 4 filled in through the section on
recorded test data, for all sample runs.
     In the field team's home laboratory the auditor should verify, by
checking calibration records and field data sheets from previous field
tests, that the performance criteria as given in table 2 of section III
have been satisfied over the period since the last audit.  Also, using
his own calibrated standards, perform the following calibration checks.
     1.  Using his own calibrated wet test meter, or equivalent, calibrate
the dry gas meter and the orifice meter as directed in subsection 2.2.3 of
section II.  Record these audit values as y  and AH@ in the form in
                                           a
figure 11.
     2.  Determine the sampling nozzle diameter, D  , according to the
                                                  na
procedure of subsection 2.2.1.  Calculate the cross-sectional area, A  ,
in square meters by
                       A   = 0.25 x |i x (D   2    1  m
                        na   "' "   7    v na'    ._6   2
                                                  10  mm
                       A   = 7.85 x 10 7 (D  )2 = 	 m2,
                        na                 na     ——•	•——
     Record D   and A   on t'ne audit data sheet of figure 11.
             na      na
                                   116

-------
     3.  Using a calibrated pitot tube, calibrate the field pitot tube
according to the procedure given in subsection 2.1.2, page 11,of the quality
assurance document of this series for Method 2 (ref. 1) or the EPA revised
Method 2 as reproduced in reference 4.  The field pitobe assembly must be
configured as shown in figure 5-1 of Appendix A.  The average coefficient,
C  , applicable to the AP range measured in the field test is determined
 Pa
from this calibration data.  Record C   on the form in figure 11.
                                     ^a
4.3.3  Treatment of Audit Data
     Using the above audit data where applicable and the raw field data,
perform the calculations indicated in figure 11.  All variables are in the
same units as used in subsection 2.5.3 of the operations manual.  In
figure 11 audit measurements and/or parameters computed using audit measure-
ments are subscripted with an a.  Parameters such as (/AP)    , (T )   , M ,
                                                          avg    s avg   s
and B   should be calculated by the auditor from the field crew's original
     ws                       J
data.  All calculations are recorded on the audit data sheet of figure 11.
     A comprehensive discussion of estimating the true particulate mass
emission rate by the average of PMR  and PMR  is contained in reference 23.
                                   C        3.
Also, the importance of sampling isokinetically for particles down to about
5 ym in diameter is illustrated in figure 7.8, page 75, of reference 16.
Unless it is known that the particle size distribution is below 5 ym for
the stack gas being sampled,  the above averaging technique appears  to  be
an improvement over using just the value of PMR  as  the true emission  rate.
     The auditor's report of  a specific field test  to the manager should
include copies of (1)  a completed data sheet from the field team (fig.  4),
(2)  a completed checklist with comments (table 6),  (3)  a completed  audit
data sheet with calculations  (fig.  11)  and  (4)  a summary of the field
team's strong/weak points with an overall numerical  rating and recommended
actions as discussed in the following subsection.
4.3.4  Overall Evaluation of  Field Team Performance
       In a summary-type statement,  the field team should be evaluated on
its  overall performance.   Using the checklist filled out in the field
                                   117

-------
(table 6) in conjunction with the results of the comparison of audit and
field team values of PMR and the circumstances under which the test was
performed, the field team could be rated on a scale of 1 to 5 as follows:
                   5 - Excellent
                   4 - Above average
                   3 - Avera.ge
                   2 - Acceptable, but below average
                   1 - Unacceptable performance.
     Justification for the rating in the form of a list of the team's
strong/weak points with recommendations for improving weak points should
be included in the auditor's report.

4.4  DATA QUALITY ASSESSMENT
     Two aspects of data qua.lity assessment are considered in this section.
The first considers a means of estimating the precision and accuracy of
the reported data, e.g., reporting the bias, if any, and the standard
deviation associated with the measurements.  The second consideration is
that of testing the data qua.lity against given standards using sampling by
variables.  For example, lower and upper limits, L and U, may be selected
to include a large percentage of the measurements and outside of which it
is desired to control the percentage of measurements to, say, less than
10 percent.  If the data quality is not consistent with these limits, L
and U, then action is taken to correct the possible deficiency before
future field tests are performed and to correct the previous data when
possible.
     The determination of the audit level is indicated by using estimated
costs associated with falsely inferring that good (poor) quality data are
of poor (good) quality and with auditing n stacks.  In addition, prior
information concerning data quality is assumed in order to determine an
expected or average cost resulting from the statistical sampling plan.
The cost estimates provided herein are assumed for the purpose of illus-
trating the methodology.  It. is emphasized that managers need to supply
their own costs in making such analyses.
                                   118

-------
 4.4.1   Estimating  the Precision/Accuracy  of  the Reported Data
        Methods  for estimating  the precision  (standard deviation) and
 bias of the  particulate  emission rate  (PMR)  measurements were
 given  in section 4.1.  This  section will  indicate how the audit data
 collected in accordance  with the procedure described in section 4.3 will
 be  utilized  to  estimate  the  precision  and accuracy of the measure of
 interest.  Similar techniques  can also be used by a specific firm or  team
 to  assess their own measurements.  However,  in this case no bias data among
 firms  can be obtained.   The  audit data collected as a result of following
 the procedures  in  the previous section are the measured and audited values
 of  PMR  and  the  difference.
                             PMR. - PMR  .
                        d. = - J - - ^ x  100                       (28)
                          .
                          3
                                PMR
where   PMR. = Field measured value of particulate mass emission rate,
               average of three replicates, and
       PMR  . = Audited value of particulate mass emission rate, average
               of  three replicates.
     Let the mean and standard deviation of the differences d., j  = 1, ...n
field tests be denoted by 3 and s,, respectively.  Thus,
                            d  =      d-/n '
                                 r n        -         11/2
and                        s   =  E  (d-  - d)2/(n - 1)               (30)
                            d    Lj-1   J              -1
4.4.2  Statistical Tests
       The mean d is an estimate of the relative bias in the measurements
                                   119

-------
(i.e., relative to the audited value).   Assuming the audited data to be
unbiased, the existence of a bias in the field data can be checked by the
appropriate t-test, i.e.,
                                                                     (31)
     See reference 29 for a discussion of the t-test.   If t is significantly
large in absolute values, i.e.,  greater than the tabulated value of t with
n - 1 degrees of freedom, which is exceeded by chance only 5 percent of the
time, then the bias is considered to be real and some check should be made
for a possible cause of the bias.  If t is not significantly large, then
the bias should be considered zero or negligible.
     The standard deviation, s,, is a function of both the standard devia-
                              d
tion of the field measurements and of the audit measurements.  Assuming the
audited measurements are obtained with much greater precision than the field
measurements, then the calculated Sj is an estimate of the standard deviation
of the field measurements.  Furthermore, since s, is in percent ? it is an es-
timate of the coefficient of variation, CV{PMR}.  Table 7 in the following
subsection contains an example calculation of d and s , , starting with the
differences for a sample size of n = 5.
     The calculated standard deviation can then be utilized to check the
reasonableness of the assumption made in section 4.1 concerning CV{PMR} =
9.3 percent for m  = 100 mg, for example.  (Remember that CV{PMR} is equal
to s ).  The calculated standard deviation, s , , may be directly checked
against the assumed value, a,, by using the statistical test procedure
                                                                    (32)
       2
where x /f is the value of a random variable having the chi-square distri-
                                               2
bution with f = n - 1 degrees of freedom.  If x /f i-s larger than the
                                      120

-------
tabulated value exceeded only 5 percent of the time, then it would be
concluded that the test procedure is yielding results with more variability
than is acceptable due to some assignable cause of large variation.
     The measured values should be reported along with the estimated bias,
d, standard deviation, s .,, the number of audits, n, and the total number
                        Q
of field tests, N, sample (n <_ N) .  Estimates, i.e., s, and d, which are
significantly different from the assumed population parameters should be
identified on the data sheet.  For example, based on the data of table 7,
if the field team reported a value of PMR =22.9 g/hr for one of the N
field tests not audited, then that measurement would be reported as
     1.  Measured value, PMR =22.9 g/hr
     2.  Calculated bias, t{PMR} = d x PMR = 1.51 g/hr
     3.  Calculated standard deviation, &{PMR} = s  x PMR =1.9 g/hr
     4.  Auditing level, n = 5, N = 20.
     From the above data, users of the data can calculate confidence limits
appropriate to what the data are to be used for.
                     2
     The t-test and x -test described above, and in further detail in the
final report on this contract, are used to check on the biases and standard
deviations separately.  In order to check on the overall data quality as
measured by the percent of measurement deviations outside prescribed limits,
it is necessary to use the approach described in subsection 4.4.3 below.

4.4.3  Sampling by Variables
     Because the lot size (i.e., the number of field tests performed by
a team or laboratory during a particular period, normally a calendar quarter)
is small, N = 20, and consequently, the sample size is small on the order
of n = 3 to 7, it is important to consider a sampling by variables approach
to assess the data quality with respect to prescribed limits.  That is,
it is desired to make as much use of the data as possible.  In the variables
approach, the means and standard deviations of the sample of n audits are
used in making a decision concerning the data quality.
     Some background concerning the assumptions and the methodology is
repeated below for convenience.  However,  one is referred to one of a num-
ber of publications having information on sampling by variables; e.g.,
                                    121

-------
see references 30-33.   The discussion below will be given in regard  to the
specific problem herein which has some unique features as compared with
the usual variable sampling plans.
     In the following discussion,  only the audited value PMR is discussed.
This same procedure can be a.pplied to audits of sampling train components
e.g., the pitot tube calibration,  dry gas meter, and orifice meter.
     The difference between the team-measured and audited value of PMR
is designated as d., and the mean difference over n audits by d, that is,
                                                                      (33)
     Theoretically, PMR. and PMR .  should be measures of the same particulate
mass emission rate, and their difference should have a mean of zero on the
average.  In addition, their differences should have a standard deviation
approximately equal to that associated with measurements of PMR. separately.
     Assuming three standard deviation limits (using the assumed CV = 9.3
percent as derived in the variance analysis of subsection 4.1), the values
-3(9.3%) « -28 percent and 3(9.3%).« 28 percent define lower and upper
limits, L and U, respectively, outside of which it is desired to control
the proportion of differences, d..  Following the method given in reference
30, a procedure for applying the variables sampling plan is described below.
Figures 12 and 13 illustrate examples of satisfactory and unsatisfactory
data quality with respect to the prescribed limits L and U.
     The variables sampling plan requires the sample mean difference, d;
the standard deviation of these differences, s,; and a constant, k, which
is determined by the value of p, the proportion of the differences outside
the limits of L and U.  For example, if it is desired to control at 0.10
the probability of not detecting lots with data quality p equal to 0.10
(or 10% of the individual differences outside L and U) and if the sample
size n = 5, then the value of k can be obtained from Table II of reference
                                   122

-------
/ 1
/ 1
X i
.s \
^"^ \
\

\

\
\^ P2
^--A-
                                                        0.10
Figure 12.  Example illustrating p < 0.10 and satisfactory data quality.
                                                      p (percent  of measured
                                                         differences outside
                                                         limits L and U)  >  0.10
                                                    U
    Figure 13.   Example illustrating p >  0.10 and unsatisfactory  data
                quality.
                                  123

-------
           Table 7.  Computation of mean difference,  d,  and

                 standard deviation of differences,  s,
                                                     d
    General formulas                                 Specific  example
     PMR. - PMR .

d. = 	J	SI x 100
 J
        PMR .                                               .        .
           aj                                          Data (percent)
dl                   dl
                     4
d4                   d4
                      2

 ,                  £d ,                               33.0        49.5
 J                     J


     Ed.
 d = —J-                                              d = 6.6%
      n
      Ed 2 - (Ed )2/n
S2 =  _J_^	_J	                                 2

 d        (n - 1)                                     d
12.0
-6.0
3.0
15.0
9.0
14.4
3.6
0.9
22.5
8.1
s , = Ws ,                                              s ,  = 8.3%
 did                                               d
    Table 8.   Sample plan constants,  k for P{not detecting a lot

               with proportion p outside limits L and U}  <_ 0.1




 Sample size n               k(p = 0.2)                       k(p = 0.1)



       3                       3.039                            4.258

       5                       1.976                            2.742

       7                       1.721                            2.334

      10                       1.595                            2.112

      12                       1.550                            2.045
                                 124

-------
30.  The values of d and s, are computed in the usual manner; see table 8
for formulas and a specific example.  Given the above information, the test
procedure is applied and subsequent action is taken in accordance with the
following criteria:
     1.  If both of the following conditions are satisfied:

                     d - k sd _> L = - ^28 percent,                     (34)

                     d + k sd £ U = 28 percent                         (35)

the individual differences are considered to be consistent with the
deficiencies exist in the measurement process as carried out for that
particular lot (group) of field tests.  These deficiencies should be iden-
tified and corrected before future field tests are performed.  Data cor-
rections should be made when possible, i.e., if a quantitative basis is
determined for correction.
     Table 8 contains a few selected values of n, p, and k for convenient
reference.
     Using the values of d and s, in table 8,  k = 2.742 for a sample size
n = 5, and p = 0.10, the test criteria can be checked; i.e.,

       d - k sd = 6.6 - 2.742 (8.3)  = -16.2 > L = -28 percent       (36)
and
       d + k sd = 6.6 + 2.742(8.3) = 29.4 > U = 28 percent.         (37)

Therefore, the upper limit is not satisfied and the lot of N = 20 measure-
ments is not consistent with the prescribed quality limits.  The plan is
designed to protect against not detecting lots with 10 percent or more
defects (deviations falling outside  the designated limits L and U)  with
a risk of 0.10; that is ,  on the average, 90 percent of the lots with 10
percent or more defects will be detected by this sampling plan.

4.4.4  Cost Versus Audit Level
     The determination of  the audit  level (sample size n) to be used in
assessing the data quality with reference to prescribed limits L and U
                                   125

-------
can be ..made on a statistical basis by defining acceptable risks for type
I and type II errors, knowing or estimating the quality of the incoming
data, and specifying the described level of confidence in the reported
data, or on a cost bassis as described herein.  In this section, cost data
associated with the audit procedure are estimated or assumed for the pur-
pose of illustrating a method of approach and identifying which costs
should be considered.
     A model of the audit process, associated costs, and assumptions made
in the determination of the audit level is provided in figure 14.  It is
assumed that a collection of source emissions tests for N stacks is to be
made by a particular firm, and that n measurements (n <_ N) are to be
audited at a cost, C  = b + en, where b is a constant independent for n,
                    A
and c is the cost perstack measurement audited.  In order to make a specific
determination of n, it is also necessary to make some assumptions about
the quality of the source emissions data from several firms.  For example,
it is assumed in this analysis that 50 percent of the data lots are of
good quality, i.e., one half of the firms are adhering to good data quality
assurance practice, and that 50 percent of the data lots are of poor
quality.  Based on the analysis in section 4.1, good quality data is
defined as that which is consistent with the estimated precision/bias
using the reference method.  Thus, if the data quality limits L and U
are taken to be the lower and upper 3a limits corresponding to limits
used in a control chart, the quality of data provided by a firm adher-
ing to the recommended quality assurance procedures should at most con-
tain about 0.3 percent defective measurements (i.e., outside the limits
defined by L and U) .  Herein., good quality data is defined as that con-
taining at most 10 percent defective measurements.  The definition of
poor quality data is somewhat arbitrary, for this illustration it is
taken as 25 percent outside L and U.
     In this audit procedure the data are declared to be of acceptable
quality if both of the following inequalities are satisfied
                              d + ks, < U                          (39)
                                    d
                                   126

-------
                              d - ks, > L,                         (40)
                                    d
where d and s, are the mean and standard deviation of the data quality
             d
characteristic (i.e., the difference of the field and audited measure-
ments) being checked, and not of desired quality if one or both inequali-
ties is violated, as described in section 4.3.  The cost associated with
these actions are assumed to be as follows:
     C. = Audit cost = b + en.  b is assumed to be zero for this example
      A
          and c is taken as $600/measurement.
   C  i
    P|G = Cost of falsely inferring that the data are of poor quality, P,
          given that the data are of good quality, G.  This cost is
          assumed to be one-half the cost of collecting emissions data for
          N = 20 stacks (i.e., 0.5 x $1000 x 20 = $10,000).  This cost would
          include that of searching for an assignable cause of the inferred
          data deficiency when none exists, partial repetition of data
          collection, decision resulting in the purchase of equipment to
          reduce emission levels of specific pollutants, etc.
   C_ p - Cost of falsely stating that the data are of good quality,  G,
          given that they are of poor quality.  This cost is assumed to be
          $15,000 (= 0.75 x $1,000 x 20).  This cost is associated with
          health effects,  litigation, etc.
   C  i  = Cost savings resulting from correct identification of poor quality
          data.   This cost is taken to be $7,500, i.e., equal to one-half of
          C_,|_ or equal to 0.375 x $1,000 x 20, the total cost of data
          collection.

      These costs are given in figure 14.  These cost data are then used in
conjunction with the a priori information concerning the data quality to
select an audit level n.  Actually, the audit procedure requires the
selection of the limits L and U, n, and k,  L and U are determined on the
basis of the analysis of section 4.1.  The value of k is taken to be the
value associated with n in table 8  of section 4.4.3, i.e., the value
selected on a statistical basis to control the percentage of data outside
                                   127

-------
                       Collection of Source Emission
                         Tests (Lots of Size N)
_ 50% of Lots
< 10% Defective
A
Acceptable
Quality

,
.
Not Acceptable
Quality
•4


50% of Lots
> 10% Defective
Audit n
Measurements

f
W



C = b+cn == $600

•*-
Audit n
Measurements
f

\

I
<—
Select Audit
Parameter n, k
_l t
1
   Data Declared
     to be of
    Acceptable
     Quality
   Data Declared
   not to be of
    Acceptable
     Quality
      Report
       Data
   Data Declared
     to be of
    Acceptable
     Quality
Institute Action to
Improve Data Quality
  (Correct Data if
     Possible)
 Expected Cost of
  Treating Poor
 Quality Data as
Good Quality Data
 C    = $15,000
               Expected Cost  of
               Falsely Inferring
               Data  are of  Poor
                Quality Cp  Q  =

                  $10,000
                                             1
                Expected Cost
              Saving of Taking
             Correct Action with
               Respect to Poor
                Quality Data
                6p|p ^$7,500
    Figure 14.   Flow  chart of the audit level selection process.

                                   128

-------
the limits L and U.  Thus, it is only necessary to vary n and determine
the corresponding expected total cost E(TC) using the following cost model.

       E(TC) - - CA - 0.5 Pp|G  Cp|G + 0.5 Pp|p  Cplp - 0.5 PG|P CG|P  (41)

where the costs are as previously defined.  The probabilities are defined
in a'similar way to the corresponding costs.

      P  I  = Probability that a lot of good quality data is falsely
       P|Gr
             inferred to be of poor quality due to the random variations
             in the sample mean d and standard deviation, s,, in small
             samples of size n.
      P  I  = Probability that a lot of poor quality data is correctly
             identified as being of poor quality.
      P  i_ = Probability that a lot of poor quality data is incorrectly
       Gr|f
             judged to be of good quality due to sampling variations of
             d and s.

     These three probabilities are conditional on the presumed lot quality
and are preceded by a factor of 0.5 in the total cost model to correspond
to the assumed percentage of good (poor) quality data lots.
     In order to complete the determination of n,  it is necessary to
calculate each of the conditional probabilities using the assumptions stated
for a series of values of n (and associated k which is given in table 9).
The computational procedure is given in the Final Report of this contract.
These calculations were made for the cases n = 3,  5, 7, and 10 and for two
degrees of control on the quality of the data that can be tolerated, i.e.,
p = 0.2 and p = 0.1,  the portion outside the  limits L and U for which it
is desired to accept the data as of good quality with probability less than
or equal to 0.10.   These computed probabilities are then used in conjunction
with the costs associated with each condition, applying equation (41) to
obtain the average cost versus sample size n for the two cases p = 0.1 and
0.2.   The curves obtained from these results are given in figure 15.  It can
be seen from these curves that the minimum cost is obtained by using n - 5
                                   129

-------
independent of p.  However, it must be recognized that the costs used in the
example are for illustrative purposes and may vary from one region to
another, thus within the reasonable uncertainty of the estimated costs,
values of n between 3 and 7 would seem to be reasonable.  The assumed costs
suggest that p = 0.2 which tends to permit data of podrer quality to be
accepted, is more cost effective.
                                   130

-------
      $8000
o
H

W
I

•u
en
o
cu
M
cfl
01
      $6000  •
      $4000  -
      $2000  -
                                4567

                                 Audit Level (11)
10
                                                              ""
                p  =  Proportion defective measurements in the  "lot


                P{Acc.  lot with p} <_ 0.1
                   Figure 15.   Average cost vs audit level  (n).



                                   131

-------
LIST OF REFERENCES
        132

-------
                            LIST OF REFERENCES

 1.  EPA-650/14-74-005-a "Guidelines for Development of a Quality Assurance
     Program—Determination of Stack Gas Velocity and Volumetric Flow Rate
     (Type S Pitot Tube)" Environmental Protection Agency, Research Triangle
     Park, North Carolina 27711, 1974.

 2.  EPA-650/14-74-005-b "Guidelines for Development of a Quality Assurance
     Program—Gas Analysis for Carbon Dioxide, Oxygen, Excess Air, and Dry
     Molecular Weight" Environmental Protection Agency, Research Triangle
     Park, North'Carolina 27711, 1974.

 3.  EPA-650/14-74-005-C "Guidelines for Development of a Quality Assurance
     Program—Determination of Moisture in Stack Gases," Environmental Pro-
     tection Agency, Research Triangle Park, North Carolina 27711, 1974.

 4.  F. Smith ,et_ _aJL.  "Guidelines for Development of Quality Assurance
     Programs Applicable to Stationary Source Emission Stream Characteriza-
     tion Techniques," Final Report, EPA Contract No, 68-02-1234, Research
     Triangle Institute, Research Triangle Park, North Carolina 27709, 1976.

 5.  E, S. Kipecki, "Stainless Steels." Machine Design, 1970 Metals Reference
     Issue 4, Vol. 42, Cleveland, Ohio: Penton Pbulishing Company, February
     12, 1970, pp. 34-38.

 6.  R. M. Martin. Construction Details of Isokinetic Source Sampling Equip-
     ment. Publ. No. APTD-0581. Air Pollution Control Office, Environmental
     Protection Agency,  Research Triangle Park, North Carolina 27711, 1971.

 7.  A. W. Gnyp et al.  "An Experimental Investigation of the Effect of
     Pitot Tube-Sampling Probe Configurations on the Magnitude of the S-Type
     Pitot Tube Coefficient for Commercially Available Source Sampling
     Probes," Technology Development and Appraisals Section, Air Resources
     Branch, Ministry of the Environment, Province of Ontario, Toronto,
     Canada; University of Windsor, February, 1975.

 8.  W. S. Smith.  Stack Sampling News 1, No. 7, 1974.

 9.  J. J. Rom. Maintenance, Calibration, and Operation of Isokinetic Source
     Sampling Equipment.  Publ. No. APTD-0576.  Office of Air Programs,
     Environmental Protection Agency, Research Triangle Park, North Carolina,
     1972.

10.  "Occupational Safety and Health Standards:  National Concensus Standards
     and Established Federal Standards."  Federal Register 36, No. 105,
     May 29, 1971.

11.  "Standards of Performance for New Sources."  Federal Register 36,
     No. 247, December 23, 1971.
                                    133

-------
12.  W. S. Smith and D.  J.  Grose.   Stack Sampling Nomographs for Field
     Estimations.  Entropy Environmentalists,  Inc.,  Research Triangle Park,
     North Carolina, 1973.

13.  W. S. Smith. Stack Sampling News 1, No.  1,  1973.

14.  R. F. Yarnor.  Industrial Source Sampling.   Ann Arbor Science Publishers,
     Inc., 1971.

15.  W. J. Mitchell. Evaluation Report:   Additional Studies on Obtaining
     Replicate Particulate Samples from Stationary Sources.  Environmental
     Protection Agency,  Research Triangle Park,  North Carolina 27711, 1973.

16.  EPA-650/4-74-029 "Collaborative Study of  Method for the Determination
     of Particulate Matter Emissions from Stationary Sources (Portland
     Cement Plant)," Environmental Protection  Agency,  Research Triangle
     Park, North Carolina 27711, May 1974.

17.  EPA-650/4-74-021 "Collaborative Study of  Method for the Determination
     of Particulate Matter Emissions from Stationary Sources (Fossil
     Fuel-Fired Steam Generators)," Environmental Protection Agency,
     Research Triangle Park,  North Carolina 27711, June, 1974.

18.  EPA-650/4-74-022 "Collaborative Study of  Method for the Determination
     of Particulate Matter Emissions from Stationary Sources (Municipal
     Incinerators), Environmental Protection Agency, Research Triangle
     Park, North Carolina 27711, July, 1974.

19.  Administrative and Technical Aspects of Source Sampling for Particu-
     lates.  Publ.  No. APTD-1289.   Environmental Protection Agency,
     Research Triangle Park,  North Carolina 27711, May, 1971.

20.  E. L. Grant and R.  S.  Leavenworth.   Statistical Quality Control.
     4th ed., St. Louis:  McGraw-Hill, 1972.

21.  D. A. Simons.   Practical Quality Control.  Reading, Mass.:  Addison-
     Wesley Publishing Company, 1970, pp. 131-150.

22.  EPA-600/9-76-005 "Quality Assurance Handbook for Air Pollution Mea-
     surement Systems," Volume-1 Principles,  Environmental Protection
     Agency, Environmental Monitoring and Support Laboratory, Research
     Triangle Park, North Carolina 27711, March, 1976.

23.  P. K. Mueller ^t al. "Selection of Filter Media:   An Annotated Out-
     line."  Presented at the 13th Conference on Methods in Air Pollu-
     tion and Industrial Hygiene Studies, University of California,
     Berkeley, California,  October 30-31, 1972.

24.  R. M. Burton _e_t a±. "Field Evaluation of the High-Volume Particle
     Fractionating Cascade Impactor—A Technique for Respirable Sampling."
                                   134

-------
     Presented at the 65th Annual Meeting of the Air Pollution Control
     Association, June 18-22,  1972.

25.  W. C. L. Hemeon and A. W. Black.  "Stack Dust Sampling:   In Stack
     Filter or EPA Train."  Journal of the Air Pollution Control Associa-
     tion 22, No. 7, 1972, pp. 516-518.

26.  W. S. Smith. "A Matter of Definition."  Stack Sampling  News 1,  No.  1,
     Technomic Publishing Co., Inc.  Westport, Conn.,  July,  1973.

27.  B. D. Bloomfield. "Source Testing."  Air Pollution, Volume II,  2nd
     edition, A.  C. Stern, ed.  New York:  Academic Press,  1968, Chap-
     ter 28.

28.  W. S. Smith et^ al.  "A Method of Interpreting Stack Sampling Data."
     Stack Sampling News 1, No. 2, 1974, pp. 8-17.

29.  A. Hald. Statistical Theory with Engineering Applications.  New York;
     John Wiley and Sons, 1952.

30.  D. B. Owen.  "Variables Sampling Plans Based on the Normal Distribu-
     tion."  Technometrics 9,  No. 3, August, 1967.

31.  D. B. Owen.  "Summary of Recent Work on Variables Acceptance Sampling
     with Emphasis on Non-normality."  Technometrics 11, 1969, pp.  631-637.

32.  K. Takogi. "On Designing Unknown Sigma Sampling Plans  Based on a
     Wide Class on Non-normal Distributions."  Technometrics 14, 1972.

33.  C. Eisenhart, M. Hastay,  and W. A.  Wallis, eds.  Techniques of Sta-
     tistical Analysis.   Statistical Research Group, Columbia Univ.
     New York:  McGraw-Hill, 1947.
                                   135

-------
APPENDIX A    mm 5-DEIWINATION OF PARTICULATE EMISSIONS
              FROM STATIONARY SOURCES
                                136

-------
           METHOD 5--DETERMINATION OF PARTICULATE
             EMISSIONS FROM STATIONARY SOURCES
1.  Principle and Applicability
     1.1  Principle.  Particulate matter is withdrawn isokinetically
from the source and collected on glass fiber filter maintained at
temperatures equal to or less than 120 ± 14° C (248 ± 25° F) or such
other temperature as specified by an applicable subpart of the
standards.  The particulate mass 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 only when
specified by the test procedures for determining compliance with
new source performance standards.
2.  Apparatus
     2.1  Sampling train.  A schematic of the sampling train used in
this method is shown in Figure 5-1.  Commercial models of this train
are available.  However, if one desires to build his own, complete
construction details are described in APTD-0581; for changes from the
APTD-0581 document and for allowable modifications to Figure 5-1, see
the following subsections.
     The operating and maintenance procedures for the sampling train
are described in APTD-0576.  Since correct usage is important in ob-
taining valid results, all users should read the APTD-0576 document
and adopt the operating and maintenance procedures outlined in it,
unless otherwise specified herein.
                               137

-------
                                                     _c
                                                     'to
                                                      en
                                                      C

                                                     "5.
                                                      £
                                                     22
                                                     _co

                                                      u
                                                      to
                                                     O-
                                                     LO

                                                      OJ



                                                      01
138

-------
     2.1.1  Probe nozzle—Stainless steel  (316)  with sharp,  tapered
                                               o
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.  The wall  thickness  of the  nozzle
shall be less  than or equal to that of a 20 gauge tubing, i.e., 0.165 on
(0.065 in.) and the distance from the tip of the nozzle to  the first
bend or point  of disturbance shall be at least two times the outside
nozzle diameter.  The nozzle shall be constructed from seamless stain-
less steel tubing.  Other configurations and construction material  may
be used with approval from the Administrator.
     A range of sizes suitable for isokinetic sampling should be
available, e.g., 0.32 cm (1/8 in.) up to 1.27 cm (1/2 in.)  (or larger
tf 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  the calibration section.
     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 no greater than 120 ± 14° C (248  + 25° F) or no
greater than such other temperature as specified by  an applicable
subpart of the standards.  Since the actual temperature at  the outlet
of the probe is not 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 as  acceptable.
                                 139

-------
     Porosilicate or auartz glass probe liners shall  be  used for
temperatures up to about 480° C (900° F) and auartz liners  for
tenperatures up to about 900° r (1650° F).   Both nay  be  used at
higher temperatures for short periods of time, but nust  be  approved
by the Administrator.  The softening temperature for  borosilicate
is 820° C (1508° F) and for ouartz it is 1500° C (2732°  F).
     When length limitations, i.e. oreater  than about 2.5 m (8.2 ft),
are encountered at temperatures less than 320° C (608° F),  stainless
steel (316) or Incoloy 825  (both of seamless tubing), or other
materials as approved by the Administrator, may be used. Metal
probes for sampling pas streams at temperatures in excess of 320°  C
(608° F) must be approved by the Administrator.
     2.1.3  Pitot tube—Type S, or other device approved by the
Administrator, attached to probe to allow constant monitoring of the
stack gas velocity.  The face openings of the pitot tube and the probe
nozzle shall be adjacent and parallel to each other,  not necessarily
on the same nlane, during sampling.  The free space between the nozzle
and pitot tube shall be at least 1.9 cm (0.75 in.).  The free space
shall be set based on a 1.3 cm (0.5 in.) ID nozzle.  If  the sampling
train is designed for sampling at higher flow rates than that described
in PPTD-CSSl, thus necessitating the use of larger sized nozzles,  the
largest sized nozzle shall be used to set the free space.
     The nitot tube must also reet the criteria specified in Method 2
and calibrated according to the procedure in the calibration section
of that method.
 Mention of trade names or specific products does not constitute
 endorsement by the Environmental Protection Agency.
                               140

-------
     2.1.4  Differential pressure gauge—Inclined manometer capable
of measuring velocity head to within 10% of the minimum measured value.
Below a differential pressure of 1.3 mm (0.05 in.) water gauge,
micromanometers with sensitivities of 0.013 mm (0.0005 in.) should
be used.  However, micromanometers are not easily adaptable to field
conditions and are not easy to use with pulsating flow.  Thus, methods
or other devices acceptable to the Administrator may be used when con-
ditions warrant.
     2.1.5  Filter holder--Borosilicate glass with a glass frit
filter support and a silicone rubber gasket.  Other materials of
construction may be used with approval from the Administrator,
e.g. if probe liner is stainless steel, then filter holder may be
stainless steel.  The holder design shall  provide a positive seal
against leakage from the outside or around the filter.
     2.1.6  Filter heating system—Any heating system capable of
maintaining a temperature around the filter holder during sampling
of no greater than 120 ± 14° C (248 + 25° F), or such other temperature
as specified by an applicable subpart of the standards.  A temperature
gauge capable of measuring temperature to within 3° C (5.4° F) shall
be installed such that temperature around the filter holder can  be
regulated and monitored during sampling.  Heating systems other  than
shown in APTD-0581 may be used.
     2.1.7  Condenser—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.  Acceptable means are to
                              141

-------
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
Dalton's law or (2) by passing the sample gas stream through a tared
silica gel trap with exit gases kept below 20  C (68  F) and determining
the weight gain.
     Note:  If "condensible particulate matter" is desired, in addition
to moisture content, the following system shall be used—four impingers
connected in series with ground glass, leak free fittings or any
similarly leak free noncontaminating 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.
Individual States or control agencies requiring this information shall
be contacted as to the sample recovery and analysis of the impinger
contents.
     For purposes of writing the procedure of this method, the system
described in the note above will be used for determining the moisture
content of the stack gas.  Modifications (e.g. using flexible con-
nections between the impingers or using materials other than glass)
may be used with approval from the Administrator.
     If means other than silica gel are used to determine the amount of
moisture  leaving the condenser, it is recommended that silica gel still
be used between the condenser system and pump to prevent moisture  con-
densation in the pump and metering devices.
                                142

-------
     Unless otherwise specified by the Administrator, flexible
vacuum lines may be used to connect the filter holder to the con-
denser.
     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
with 2% accuracy, and related equipment, or equivalent,  as  required to
maintain an isokinetic sampling rate and to determine sample volume.
Sampling trains utilizing metering systems designed for  higher flow
rates than that described in APTD-0581 or APTD-0576 may  be  used pro-
vided that the specifications in section 2 of this method are met.  When
the metering system is used in conjunction with a pi tot  tube, the system
shall enable checks of isokinetic rates.
     2.1.9  Barometer—Mercury, aneroid, or other barometers 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
weather bureau station, in which case the station value  shall be
requested and an adjustment for elevation differences shall  be applied
at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m (100  ft)  elevation
increase.
     2.1.10  Gas density determination equipment—Temperature and
pressure gauges and gas analyzer as described in Methods 2  and 3.
     2.1.11  Temperature and pressure gauges—If Dalton's law is
used, to monitor temperature and pressure at condenser outlet.  The
temperature gauge shall have an accuracy of 1° C (2° F). The pressure
gauge shall be capable of measuring pressure to within 2.5  mm Hg
                                143

-------
(0.1 in. Hg).  If silica gel  is  used  in  the  condenser system the
temperature and pressure nust be reasured  before the silica gel
component.
     2.2  Sample recovery,,
     2.2.1  Probe liner and nrobe nozzle brushes—Nylon bristles
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 raterial.   Poth brushes shall be properly
sized and shaped to brush out the nrcbe  liner and nozzle.
     2.2.2  Glass wash bottles—Two.
     2.2.3  Glass sample storage containers—Chemically resistant,
borosilicate narrow mouth glass  bottles, for acetone washes, 500 ml or
1,000 ml.  Screw cap closures shall be teflon rubber-backed liners or of
such construction so as to be leak free  and  prevent chemical attack
from the acetone.  Other types of containers must be approved by the
Administrator.
     2.2.4  Petri dishes--For filter  samples, alass or plastic, 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 are
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.
                                144

-------
     2.3  Analysis.
     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 a.
     2.3.5  Reakers~250 ml.
     2.3.6  Hygrometer—To measure  the relative humidity  of the
laboratory environment.
     2.3.7  Temperature gauge—To measure the temperature of the
laboratory environment.
3.  Reagents
     3.1  Sampling.
     3.1.1  Filters--Glass fiber filters, without  organic binder
exhibiting at least 99.95% efficiency (5 0.05% penetration)  on
0.3 micron dioctyl phthalate smoke  particles.   The filter efficiency
test shall be conducted in accordance with /'STM standard  method
D 2986-71.  Test data from the supplier's duality  control program
is sufficient for this purpose.
     3.1.2  Silica gel —Indicating  type, 6-16 mesh.   If previously
used, dry at 175° C (350° F)  for 2  hours.  New silica pel may be
used as received.
     3.1.3  Water—Men 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.
                              145

-------
     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.
     3.2  Sample recovery.
     3.2.1  Acetone—Reagent grade, < 0.001% residue, in glass  bottles.
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%)
shall be used.
     3.3  Analysis.
     3.3.1  Acetone—Same as 3.2.1.
     3.3.2  Desiccant—Anhydrous calcium sulfate, indicating type.
4.  Procedure
     4.1  Sampling.  The sampling shall be conducted by competent
personnel experienced with this test procedure.
     4.1.1  Pretest preparation.  All the components shall be main-
tained and calibrated according to the procedure described in APTD-0576,
unless otherwise specified herein.
     Weigh approximately 200-300 g of silica gel in air tight containers
to the nearest 0.5 g.  Record the total weight,  both silica gel and
container, on the container.  More silica gel may be used but care
should be taken during sampling that it is not entrained and carried
out from the impinger.  As an alternative, the silica gel may be
weighed directly in the impinger or its sampling holder just prior
to the train assembly.
                                146

-------
     Check filters visually against light for irregularities and
flaws or pinhole leaks.  Label a filter of proper diameter on the
back side near the edge using numbering machine ink.  As an alterna-
tive, label the shipping container (glass or plastic petri dishes)
and keep the filter in this container 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 6 or more hour intervals
to a constant weight, i.e., < 0.5 mg change from previous weighing,
and 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%.
     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 and
moisture content using Approximation Method 4 or its alternatives
for the purpose of making isokinetic sampling rate calculations.
Estimates may be used.  However, final results will be based on actual"
measurements made during the test.
     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 differential pressure gauge is capable of
measuring the minimum velocity head value to within 10%, or as
specified by the Administrator.
                              147

-------
     Select a suitable probe liner and probe length such that all
traverse points can be sampled.  Consider sampling from opposite
sides for large stacks 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 the sampling time per point is not
less than 2 min. or some greater time interval as specified by the
Administrator and the sample volume that will be taken will exceed
the required minimum total gas sample volume specified in the test
procedures for the specific industry.  The latter is based on an
approximate average sampling rate.  Note also that the minimum total
sample volume is corrected to standard conditions.
     It is recommended that 1/2 or an integral number of minutes be
sampled at each point in order to avoid timekeeping errors.
     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
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 place approximately 200-300 g or more,
if necessary, of preweighed silica gel in the fourth impinger.  Record
                               148

-------
the weight of the silica pel and container to the nearest 0.5 p.
Place the container in a clean place for later use in the sample
recovery.
     Using a tweezer or clean disposable surgical ploves, place the
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 not allow the sample pas stream to circumvent the filter.
Check filter for tears after assembly is completed.
     When class liners are used, install selected nozzle using a
Viton A 0-ring when stack temperatures are less than 260° C (500° F)
or an asbestos string nasket when temperatures are higher.   The Viton
A 0-ring and asbestos string gasket are installed as a seal where
the nozzle is connected to a glass liner.  See APTD-0576 for details.
When metal liners are used, install the nozzle as above or by a leak
free direct mechanical connection.  Mark nrobe with heat resistant
tape or by sone other method to denote the proper distance into the
stack or duct for each sampling point.
     Unless otherwise specified by the Administrator, attach a
temperature probe to the metal sheath of the sampling nrobe so that
the sensor extends beyond the nrobe tin and does not touch any metal.
Its position should be about 1.9 to 2.54 cm (0.75 to 1 in.) from
the pi tot tube and probe nozzle to avoid interference with the gas  flow.
     Set up the train as in Figure 5-1, using, if necessary, a very
light coat of silicone nrease on all ground glass joints, greasing
only the outer oortion (see APTD-0576) to avoid possibility of
                               149

-------
contamination by the silicone grease.   V.'ith  approval  from  the
Administrator, a nlass cyclone ray be  used between  the probe and
filter holder.
     Place crushed ice around the impingers.
     4.1.4  leak check procedure—After the  sampling  train has  been
assembled, turn on and set the filter  and nrobe heating system  to  the
pov/er required to reach a temperature  of 120 + 14°  C  (248  + 25° F)
or such other temperature as specified by an applicable subpart of
the standards for the leak check.  (If water condensation  is not a
problem the probe and/or filter heating system need not be used.)
Allow time for the temperature to stabilize.   If a  Viton A 0-ring
or other leak free connection is used  in assembling the probe nozzle
to the rrobe liner, leak check the train at  the sampling site by plug-
ging 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 as  above by
first plugging the inlet to the filter holder.  Then  connect the probe  to
the train and leak check at about 25 rm Hg (1 in. Ho) vacuum.   A leakage
rate in excess of 4?^ of the average samnlino rate or  0.00057 m  /min.
(0.02 cfn), whichever is less, is unacceptable in either case.
     The following leak check instructions for the  sampling train
described in APTD-C576 and APTD-0581 nay be  helpful.   Start the pump
with by-pass valve fully open and coarse adjust valve completely
closed.  Partially open the coarse adjust valve and slowly close
the by-pass valve until 380 mm Mo (15 in. Hg) vacuum  is reached.
Po not reverse direction of by-pass valve.  This will cause water  to
back up into the filter holder.  If 380 rm Hg (15 in. Hg)  is exceeded,
                               150

-------
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 or filter holder 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.
     Leak checks shall be conducted as described whenever the train
is disengaged, e.g. for silica gel or filter changes during the
test, prior to each test run, and at the completion of each test  run.
If leaks are found to be in excess of the acceptable rate, the test
will be considered invalid.  To reduce lost time due to leakage
occurrences, it is recommended that leak checks be conducted
between port changes.
     4.1.5  Particulate train operation—During the sampling  run,
isokinetic sampling rate to within 10%, or as specified by the
Administrator, of true isokinetic and the temperature around  the
filter of no greater than 120 ± 14° c (248 ± 25° F), or as specified
by an applicable subpart of the standards, shall be maintained.
     For each run, record the data required on the example data
sheet 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, and when sampling is halted.  Take other data point readings
at least once at each sample point during each time increment and
                              151

-------
          _
     00   OC
     LU   =}
     OC   t-
     Q.   CO   X
E   —
I   s
=   °   =
«   cc   £
S   <   co
<   CD   <
                         E
                         u

                        oc"
                        LU

                        LU
                        S

                        5
                        N
                        IM
                        a
<  I—

£  S
-  OC
                   (si
                        a
                        <
                        EC
               o
               OC
                                 <   _i
                                 5-i
                                 <
             o
             a:
             a.
                o
                LU
                CO

                CO
                O
                cc
                O

                U
                                         o
                                         o
                                         I
                                         u
                                         in




z
o




ac
0





i.. ^
t- <








c



o




^ z
o x ®
00 <=> 5
CO ~2;5:>— t— 2
cc


























































































































































































































































































































































































o>

>




















_J
0







01


















LU
CC

                                                                                                                                         CO

                                                                                                                                         CO
                                                                                                                                         T3
                                                                                                                                                        0)
                                                                                                                                                        (U
                                                                                                                                                        *•—
                                                                                                                                                        ffl
                                                                                                                                                         o
                                                                                                                                                        ca
                                                                                                                                                        Q.
                                                                                                                                                        LO

                                                                                                                                                         a>

                                                                                                                                                         o>
                                                                                                                                                        LL
                                                                       152

-------
additional readings when significant changes (20% variation in
velocity head readings) necessitate additional  adjustments in flow
rate.  Level and zero the manometer.
     Clean the portholes prior to the test run  to minimize chance
of sampling the deposited material.  To begin sampling, remove the
nozzle cap, verify that the filter and probe are up to temperature,
and that the pitot 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 for sampling
trains using type S pitot tubes with 0.85 + °-02 coefficient and
when sampling in air or a stack gas with equivalent density (molecular
weight equal to 29+4), which aid in the rapid adjustment of the
isokinetic sampling rate without excessive computations.  APTD-0576
details the procedure for using these nomographs.  If C  and M . are
outside the above stated ranges, do not use the nomograph unless
appropriate steps are taken to compensate for the deviations.
     When the stack is under significant negative stack pressure
(height of impinger stem), take care to close the coarse adjust valve
before inserting the probe into the stack to avoid water 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.
                            153

-------
     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 to
minimize chance of extracting deposited material.
     Turing the test run, rake periodic adjustments to keep the
temperature around the filter holder at the proper temperature  and
add more ice and, if necessary, salt to maintain a temperature  of
less than 20° C (68° F) at the condenser/silica ael outlet to avoid
excessive moisture losses.  /Hso, periodically check the level  and
zero of the nanometer.
     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 he used rather than attempting to change the filter
itself.  /*fter the new filter or filter assembly is installed
conduct a leak check.  The parti oil ate veirht shall include the
summation of all filter assembly catches.
     P single train shall be used for the entire sample run, except
for filter and silica rel changes.  However, if approved by the
Administrator, two or pore trains may be used for a single test run
when there are two or more ducts or sampling ports.  The results shall
be the total of all sampling train catches.
     At the end of the sample run, turn off the oump, remove the
probe and nozzle from the stack, and record the final dry gas meter
reading.  Perform a leak check at a vacuum egual  to or greater  than
the maximum reached during sampling.  Calculate percent isokinetic (see
calculation section) to determine whether another test run should be
                               154

-------
made.  If there is difficulty in maintaininq isokinetic rates due
to source conditions, cons'dt with the Administrator for possible
variance on the isokinetic rates.
     4.2  Sample recoverv.  Proper cleanuo nrocedure heoins as
soon as the nrobe is removed from the stack at the end of the samolina
peri od,
     When the probe can he safely handled, wipe off all external
particulate matter near the tio of the nrohe nozzle and place a cap
over it to prevent losina or aainina oarticulate matter.  Do not cap
off the orobe tip tightly while the samplinq train is coolinq down as
this would create a vacuum in the filter holder, thus drawinq water
from the impingers into the filter.
     Before movinq the sample train to the cleanun site, remove the
probe •from the samnle train, wipe off the silicone grease, and can
the ooen outlet of the probe.  Be careful not to lose any condensate,
if present.  Wipe off the silicone grease from the filter inlet where
the probe was fastened and can it.  Remove the umbilica"1 cord from the
last impinaer and cap the impinoer.  If a flexible line is used between
the first imninaer or condenser and the -filter holder, disconnect the
line at the filter holder and let any condensed water or liquid drain
into the impinqers or condenser.  After wipino off the silicone nrease,
cap off the filter holder outlet and imninqer inlet.  Either qround
glass stoppers or plastic caps or serum cans may be used to close
these openings.
     Transfer the probe and filter-impinqer assembly to the cleanup
area.  This area should be clean and nrotected from the wind so that
                               155

-------
the chances of contaminating or losing the sample will  be minimized.
     Save a portion of the acetone used for cleanup as  a blank.
Place about 200 ml of this acetone 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 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
particulate cake is inside the fold.  Quantitatively remove any
particulate matter and/or filter which adheres to the filter holder
by carefully using a dry nylon bristle brush and/or a sharp-edged
blade and place into this container.  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 into a glass container in the following manner.
     Distilled water may be used when approved by the Administrator
or shall be used when specified by the Administrator.   In these cases,
save a water blank and follow Administrator's directions on analysis.
     Carefully remove the probe nozzle and clean the inside surface
by rinsing with acetone from a wash bottle and brushing with a nylon
                               156

-------
bristle brush.  Brush until acetone rinse shows no visible particles,
after which make a final rinse of the inside surface with acetone.
     Brush and rinse with acetone the inside parts of the Swagelok
fitting in a similar way until no visible particles remain.
     Rinse the probe liner with acetone by tilting the probe and
squirting acetone into its upper end, while rotating the nrobe so
that all inside surfaces will be rinsed with acetone.  Let the
acetone drain from the lower end into the sample container.  A funnel
may be used to aid in transferring liquid washes to the container.
Follow the acetone rinse with a nrobe brush.  Hold the probe in an
inclined position, sauirt acetone into the upner 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 particulate matter which is brushed from the nrobe.  Run the brush
through the nrobe three tines or more until no visible particulate
matter is carried out with the acetone or 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.
     It is recommended that two people be used to clean the probe to
minimize losing the sample.  Between sampling runs, keep brushes clean
and protected from contamination.
                               157

-------
     After ensurinq that all  joints are 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 rinsinn 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.  After all acetone washinqs and oarticulate  matter are
collected in the sample container, tiqhten the lid on the samnle
container so that acetone will not leak out when it is shipped to
the laboratory.  Mark the heiqht of the fluid level  to determine
whether or not leakaqe occurred durinq transport.  Label container
to clearly identify its contents.
     Container No. 3.  Note color of indicatinq silica qel to deter-
mine if it has been completely spent and make a notation of its
condition.  Transfer the silica qel from the fourth imninaer to  the
original container and seal.   A funnel may make it easier to pour the
silica qel without soillinq.   A rubber policeman may be used as  an aid
in removinq the silica eel from the imoinqer.  It is not necessary to
remove the small amount of dust particles that may adhere to the v/alls
and are difficult to remove.   Since the nain in weinht is to he  used
for moisture calculations, do not use any water or other liquids to
transfer the silica qel.  If a balance is available in the field, *ollow
the procedure under analysis.
     Impinqer water.  Treat the imoinaers or condenser as follows:
Make a notation of any color or film in the liquid catch.  Measure
the liquid which  is in the first  three imninqers to within ± 1 ml by
                                158

-------
using a oraduated cylinder or, if available, to within ± 0.5 q
by using a balance.  Record the volume or weight of liquid present.
This information is required to calculate the moisture content  of
the effluent aas.
     If analysis of the impinaer catch is not required, discard the
liquid after measuring and recording the volume or weiqht.   If
analysis of the impinaer catch is reauired, leave the imoinaers
intact to transfer the liquid, cap off the inlet, and pour the  liquid
throuqh the outlet into the graduated cylinder or into a sample con-
tainer after its weiqht has been determined.
     If a different tyne of condenser is used, measure the amount
of moisture condensed either volumetrically or aravimetrically.
     4.3  Analysis.  Record the data required on the example sheet
shown in Fiaure 5-3.  Handle each sample container as follows:
     Container No. 1.  Leave in shipping container or transfer  the
filter and any loose particulate from the sample container to a
tared glass weighing dish and desiccate for 24 hours in a desiccator
containing anhydrous calcium sulfate.  Weigh to a constant weinht
and report the results to the nearest 0.1 mg.  For purposes of  this
section 4.3, the term "constant weiqht" means a difference of no
more than 0.5 mq or T£ of total weioht, less tare weiaht, whichever
is qreater, between two consecutive weiahinqs, with no less than 6
hours of desiccation time between weiqhinas and no more than 2  minutes
exposure to the laboratory atmosphere (must be less than 50% relative
humidity) durina weighing.
                               159

-------
Plant.
Date	
Run No	
Relative Humidity.
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 PARTICULATE COLLECTED,
mg
FINAL WEIGHT


:xr
TARE WEIGHT

:xr
Less acetone blank
Weight of participate matter
WEIGHT GAIN






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




SILICA GEL
WEIGHT,
g



9* ml
       CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
       INCREASE BY DENSITY OF WATER (1g/ml).
                                                : VOLUME WATER, ml
                                      1 g/ml
                          Figure 5-3. Analytical data.
                                 160

-------
     Container No. 2.  Note level of liquid in container and
confirm on analysis sheet whether or not leakage occurred during
transport.  Measure the liquid in this container either volume-
trically 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 nig.
     Container No. 3.  Weigh the spent silica gel to the nearest
0.5 g using a balance.  This step may be conducted 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.
5.  Calibration
     Maintain a laboratory log of all calibrations.
     5.1  Probe nozzle.  Using a micrometer, measure the inside
diameter of the nozzle to the nearest 0.025 mm (0.001 in.).  Make
3 separate measurements usina 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 permanently and uniquely identified.
     5.2  Pi tot tube.  The pi tot tube shall be calibrated according
to the procedure outlined in Method 2.
                               161

-------
     5.3  Dry gas meter and orifice meter.  Both meters shall be
calibrated according to the procedure outlined in APTD-0576.  When
diaphragm pumps with by-pass valves are used, check for proper
metering system design by calibrating the dry aas meter at an
                                •?
additional flow rate of 0.0057 m /min. (0.2 cfm) with the by-pass
valve fully opened and then with it fully closed.  If there is more
than ± 2% difference in flow rates when compared to the fully closed
position of the by-pass valve, the system is not designed properly
and must be corrected.
     5.4  Probe heater calibration.  The probe heating system shall
be calibrated according to the procedure contained 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 pauaes.  Calibrate dial and liquid filled bulb
thermometers against mercury-in-glass thermometers.  New thermocouples
need not be calibrated.  Calibrate used thermocouples aaainst new ones.
For other devices, check with the Administrator.
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
                                            2    2
     A   = Cross sectional area of nozzle, m  (ft  )
     B   = Water vapor in the gas stream, proportion by volume
      ws
     C   = Acetone blank  residue concentration, mg/mg
      a
     c   = Concentration  of  particulate matter  in  stack aas, dry basis,
           corrected  to standard conditions, g/dscm  (g/dscf)
                                162

-------
I        » Percent of isokinetic sampling



m        = Total amount of particulate matter collected, mg.



M        = Molecular weight of water, 18 g/g-mole (18 Ib/lb-mole)
 w


m        = Mass of residue of acetone after evaporation, mg
 a


?^       = 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)



R        = Ideal gas constant, 0.06236 mm Hg-m /°K-g-mole (21.83 in.



           Hg-ft3/°R-1b-mole)



T        = Absolute average dry gas  meter temperature (see Figure  5-2),



           °K (°R)



TS       = Absolute average stack gas temperature (see Figure 5-2),



           °K <°R).



Tstd     = standard absolute temperature, 293° K (528° R)



V.       = Volume of acetone blank,  ml
 a


V,,       = Volume of acetone used in wash, ml
 «W


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 / td\  = Volume of gas sample measured by the dry gas meter



           corrected to standard conditions, dscm (dscf).



V / .  .\  * Volume of water vapor in  the gas sample  corrected to



           standard conditions, son  (scf).
                              163

-------
     Wa
     AH
      w
          = Stack gas velocity, calculated by Method 2,  Equation 2-7
            using data obtained from Method 5, m/sec (ft/sec)
          = Weight of residue in acetone wash, mg
          = Average pressure differential across the orifice (see
            Figure 5-2), meter, mm H,,0 (in. H20)
           = Density of acetone, mg/ml (see label on bottle)
           = Density of water, 1 g/ml (0.00220 Ib/ml)
     e     = Total sampling time, min.
     13.6 = Specific gravity of mercury
     60   = sec/mi n
     TOO  = 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 standarc conditions (20  C, 760 mm Hg or 68  F,
29.92 in. Hg) by using Equation 5-1.
     Vm(std)  =  Vm
                                      AH
                                  std
                                           = K V.
                                                m
                                                         + AH/13.6
                                                Equation 5-1
     where:
          K
               0.3855 °K/mm Hg for metric units
               17.65 °R/1n. Hg for English units
                                 164

-------
     6.4  Volume of water vapor.
     'w(std)
                         K Vlc    Equation 5-2
     where
                       3
          K = 0.00134 m /ml for metric units
            = 0.0472 ft /ml for English units
     6.5  Moisture content.
     6.
                   Vstd)
      ws
m(std)
                           w(std)
     6.6  Acetone blank concentration.
                                 Equation 5-3
                                                Equation 5-4
     6.7  Acetone wash blank.
     W   •  C   V    p
      a      a   aw   a
                                 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).
     6.9  Particulate concentration.
     cs  -  (0.001 g/mg)
                                 Equation 5-6
                              165

-------
6.10  Conversion factors:
From            jp_            Multiply by
                                0.0283
                               15.4
                                2.205 x 10"3
                               35.34
6.11  Isokinetic variation.
6.11.1  Calculations from raw data.
scf
•3
g/ft3
g/ft3
g/ft3
oj
m
3
gr/ft
lb/ft3
g/m3
                                  ("
                                    bar
                  60 0 v  P  A
                                           Equation 5-7
where:
     K = 0.00346 mm Hg-m3/ml-°K for metric units
       = 0.00267 in. Hg-ft3/ml-°R for English units
6.11.2  Calculations from intermediate values.
                                100
 I  =
              s  ym(std)   std
        _
       Tstd vs eAnPs  60
                                            Equat1on 5"
where:
     K = 4.323 for metric units
       = 0.0944  for Enolish units
                         166

-------
     6.12  Acceptable results.   If 90% < I < 110%,  the results  are
acceptable.  If the results are low in comparison to the standards
and I is beyond the acceptable  range, the Administrator may option
to accept the results.  Use reference 7.4 to make judgments.  Other-
wise, reject the results and repeat the test.
7.  References
     7.1  Addendum to Specifications for Incinerator Testing  at
Federal Facilities, PHS, NCAPC, Dec. 6, 1967.
     7.2  Martin, Robert M., Construction Details of Isokinetic Source
Sampling Equipment, Environmental  Protection Agency, APTD-0581.
     7.3  Rom, Jerome J., Maintenance, Calibration, and Operation
of Isokinetic Source Sampling Equipment, Environmental Protection
Agency, APTD-0576.
     7.4  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.
     7.5  Smith, W. S., et al., Stack Gas Sampling  Improved and
Simplified with New Equipment,  APCA paper No. 67-119,  1967.
     7.6  Specifications for Incinerator Testing at Federal Facilities,
PHS, NCAPC, 1967.
                                167

-------
APPENDIX B     ILLUSTRATED USE OF NOMOGRAPHS
                    168

-------
APPENDIX B    ILLUSTRATE) USE OF NOMOGRAPHS
     The material in this appendix is, in the most part, reproduced  from
APTD-0576 (ref.  9).
NOMOGRAPHS
     The correction factor nomograph  (fig. Al) and the operating nomograph
(fig. A2) have been designed for use with the sampling train as aids for
rapid isokinetic sampling rate adjustments and for selection of proper
nozzle size.  To determine the correction factor, C, on the nomograph,  the
following information is first required:
     (1)  Percent moisture, %H20.  This may be determined  from a previous
test or presurvey, or before the sample run.
     (2)  Orifice calibration factor, AH@.  This is determined from  the
laboratory calibration (see section on Calibration).
     (3)  Meter temperature, T .  Temperature at the meter rises above
                              m
ambient temperature because of the pump and can easily be  estimated  with
experience.   An estimate within 10° F  (approximately + 1 percent error)  is
all that is necessary (an initial estimate of about 25°F above ambient
temperature has  been used).  This approximation above ambient temperature
is not required if the pump is located outside the meter box console.
                                  RET 2
                   ~^~
                                         -z a
                                         -l 5
1   __-
                                       .=-^0	1T£_!1_ " ~
                                         -0 6
                                         -0 5
                                     EXAMPLE AH^; i 8
                                            Tm = 100 °F
                                          % H2O : 10
                                          Ps/Pm -- 1 05
                                         FIND C : 1 0
rS/rM
- I 2
           Figure Al.  Nomograph for  correction factor,  C.
                                   169

-------
      (4)  Stack pressure,  P .   This is measured before the sample run; or
                            s
if the sampling site is near the exit of the stack, atmospheric pressure
is used.
     (5)   Meter pressure, P .  Same as atmospheric pressure.
     To obtain correction factor, C (fig. Al):
     (1)   Draw line from AR@ to T  to obtain point "A" on reference line 1
(ref. 1).
     (2)   Draw line from point "A" to %H~0 to obtain point "B" on reference
line 2 (ref. 2).
     (3)   Draw line from point "B" to the calculated value P /P  to obtain
                                                            S  TD.
correction factor, C.
     To select the nozzle size and to set the K-factor on the operating
nomograph, the following information is first required:
     (1)   C factor.  This is obtained from the correction-factor nomograph
(fig. Al).
          Note:  If the coefficient, C , of the type-S pitot tube is not
                                      P
                 equal to .85 +  -02, the following is required:  (a)  Mul-
                               /C  \
                 tiply C times I  gTJ = C1 for the correct C factor in
                 obtaining the K-factor, or (b) if C' is less than 0.5, then
                                                       /C  \2
                 use C and multiply each AP reading by (  1,. ) for each adjust-
                 ment.
     (2)  Stack temperature, T .   This is determined in °F by a rough
                              S
temperature traverse to within + 25°F before the sample run.
     (3)  Average velocity pressure, AP.  This is determined by a rough
preliminary pitot traverse, using the average of minimum and maximum AP's
in inches of water.
     (4)  Exact available nozzle sizes, D.  This is obtained from the cali-
bration of available nozzles.
     To select the nozzle size and to set the K-factor pivot point, use the
following procedure (fig. A2):
     (1)  Set correction fs.ctor,  C, on sliding scale to the reference mark,
"A."
     (2)  Align T  with average AP, note probe tip diameter on D-scale, and
select exact nozzle size closest to it.
                                 170

-------
CORRECTION
FACTOR,
C
ORIFICE READING,
A H
10
9—
8 —
7^—


6-=
=
•3
5^s
^
4-i
=

—
3~
~
3
2_5
—
—



	
—
, ~
0 9 	
0 & 	
0 7 	

0 6-H
0 5-|

0 4-^

0 3-=


0 2 	





0 1 	



REF A 	















S,REF B
^ f

























— 2 0

— 1 5

~ STEP 1
— ! 0

— 09

	 08

— 07

	 0 6
— 05











•-•^



-




—2500
-
—3000
-
— 1 500
I
—
— 1000


— 800
— 600.
Z- 500
	 400
•^••4?." 	
	 ^00

	 100
	 0
STACK
TEMPERATURE,
T
S



SLIDING
SCALE
CUT ALONG LINES




PITOT READING,
K FACTOR o 001 	



























^-£rf/3
'""•^.^
__S_TEF_2
	 " 	













6.H: m. HjO
C ; dimension les
Ts =«>,.

"=
0 002^
•j
0 003-;
—
0 004^

_j

PROBE 0 °°5-
TIP DIAMETER, ~
0 006—
U —
001—^

















-^.-Jfc

	















5-0 9 -;

^-08 002-

^-07 0 03 —
- 0 04-
:" 005 —
r 006-

E-o 5 —
- 0 08 	

i-0 4
" 0 2 	
~ 03-
~ ~
~ 04-

? 	 .^ ' ^6.
- 	 °'^
— 02 0 « —
1 0 —
-
_
2 0 —
3 0-
_ 40-
5 0.
6 0 —
8 ''_
1 0 0 —















































EXAMPLE C : 1 0
K - dimension less Tg = 300 *F
D : in AP i 0 5 m HjO
AP : in. H2O D ; 0 250 in., 0 375 in
Figure A2.   Use of the nomograph in selecting nozzle size
            and setting K factor.
                          171

-------
     (3)  Align T  with exact nozzle size selected and obtain a value on
                 &
the AP scale.
     (4)  Align the AP value with reference mark, "B", on AH scale, and set
the K-factor pivot point.
     To obtain the orifice meter settings, AH, for isokinetic conditions
after the K-factor pivot point has been set, use the following procedure
(fig. A3):
     (1)  Position the pitobe nozzle at the sampling point.
     (2)  Read the pitot tube AP.
     (3)  Align the AP through the K-factor pivot point
     (4)  Obtain AH and adjust metering valves.
     The nomograph assumes the following, once the K-factor pivot point is
set:
     (1)  T  does not change more than 25° for T  < 1000°F or 50° for
           s                                    s
T  > 1000°F.
 s
     (2)  D is not changed during the test.
     (3)  T  was estimated correctly and does not vary more than 10°.
     (4)  Percent H^O remains constant, within +1.0 percent.
     (5)  P  and P  remain constant, within +1.0 percent.
           s      m                         —
                                  172

-------
CORRECTION
FACTOR,
C PITOT READING,


ORIFICE READING,
AH
\o^
9 —
8 —
7 —
6— •
.5
•=
5~1
«:

i- =
—
^

—
™
~
~
2_
_
^
__
—


i —
0 9—
0 8 —
0.7 —
0.6-=
0.5-1
z
0 4HE
-H
0 3-=
""
0 2—
—
—
~

0 1 —



REF. A —















•-REF. B
£>d..
•~£4Mp/f: .
^^-C5 ^
r-i, i^
-Z^WlPLE •
-..^
















— 2 0
-

— 1 5
—
_
— 1.0
— 09
HLo.8

«— 0.7
•—
^— 0 6

^
•— 0 ^












.





— 2500
Z.
—7000
-
— 1500
1.
-^-1 000

— 800
^_
-^,600
^560-^,^
— 400 **•'
«- 300
— 200
— 1 00
— 0
STACK
TEMPERATURE,
TS


SLIDING
SCALE
CUT ALONG LINES



AP

K FACTOR o.ooi —


























.^^PIVOT POINT
••-^^.N.
^^













—
0.002^
0 003-^
—
0 004^
-5
PROBE o 005-S
TIP DIAMETER, —
0 006-=
LJ — ^
0 01 —

















'*
-------
APPENDIX C    ILLUSTRATED AUDIT PROCEDURES

     A flow chart of the operations involved in an auditing program from
first setting desired limits on the data quality to filing the results is
given below.  Assumed numbers are used and a sample calculation of an audit
is performed in the flow chart.  Each operation is referred to the section
in the text of the report where it is discussed.
                                   174

-------
MANAER
7.
    LIMITS FOR DATA QUALITY CAN BE SET BY WHAT
    IS DESIRED OR FROM THE NATURAL VARIABILITY
    OF THE METHOD WHEN USED BY TRAINED AND
    COMPETENT PERSONNEL^	FOR THIS EXAMPLE, IT
    IS ASSUMED THAT CV{PMR} =9.3 PERCENT
    (subsec.4.1), AND USING + 3 CV{PMR},  THE
    LIMITS ARE L = -28 PERCENT AND U = 28
    PERCENT.

    FROM PRIOR KNOWLEDGE OF DATA QUALITY, ESTIMATE
    THE PERCENTAGE OF FIELD MEASUREMENTS  FALLING
    OUTSIDE THE ABOVE LIMITS.  IF NO INFORMATION
    IS AVAILABLE, MAKE AN EDUCATED GUESS.  IT IS
    ASSUMED IN THIS EXAMPLE THAT 50 PERCENT OF THE
    FIELD DATA ARE OUTSIDE THE LIMITS L AND U
    (subsec. 4.4.4).

    DETERMINE:  (1) COST OF CONDUCTING AN AUDIT,
    (2) COST OF FALSELY INFERRING THAT GOOD DATA
    ARE BAD, (3) COST OF FALSELY INFERRING THAT
    BAD DATA ARE GOOD, AND (4) COST SAVINGS FOR
    CORRECTLY IDENTIFYING BAD DATA (subsec. 4.4.4).

    DETERMINE THE AUDIT LEVEL EITHER BY (1) MINI-
    MIZING AVERAGE COST USING EQUATION (41) OF
    SUBSECTION 4.4.4, OR (2) ASSURING A DESIRED
    LEVEL OF CONFIDENCE IN THE REPORTED DATA
    THROUGH STATISTICS.  FOR THIS EXAMPLE, THE
    AUDIT LEVEL IS TAKEN AS n = 5 (fig. 15 ).
BY TEAMS, TYPES OF SOURCES, OR GEOGRAPHY,
GROUP FIELD TESTS INTO LOTS (GROUPS) OF ABOUT
20 THAT WILL BE PERFORMED IN A PERIOD OF ONE
CALENDAR QUARTER.

SELECT n OF THE N TESTS FOR AUDITING.  COMPLETE
RANDOMIZATION MAY NOT BE POSSIBLE DUE TO AUDI-
TOR'S SCHEDULE.  THE PRIMARY POINT IS THAT THE
FIELD TEAM SHOULD NOT KNOW IN ADVANCE THAT
THEIR TEST IS TO BE AUDITED.

ASSIGN OR SCHEDULE AN AUDITOR FOR EACH FIELD
TEST.
                                                         SET DESIRED
                                                       LOWER AND UPPER
                                                       LIMITS FOR DATA
                                                      QUALITY, L AND U
                                                      ESTIMATE AVERAGE
                                                      QUALITY OF FIELD
                                                      DATA IN TERMS OF
                                                           L AND U
                                                        DETERMINE OR
                                                       ASSUME RELEVANT
                                                            COSTS
                                                            I
                                                       DETERMINE AUDIT
                                                         LEVEL FROM
                                                       STATISTICS,  OR
                                                        AVERAGE COST
                                                          GROUP FIELD TESTS
                                                          INTO LOT SIZES  OF
                                                            ABOUT N = 20
                                                           RANDOMLY  SELECT
                                                           n  OF THE  N TESTS
                                                            FOR AUDITING
                                                           ASSIGN/SCHEDULE
                                                           AUDITOR(S)  FOR
                                                           FOR THE n AUDITS
                                                                T
                                   175

-------
 AUDITOR
 8.
10.
11.
12.
13.
THE AUDITOR OBTAINS APPROPRIATE CALIBRATED
EQUIPMENT AND SUPPLIES FOR THE AUDIT
(subsec. 4.3).
     OBSERVE THE FIELD TEAM'S  PERFORMANCE  OF THE
     FIELD TEST.  FILL IN THE  AUDITOR'S  CHECKLIST
     (table 8) AND NOTE ANY UNUSUAL CONDITIONS
     THAT OCCURRED DURING THE  TEST.
                                                           PREPARE  EQUIPMENT
                                                              AND  FORMS
                                                           REQUIRED IN AUDIT
IN THE FIELD TEAM'S HOME LABORATORY, MAKE
INDEPENDENT DETERMINATIONS OF Cp> Dn, y, AND
AH@ (subsec. 4.3) ACCORDING TO THE CALIBRATION
PROCEDURES GIVEN IN SUBSECTION 2.2.
10
OBSERVE ON-SITE
PERFORMANCE
OF TEST
+
VERIFY CALIBRATION
RECORDS AND PERFORM
CALIBRATION CHECKS
IN TEAM'S HOME
LABORATORY
STARTING WITH THE RAW DATA FROM THE FIELD
AND USING AUDIT VALUES, PERFORM ALL THE
CALCULATIONS NECESSARY TO ARRIVE AT A VALUE
FOR d (subsec. 4.3, fig.,  10).
THE AUDITOR'S REPORT SHOULD INCLUDE (1) DATA
SHEET FILLED OUT BY THE FIELD TEAM (fig. 3),
(2) AUDITOR'S CHECKLIST WITH COMMENTS
(table 8), (3) AUDIT DATA SHEET WITH CALCULA-
TIONS (fig. 11), and (4) A SUMMARY OF THE
TEAM'S PERFORMANCE WITH A NUMERICAL RATING
(subsec. 4.3).

THE AUDITOR'S REPORT IS FORWARDED TO THE
MANAGER.
11
                                                           PERFORM CALCULA-
                                                          TIONS  TO DETERMINE
                                                              PMR-PMR.
                                                          d = ^MR-^x100
12
                                                                PREPARE
                                                                 AUDIT
                                                                REPORT
13
                                                                FORWARD
                                                               REPORT TO
                                                                MANAGER
MANAGER
14.  COLLECT THE AUDITOR'S REPORTS FROM THE n
     AUDITS OF THE LOT OF N STACKS.  IN THIS
     CASE n = 5 AND ASSUMED VALUES FOR THE
     AUDITS ARE dj = 12.0,d2 = -6.0, d3 = 3.0,
     d  = 15.0 AND d,- = 9.0 (table 8).
                                                  14
                                                           COMBINE
                                                         RESULTS OF
                                                          n AUDITS
                                                                 I
                                    176

-------
15.   CALCULATE d AND s .  ACCORDING TO THE  SAMPLE  IN
     TABLE 10.  RESULTS  OF THIS  SAMPLE  CALCULATION
     SHOW 3 = 6.6,
     4.4.3).
                   AND s .  = 8.3 (table 8,  subsec.
                                                        15
                                                             CALCULATE THE
                                                             MEAN, 3, AND
                                                               STANDARD
                                                             DEVIATION, sd
16.
17.
18.
19.
20.
     USE A t-TEST TO CHECK d FOR SIGNIFICANCE,  FOR
     THIS EXAMPLE t = 6.6 x /5/S.3 = 1.78.   THE
     TABULATED t-VALUE FOR 4 DEGREES OF FREEDOM AT
     THE 0.05 LEVEL IS 2.13; HENCE, d IS NOT
     SIGNIFICANTLY DIFFERENT FROM 0 AT THIS LEVEL.
     ALSO, s, IS CHECKED AGAINST THE ASSUMED VALUE
     OF 9.3 PERCENT BY A CHI-SQUARE TEST.
                                                       16
     X2/f =
                    =  (8.3)2/(9.3)2  =  0.797
                                                        17
     THE TABULATED VALUE  OF x/4  AT  THE  95  PER-
     CENT LEVEL IS 0.711; HENCE,  s,  IS SIGNIF-
     ICANTLY DIFFERENT FROM 9.3 PERCENT  (In this
     case it is a  significant  improvement).

     OBTAIN THE VALUE  OF  k FROM TABLE 9,  FOR n =  5
     AND p = 0.1.   THIS VALUE  IS  2.742,  THEN
     3 + k s .  = 6.6 +  2.742(8.3)  = 29.4  AND
     3 = k s°  = 6.6 -  2.742(8.3)  = -16.2
     (subsec?  4.4.3).
     COMPARE THE ABOVE CALCULATIONS  WITH  LIMITS         18
     L AND U (subsec.  4.4.3).   FOR THIS EXAMPLE

               3 + k sd =  29.4  >  U = 28

               d - k s . =  -16.2 > L  = -28.
                      d
     THE UPPER LIMIT U HAS BEEN EXCEEDED.   BOTH
     3 AND s .  WERE ACCEPTABLE INDIVIDUALLY  BUT
     WHEN COMBINED THE UPPER LIMIT WAS EXCEEDED.

     STUDY THE AUDIT AND FIELD  DATA  FOR SPECIFIC        19
     AREAS OF  VARIABILITY, SELECT THE MOST  COST
     EFFECTIVE ACTION OPTION(S) THAT WILL RESULTS
     IN GOOD QUALITY DATA  (subsec. 4.2).  NOTIFY
     THE FIELD TEAMS TO IMPLEMENT THE SELECTED
     ACTION OPTION(S).

     A COPY OF THE AUDITOR'S REPORT  SHOULD  BE SENT      20
     TO THE RESPECTIVE FIELD TEAM.   ALSO, THE DATA
     ASSESSMENT RESULTS, i.e.,  CALCULATED VALUES OF
     d, s ,, AND COMPARISON WITH THE  LIMITS  L AND U
     SHOUCD BE FORWARDED TO EACH  TEAM INVOLVED IN
     THE N FIELD TESTS.
                                                                 TEST
                                                               3 AND s.
i
                                                               CALCULATE
                                                               d +  k s .
                                                                  AND Q
                                                               3 -  k s,
                                                                  I
                                                                COMPARE
                                                                (16) WITH
                                                                L AND U
                                                                MODIFY
                                                              MEASUREMENT
                                                                METHOD
                                                                INFORM
                                                              FIELD TEAMS
                                                               OF AUDIT
                                                                RESULTS
                                  177

-------
21.  THE FIELD DATA WITH AUDIT RESULTS ATTACHED ARE
     FILED.  THE AUDIT DATA SHOULD REMAIN WITH THE
     FIELD DATA FOR ANY FUTURE USES.
21
        FILE AND
      CIRCULATE OR
      PUBLISH FIELD
          DATA
                                    178

-------
APPENDIX D
            GLOSSARY OF SYMBOLS
     This is glossary of symbols as used in this document.  Symbols used and
defined in the reference method (appendix A) are not repeated here.
SYMBOL
  N
  n
CV{X}
CV{X}
 a{X}

 s(X}
   R
 e{M
    n
   P
   k
 P{Y}
 (n - D

 2/(n - D
                         DEFINITION
Lot size, i.e., the number of field tests to be treated as
a group.
Sample size for the quality audit (section IV).
Assumed or known coefficient of variation (100 ax/yx)
Computed coefficient of variation (100 s /X) from a finite
                                        A
sample of measurements.
Assumed standard deviation of the parameter X (population
standard deviation).
Computed standard deviation of a finite sample of measure-
ments (sample standard deviation)
Computed bias of the parameter X for a finite sample
(sample basis).
Range, i.e., the difference in the largest and smallest
values in r replicate analyses.
Random error associated with the measurement of particulate
mass, M .
The percent difference in the audit value and the value of
                                                        .th
PMR arrived at by the field crew for the j   audit.
Mean difference between PMRj and PMR .  for n audits expressed
as a percent.
Computed standard deviation of differences between PMR. and
PMR .  expressed as a percent.
Percent of measurement outside specified limits L and U.
Constant used in sampling by variables  (section IV).
Probability of event Y occurring
Statistic used to determine if the sample bias, d, is
significantly different from zero (t-test).
                                                     2
Statistic used to determine if the sample variance, s , is
                                                    2
significantly different from the assumed variance, a , of
the parent distribution (chi-square test)
                                   179

-------
APPENDIX D
      GLOSSARY OF SYMBOLS (CONTINUED)
SYMBOL
   L
   u
   CL
  LCL
  UCL
  PMR

  PMRc

  PMR
     a

  PMR
                       DEFINITION
Lower quality limit used in sampling by variables.
Upper quality limit used in sampling by variables.
Center line of a quality control chart.
Lower control limit of a quality control chart.
Upper control limit of a quality control chart.
Particulate mass emission rate reported by the field team for
a sample run; it could be either PMR  or 1/2(PMR  + PMR ).
                                    C           C      3.
Particulate mass emission rate calculated by the sample con-
centration method, i.e., PMR  = C  x Q , g/hr.
                            OSS
Particulate mass emission rate calculated by the ratio of
                          Mn As
area method, i.e., PMR  = — —> g/hr.
                              n
Average particulate mass emission rate for a field test, i.e.,
the average of three sample runs, g/hr.
                                    180

-------
APPENDIX E                  GLOSSARY OF TERMS

     The following glossary lists and defines the statistical terms as used
in this document.

Accuracy. ...... A measure of the error of a process expressed as a
                      comparison between the average of the measured values
                      and the true or accepted value. It is a function of
                      precision and bias.
Bias	The systematic or nonrandom component of measurement
                      error.
Lot	.A specified number of objects to be treated as a
                      group, e.g., the number of field tests to be conducted
                      by an organization during a specified period of time.
Measurement method. . A set of procedures for making a measurement.
Measurement process . The process of making a measurement including method,
                      personnel, equipment, and environmental conditions.
Population	A large number of like objects (i.e., measure-
                      ments, checks, etc.)  from which the true mean and
                      standard deviation can be deduced with a high degree
                      of accuracy.
Precision 	 The degree of variation among successive, independent
                      measurements (e.g.,  on a homogeneous material) under
                      controlled conditions, and usually expressed as a
                      standard deviation or, as is done here, as a
                      coefficient of variation.
Quality audit .... A management tool for independently assessing data
                      quality.
Quality control
   check	Checks made by the field crew on certain items of
                      equipment and procedures to assure data of good
                      quality.
Sample  	 Objects drawn, usually at random, from the lot for
                      checking or auditing purposes.
                                   181

-------
APPENDIX F
CONVERSION FACTORS
Conversion factors for converting the U.S. customary units to the
International System of Units (SI)* are given below.
      To Convert from
               To
                       Multiply by
                                   Length
foot
inch
inch of mercury (in. of Hg) (32°F)
inch of mercury (in. of Hg) (60°F)
millimeter mercury  (mmHg)   (32°F)
inch of water (in. of H20) (29.2°F)

inch of water (in. of HJD) (60°F)
pound-force  (Ibf avoirdupois)


pound-mass (Ibm avoirdupois)


degree Celsius

degree fahrenheit

degree rankine

degree fahrenheit

kelvin
foot/second
foot/minute
cubic foot  (ft )
foot  /minute
    Q
foot  /second
                             9
                         (N/nu)
                         (NAO
                         (N/ni )

                         (N/m2)
  meter (m)
  meter (m)

Pressure

  Newton/meter^
  Newton/meter^
  Newt on/meter,.
  Newton/meter"

  Newton/meter

Force

  Newton (N)

Mass

  kilogram  (kg)

Temperature

  kelvin (K)

  kelvin (K)

  kelvin (K)

  degree Celsius

  degree Celsius

Velocity

  meter/second  (m/s)
  meter/second  (m/s)

Volume
       3 ,  3,
  meter  (m  )

Volume/Time
       3          3
  meter /second  (m /s)
       3          3
  meter /second  (m /s)
                                      0.3048
                                      0.0254
3386.389
3376.85
 133.3224
 249.082

 248.84
                                      4.448222


                                      0.4535924


                                     = tc + 273.15
                                     = (tp+459.67)/l.

                                     - V1-8
                                     = (tp - 32)71.8
                                  t^ =
                                          - 273.15
                                      0.3048
                                      0.00508
                                      0.02832


                                      0.0004719
                                      0.02832
 Metric Practice Guide  (A Guide to the Use of SI, the International Systems
 of Units), American National Standard Z210.1-1971, American Society  for
 Testing and Materials, ASTM Designation:E380-70, Philadelphia, Pa.,  1971.
                                   182

-------
                                   TECHNICAL REPORT DATA
                            (Please read Instructions on the reverse before completing)
 1. REPORT NO.

 EPA-650/4-74-005d
                                                            3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
 GUIDELINES  FOR  DEVELOPMENT OF A  QUALITY ASSURANCE
 PROGRAM:  DETERMINATION OF PARTICULATE EMISSIONS
 FROM STATIONARY SOURCES
                                                            5. REPORT DATE
                                                              June 1976
             6. PERFORMING ORGANIZATION CODE
7 AUTHOR(S)
                                                            8. PERFORMING ORGANIZATION REPORT NO.
 Franklin Smith
 Denny E. Wagoner
9. PERFORMING ORGANIZATION NAME AND ADDRESS

 Research Triangle Institute
 Research Triangle Park, NC   27709
              10. PROGRAM ELEMENT NO.

                 1HA327	
              11. CONTRACT/GRANT NO.
                                                               68-02-1234
 12. SPONSORING AGENCY NAME AND ADDRESS
 Environmental  Monitoring and Support Laboratory
 Office of Research and Development
 U.S. Environmental Protection Agency
 Washington,  D.  C.   20460
                                                            13. TYPE OF REPORT AND PERIOD COVERED
              14. SPONSORING AGENCY CODE
                 EPA-ORD
15. SUPPLEMENTARY NOTES
16. ABSTRACT

       Guidelines  for the quality  control of measurements of particulate emissions
 from stationary sources by the  Federal  reference method are presented.   These
 include:

       1.  Good  operating practices,

       2.  Directions on how to  assess performance  and  qualify data,

       3.  Directions on how to  identify trouble and  improve data quality,

       4.  Directions to permit  design of auditing  activities.

       The document is not a research  report.  It is  designed for use  by operating
 personnel.
17.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS  C.  COS AT I Field/Group
 Quality assurance
 Quality control
 Air Pollution
 Gas Analysis
                              13H
                              14D
                              13B
                              07D
                              14B
13. DISTRIBUTION STATEMENT
 Release to Public
                                               19. SECURITY CLASS (This Report)
                           21. NO. OF PAGES

                              1ft?	
                                               20. SECURITY CLASS (This page)
                                                Unclassified
                                                                          22. PRICE
EPA Form 2220-1 (9-73)

-------
    9
   i
O 2
3 O
U»I
?ssS
II "

-------