EPA/450/2-82/003
                            Air Pollution Training Institute        EPA 450/2-82-003
             	    »rotection     MD 20                  July, 1982
             Agency            Environmental Research Center
                            Research Triangle Park, NC 27711
             Air

             APTI

             Correspondence Course 414

             Quality Assurance for

             Source Emission

             Measurement Methods


             Guidebook
 I
 w
            Course Developed By:
            Jamas A. Jahnke. Ph.D.

            Instructional Design By:
            Monica Leslie

            Northrop Services, Inc.
            P.O. Box 12313      	
            Research Triangle Park, NC 27709

            Under Contract No.
            68-02-3573
            EPA Project Officer
            R. E. Townsend

            United States Environmental Protection Agency
            Office of Air, Noise, and Radiation
            Office of Air Quality Planning and Standards
            Research Triangle Park, NC 27711

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                                  Notice

This is not an official policy and standards document. The opinions and selections
are those of the authors and not necessarily those of the Environmental Protection
Agency. Every attempt has been made to represent the present state of the art as
well as subject areas still under evaluation. Any mention of products or organiza-
tions does not constitute endorsement by the United States Environmental Protec-
tion Agency.


                             Availability

This document is issued by the Manpower and Technical Information Branch,
Control Programs Development Division, Office of Air Quality Planning and Stan-
dards,  USEPA. It was developed for use in training courses presented by the EPA
Air Pollution Training Institute and others receiving contractual or grant support
from the Institute. Other organizations are welcome to use the document.
  This publication is available, free of charge, to schools or governmental air
pollution control agencies intending to conduct a training course on the subject
covered. Submit  a written request to the Air Pollution Training Institute, USEPA,
MD 20, Research Triangle Park, NC 27711.
  Others may obtain copies, for a fee, from the National Technical Information
Service (NTIS), 5825 Port Royal Road, Springfield,  VA 22161.
                                     n

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                        Table of Contents

                                                                Page No.
Course Introduction	1

Quality Assurance Principles	7
  Lesson A—EPA Quality Assurance Policy and Volume I Review	9
    Reading Guidance—Assignment 1	11
      Reading Assignment 1 Review Exercises	19
      Answers to Reading Assignment 1 Review Exercises	20
    Reading Guidance—Assignment 2	21
      Reading Assignment 2 Review Exercises	83
      Answers to Reading Assignment 2 Review Exercises	86
  Lesson B—Volume III Overview	87
    Reading Guidance—Assignment 3	89
    Reading Guidance—Assignment 4	93
    Reading Guidance—Assignment 5	97
      Reading Assignments 3, 4, and 5 Review Exercises	98
      Answers to Reading Assignments 3,4, and 5 Review Exercises	102

Pretest Operations	103
  Lesson C—Procurement of Equipment	105
    Reading Guidance—Assignment 6	107
      Reading Assignment 6 Review Exercises	108
      Answers to Reading Assignment 6 Review Exercises	110
    Reading Guidance—Assignment 7	Ill
      Reading Assignment 7 Review Exercises	113
      Answers to Reading Assignment 7 Review Exercises	116
    Reading Guidance—Assignment 8	117
      Reading Assignment 8 Review Exercises	118
      Answers to Reading Assignment 8 Review Exercises	121
  Lesson D—Calibration of Equipment	123
    Reading Guidance—Assignment 9	125
      Reading Assignment 9 Review Exercises	127
      Answers to Reading Assignment 9 Review Exercises	129
    Reading Guidance—Assignment 10	131
      Reading Assignment 10 Review Exercises	134
      Answers to Reading Assignment 10 Review Exercises	136
  Lesson E—Presampling Operations	137
    Reading Guidance—Assignment 11	139
      Reading Assignment 11 Review Exercises	141
      Answers to Reading Assignment 11 Review Exercises	143
                                    111

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Sampling and Analysis	145
  Lesson F—On-site Measurements	147
    Reading Guidance—Assignment 12	149
      Reading Assignment 12 Review Exercises	151
      Answers to Reading Assignment 12 Review Exercises	154
    Reading Guidance—Assignment 13	155
      Reading Assignment 13 Review Exercises	163
      Answers to Reading Assignment 13 Review Exercises	166
  Lesson G—Postsampling Operations	171
    Reading Guidance—Assignment 14	173
      Reading Assignment 14 Review Exercises	176
      Answers to Reading Assignment 14 Review Exercises	178
    Reading Guidance—Assignment 15	179
      Reading Assignment 15 Review Exercises	184
      Answers to Reading Assignment 15 Review Exercises	187

Calculations—Maintenance—Audits	189
  Lesson H—Calculations	191
    Reading Guidance—Assignment 16	193
      Reading Assignment 16 Review Exercises	196
      Answers to Reading Assignment 16 Review Exercises	197
  Lesson I—Maintenance Checks	199
    Reading Guidance—Assignment 17	201
      Reading Assignment 17 Review Exercises	201
      Answers to Reading Assignment 17 Review Exercises	203
  Lesson J—Auditing Procedures	205
    Reading Guidance—Assignment 18	207
      Reading Assignment 18 Review Exercises	210
      Answers to Reading Assignment 18 Review Exercises	213
                                    IV

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                   Course Introduction
                        Overview of Course

Course Description

This training course is a 35-hour correspondence course dealing with quality
assurance procedures for EPA manual source measurement Methods 1 through 8.
The course reviews, in detail, essentials of equipment calibration, proper testing
methods, proper use of standardized testing forms, and EPA data tolerances.
Course topics include:
  •  quality assurance principles
  •  procurement of apparatus and supplies
  •  calibration of apparatus
  •  presampling operations
  •  on-site measurement methods
  •  postsampling operations
  •  equipment maintenance methods
  •  auditing procedures
  During 1980 and 1981 a series of workshops on quality assurance for source
measurements was presented by the EPA Manpower and Technical Information
Branch in collaboration with the EPA Quality Assurance Division and the EPA
Division of Stationary Source Enforcement. Over 250 individuals, including agency
personnel and source testing contractors, attended the workshops held at Research
Triangle Park, Dallas, Denver, and San Francisco. This correspondence course is
an outgrowth of these workshops. It has been designed to provide you with training
similar to that experienced by the workshop attendees.
  The course is intended for those who have had training or experience in source
sampling methods. It  is not designed to give the theory of source sampling methods
or teach how they are done. APTI Courses 450 and 468 are intended for that pur-
pose. This course is intended to help refine the technique of a testing organization
so that quality data can be assured.
  The following documents will be used as texts:
     • EPA 600/4-77-0276 Quality Assurance Handbook for Air Pollution
      Measurement Systems.  Volume III—Source Measurements
     • EPA 600/9-76-005 Quality Assurance Handbook for Air Pollution
      Measurement Systems.  Volume I—Principles (selected sections)

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Course Goal

This course is designed to familiarize you with quality assurance guidelines
prescribed in Volume III of the EPA Quality Assurance Handbook for Air Pollu-
tion Measurement Systems. It is intended to assist you in applying quality control
methods in the performance  of Federal source testing methods.

Course Objectives

Upon completion of this course, you should be able to:
   1. explain why quality assurance procedures are a vital part of the Environ-
      mental Protection Agency's air monitoring programs.
   2. initiate the development of a source test team quality assurance program.
   3. list at least eight elements of an effective quality assurance program.
   4. define: quality assurance, quality control, representative samples, chain of
      custody, collaborative  test, audit.
   5. use the procurement sections of Volume III  and associated activity matrices
      in obtaining the proper equipment for a source sampling testing team.
   6. employ the guidelines  of Volume III in calibrating source testing equipment.
   7. use the checklists provided in Volume III in preparing sampling equipment
      before a source test.
   8. list at least five procedures which should be  routinely  followed in order to
      maintain source  testing equipment.
   9. use the data and calculation forms provided in Volume III.
  10. describe how audit samples can be used in a quality assurance program
      designed for a source test team.
  11. list at least three functions of a test auditor  and point out at least two pro-
      cedures that the auditor should specifically observe during the performance
      of each of the EPA reference methods for paniculate  matter, SOZ, NOX,
      and Oj/CO».

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Sequence, Lesson Titles, and Trainee Involvement Time


                                                     Approximate trainee
                                                       involvement time
                                                           (hours)
Course Introduction	0.5

Quality Assurance Principles
  Lesson A—EPA Quality Assurance Policy and Volume I Review .... 3.5
           Reading Assignments 1 and 2
  Lesson B —Volume III Overview	3
           Reading Assignments 3 through 5

Pretest Operations
  Lesson C—Procurement of Equipment	3
           Reading Assignments 6 through 8
  Lesson D—Calibration of Equipment	4
           Reading Assignments 9 and 10

                            Quiz 1	1

  Lesson E— Presampling Operations	3
           Reading Assignment 11

Sampling and Analysis
  Lesson F— On-site Measurements	4
           Reading Assignments 12 and 13
  Lesson G—Postsampling Operations	4
           Reading Assignments 14 and 15

                            Quiz 2	1

Calculations—Maintenance—Audits
  Lesson H—Calculations	2
           Reading Assignment 16
  Lesson I— Maintenance Checks	1
           Reading Assignment 17
  Lesson J— Auditing Procedures	3
           Reading Assignment 18

                          Final Exam	2

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Requirements for Successful Completion of this Course

In order to receive 3.5 Continuing Education Units (CEUs) and a certificate of
course completion you must:
  • take two supervised quizzes and a supervised final examination.
  • achieve a final course grade of at least 70 (out of 100) determined as
    follows:
    • Quiz 1 is 20% of the final grade.
    • Quiz 2 is 20% of the final grade.
    • The final examination is 60% of the final grade.
                     Use of Course  Materials

The Materials You'll Need

  • APTI Correspondence Course 414 Quality Assurance for Source Emissions—
    Guidebook
  • Quality Assurance Handbook for Air Pollution Measurement Systems.
    Volume HI—Source Measurements EPA  600/4-77-0276 (with updates to
    January 15, 1980)


How to Use this Guidebook

       Relationship Between Guidebook and Assigned Reading Materials
This guidebook directs your progress through Volume III of the Quality Assurance
Handbook for Air Pollution Measurement Systems. Excerpts from Volume I are
included in the guidebook to provide you with a basic introduction to quality
assurance principles. If you wish to obtain the complete text of Volume I, it may
be ordered from the Quality Assurance Division of EPA in Research Triangle
Park,  NC.
  If you use the guidebook instructions with the provided reading material, we
think you will find the subject material both interesting and enjoyable. Review
exercises and problems focus on specific and important aspects of the quality
assurance manuals. Although not all aspects of the QA guidelines are covered by
the review exercises and quizzes,  after you complete the course you  will be able to
effectively use QA Volume III.

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                      Description of Guidebook Sections
This guidebook contains ten lessons separated into four units. Each lesson contains
the following:
   • lesson learning goal and objectives
   • reading assignment(s)
   • reading guidance
   • review exercises
   • answers to review exercises
   Complete the review exercises immediately after reading the assigned materials.
You may find it helpful to look over the review questions before reading. By having
an idea of what to look for in the reading materials, your attention will be better
focused and your study will be more efficiently directed.
NOTE: If more than one person will be using these materials, we recommend that
you use a separate sheet of paper to record your answers to the review exercises.


Instructions for Completing the Quizzes and the Final Examination

   • You should have received, along with this guidebook, a separate sealed
    envelope containing two quizzes and a final examination.
   • You must arrange to have someone serve as your test supervisor.
   • You must give the sealed envelope containing the quizzes and final examina-
    tion to your test supervisor.
   • At designated times during the course, under the supervision of your
    test supervisor, complete the quizzes and the final exam.
   • After you have completed a quiz or the exam, your test supervisor must
    sign a statement on the quiz/exam answer sheet certifying that the quiz or exam
    was administered in accordance with the specified test instructions.
   • After signing the quiz/exam answer sheet, your test supervisor must mail the
    quiz or exam and its answer sheet to the following address:
                      Air Pollution Training Institute
                      Environmental Research Center
                      MD-17
                      Research Triangle Park,  NC 27711
   • After completing a quiz, continue with the course. Do not wait for quiz results.
   • Quiz/exam and course grade results will be mailed to you.

// you have questions, contact:

                      Air Pollution Training Institute
                      Environmental Research Center
                      MD-17 .
                      Research Triangle Park,  NC 27711
                      Telephone numbers:
                              Commercial: (919) 541-
                              FTS: 629-

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                          02
'0*?

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     Quality Assurance
            Principles
Lesson A—EPA Quality Assurance Policy and Volume I Review
        Reading Assignment 1
        Reading Assignment 2

Lesson B —Volume III Review
        Reading Assignment 3
        Reading Assignment 4
        Reading Assignment 5

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                        Lesson  A
      EPA Quality Assurance Policy and
                    Volume I Review
Lesson Goal

The goal of this lesson is to familiarize you with EPA's quality assurance policies
and its approach to implementing the use of quality assurance plans for manual
source sampling programs.

Lesson Objectives

After completing this lesson, you should be able to:
  1. explain why quality assurance procedures are a vital part of the Environ-
    mental Protection Agency's air monitoring programs.
  2. initiate the development of a quality assurance program for source test teams.
  S. list at least eight elements of an effective quality assurance program.
  4. define: quality assurance,  quality control, accuracy, precision, quality
    assurance plan, quality assurance manual, performance audit, system audit.
  5. describe the importance of quality assurance programs  to an organization.
  6. recognize the contribution of training programs to the reporting of high
    quality data.
  7. list at least four items that should be included in a quality assurance report to
    management.
  8. distinguish between a quality assurance manual and a quality assurance plan.

Materials

Assignment 1
  • Memorandum—May SO, 1979, Douglas Costle
  • Strategy for the  Implementation of EPA's Mandatory Quality Assurance
    Program
  • Memorandum—June 14, 1979, Douglas Costle
  • Memorandum—November 2, 1981, Anne Gorsuch
Assignment 2
  General information (contained in this guidebook) on the topic of quality
  assurance. This material has been extracted from Volume I of the  QA Hand-
  book series.

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      Reading Guidance—Assignment 1
This lesson reviews the Environmental Protection Agency's quality assurance
policies for air pollution data. Reading Assignment 1 includes memos giving the
rationale for the development of quality assurance programs, and Reading Assign-
ment 2 provides guidance for their development.
  The Quality Assurance  Handbook aids agencies, contracting firms, and
industries that want to initiate quality assurance programs and plans within their
organizations. This correspondence course is intended to help make using the
handbook easier.
            Begin by reading pages IS through 18 of this guidebook.
                                  11

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                                                           Attachment B


           UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                            WASHINGTON. D C  20460
                                                                  THE ADMINISTRATOR
                                 May 30. 1979
MEMORANDUM
TO:        Deputy Administrator
           Director, Science Advisory Board
           Director, Office of Regional and Intergovernmental Operations
           Regional Administrators
           Assistant Administrators
           General Counsel

SUBJECT:   Environmental Protection Agency (EPA) Quality Assurance
           Policv Statement
     The EPA must have a comprehensive quality assurance effort to
provide for the generation, storage, and use of environmental data which
are of known quality. Reliable data must be available to answer
questions concerning environmental quality and pollution abatement
and control measures. This can be done only through rigorous
adherence to established quality assurance techniques and practices.
Therefore, I am making participation in the quality assurance effort
mandatory for all EPA supported or required monitoring activities.

     An Agency quality assurance policy statement is attached which
gives general descriptions of program responsibilities and basic
management requirements. For the purpose of this  policy  statement,
monitoring is defined as all environmentally related measurements
which are funded by the EPA or which generate data mandated by the EPA.

     A detailed implementation plan for a total Agency quality
assurance program is being developed for issuance at a later date.
A Select Committee for Monitoring, chaired by Dr. Richard Dowd, is
coordinating this effort, and he will be contacting you directly
for your participation and support. I know that each of you shares
my concern about the need to improve our monitoring programs and
data; therefore, 1 know that you will take the necessary actions
that will ensure the success of this effort.

                                            Douglas M. Costle


Attachment
                                   IS

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                                                                DATE:  05-19-80
                                                                Page 1 of 15
                      Strategy for the Implementation
                                  of the
                     Environmental Protection Agency's
                 Mandatory Quality Assurance (QA) Program
1.  Introduction

The EPA must have a comprehensive QA program to provide for the generation,

storage, and use of environmental data. Valid data of verifiable quality

must be available to provide a sound basis for effective decisions concerning

environmental quality, pollution abatement, and control measures. The QA

program can succeed only through rigorous adherence to established QA tech-

niques and practices.


In the past, there has been a high degree of fragmentation, lack of coordination,

poorly identified needs and resources, and duplication of efforts in the QA pro-

gram. For these reasons, it is now Agency policy, as enunciated by the Adminis-

trator in memoranda of May 30, 1979 and June 14, 1979, that all Regional Offices,

Program Offices, EPA Laboratories, and those monitoring and measurement efforts

supported or mandated through contracts, regulations, or other formalized agree-

ments participate in a centrally managed QA program. Regional Offices should work

cooperatively with States to assist them in developing and implementing QA programs.


The mandatory QA program covers all environmentally-related measurements.

Environmentally-related measurements are defined as "essentially all field and

laboratory investigations that generate data involving the measurement of chemical,

physical, or biological parameters in the environment; determining the presence or

absence of pollutants in waste streams; health and ecological effect studies;

clinical and epidemiological investigations; engineering and process evaluations;
                                        14

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                                                                DATE: 05-19-80
                                                                Page 2 of 15


 studies  involving laboratory simulation of environmental events; and studies

 or measurements on pollutant transport, including diffusion models.


 This document presents  the strategy for the development of an Agency QA program

 in accordance with the  Agency policy. This strategy describes, in general, the

 total program effort with respect to what must be done. This strategy does not

 attempt  to describe how, in detail, the program is to be implemented within the

 individual Program and  Regional Offices, or the EPA Laboratories. Subsequent

 guidance documents will enable the Program and Regional Offices and the EPA

 Laboratories to develop detailed QA plans.



 II.  Quality Assurance  Goals and Objectives

 The primary goal of the QA program is to insure that all environmentally-related

 measurements supported  or required by the EPA result in data of known quality.

 To meet  this goal, the  QA program must provide for the establishment and use of

 reliable monitoring and measurement systems to obtain data of necessary quality

 to meet planned Agency needs.


 Initial objectives are  the development and implementation of QA program plans by

 each of the Program and Regional Offices and EPA Laboratories which will ensure

 that the QA goal can be achieved nationally.


 Long-term objectives include (1) providing quantitative estimates of the quality

of all data supported or required by the Agency, (2) improving data quality where

 indicated, and (3) documenting progress in achieving data quality.


A continuing objective is to promote and develop optimally uniform approaches.
                                        15

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                                                               DATE:  05-19-80
                                                               Page  3 of  15
procedures, techniques, reporting methods, etc., across media and across

Regional Offices, Program Offices, and EPA Laboratories. It is important (and

most efficient and effective) for all organizations within EPA to employ the

same QA language, consistent policies, procedures, and techniques when inter-

acting with the States, industry, the public, contractors, grantees, QA-involved

professional societies, other Governmental agencies, and national and inter-

national organizations.
                                       16

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ft*
t 222
         UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                          WASHINGTON  DC  20460
                                                       Attachment C

                                                                THE ADMINISTRATOR
                               June  14,  1979
MEMORANDUM

SUBJECT:  Quality Assurance Requirements for all EPA Extramural
          Projects Involving Environmental Measurements

    FOR:  The Deputy Administrator
          Assistant Administrators
          Regional Administrators
          General Counsel
     Over the past several years, the EPA has become more and more
dependent on extramural projects to provide the environmental measure-
ments we use as a foundation for our standards, regulations and
decisions. While in most instances these projects are providing
data of proven quality that is acceptable for the Agency's purposes,
there have been, regrettably, some instances of Agency funds paid
for poor quality, unusable data.

     In order to assure that all environmental measurements done by
extramural funding result in usable data of known quality, I am
making the inclusion of the attached "Quality Assurance Requirements"
mandatory for all EPA grants, contracts, cooperative agreements, and
interagency agreements that involve environmental measurements. In
addition to these general requirements, I expect every Project Officer
to include whatever additional specific quality assurance requirements
are necessary in each extramural project under his control. Criteria
and guidelines in this area will be forthcoming from the Agency's
Quality Assurance Implementation Work Group. Further, I direct the
Assistant Administrator for Planning and Management to provide the
appropriate contract and grant regulations such that the attached
form "Quality Assurance Review for Extramural Projects Involving
Environmental Measurements" will be satisfactorily completed where
appropriate prior to the approval of any contracts or grants in FY-80.

     I recognize that this may increase the cost per environmental
measurement, but the benefits of a credible Agency data base that
provides a level of quality that meets the needs of users far out-
weigh any such increases.


                                             Douglas M. Costle

Attachment
                                   17

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            UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                             WASHINGTON DC  20460
                                                                  THE ADMINISTRATOR

                                November 2,  1981
MEMORANDUM

TO:       Associate Administrators
          Assistant Administrators
          Regional Administrators

SUBJECT:  Mandatory Quality Assurance Program


One of the major concerns of this administration and myself is that  we
support all of our actions and decisions with statistically representative
and scientifically valid measurement of environmental quality. To meet
this objective, it is essential that each of you continue to support and
implement the Agency's mandatory Quality Assurance program which is  being
implemented by the Office of Research and Development. It is especially
essential that you assure that the appropriate data quality requirements
are included in all of your extramural and intramural environmental
monitoring activities. I also am particularly concerned that you do  not
sacrifice quality for quantity when adjusting your program to meet our new
resource targets.

The attached Second Annual Quality Assurance Report demonstrates the
importance of this program in achieving our goals and objectives.
Recognizing its importance, I have asked Dr. Hernandez to closely monitor
this program's implementation and advise me of any problems that affect
the scientific data bases of the Agency.
                                              Anne M. Gorsuch

Attachment

cc:  Deputy Administrator
     Office Directors
                                    18

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             You have completed your reading for Assignment 1. Do
             the review exercises which follow and check your answers
             after you complete them. The correct answers are given
             on the page following the review exercises.
          Reading Assignment 1  Review Exercises
1. Valid and verifiable source-test data is needed by regulatory agencies:
   a.  so that source testing costs can be increased.
   b.  to provide a sound basis for regulatory decisions.
   c.  to derive theoretical models for combustion processes.
   d.  to ensure that data follow a log-normal distribution.
2. Which one of the follow is not a long-term objective of EPA's mandatory QA
   program?
   a.  to provide quantitative estimates of data quality
   b.  to document progress in improving the quality of environmental
      measurements reported to the agency
   c.  to improve data quality
   d.  to increase the amount of data reported to the agency
3. EPA's mandatory QA program affects:
   a.  EPA laboratories.
   b.  organizations receiving EPA grants or contracts.
   c.  organizations with cooperative agreements with EPA.
   d.  all of the above
4. Volume III of the Quality Assurance Handbook for Air Pollution Measurement
   Systems is important to EPA's mandatory QA program since it:
   a.  promotes the use of uniform procedures for source testing.
   b.  requires all testing contractors to use the same data reporting forms.
   c.  is the only available handbook on source testing methods.
   d.  promotes the use of uniform procedures for continuous source emissions
      monitoring.
5. True or False? EPA's mandatory QA program is applicable only to air pollution
   measurements.
6. The SST source test team reported a Method 5 compliance test result of
   0.063582  gr/dscf± 0.0316 gr/dscf for a subpart D fossil-fuel-fired steam
   generator. Would this report be consistent with EPA's mandatory QA program?
   Yes	
   No	
   If no, why not?


                                    19

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1.
2.
3.
4.
5.
 a
 a
 a
^—•>
 a
>^*<
 T
 b
>>—<
 b
 b
 b
                           Answers to
         Reading Assignment 1 Review Exercises
      c  d
6.  No, since the number of significant figures reported is inconsistent with the
   accuracy of the reference method itself. The figures are also not reported in
   the units specified in the method.
                                  20

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       Reading  Guidance—Assignment  2
This assignment reviews many of the concepts involved in the subject of quality
assurance and gives directions for setting up a quality assurance program within an
organization. Portions of Volume I of the EPA Quality Assurance Handbook are
included in this section. You may obtain the complete handbook by writing to:
                     Quality Assurance Division
                     Environmental Monitoring and Support Laboratory
                     US Environmental Protection Agency
                     Research Triangle Park, NC 27711
and requesting: Environmental Protection Agency (EPA). 1976. Quality Assurance
Handbook for Air Pollution Measurement Systems. Volume I—Principles
EPA 600/9-76-005.
  In-depth training in  the principles discussed in Volume I can be obtained by
attending EPA APTI Course 470 Quality Assurance for Air Pollution Measurement
Systems. This four-day lecture course is designed for  quality assurance coordinators
or managers involved with quality assurance activities.
  Volume I of the Quality Assurance Handbook focuses on 23 elements of the
quality assurance wheel. Eight of these elements are considered essential when
setting up a new program. The discussion given in Volume I for each of these eight
elements is reproduced here for your review.
            Begin by reading the excerpts from Volume I. They are
            on pages 25 through 82 in this guidebook.
              The following comments introduce you to the reading
            assignment. Read them along with the excerpts; they will
            help familiarize you with some of the main ideas of
            quality assurance, and will make the reading assignment
            easier to understand.
 1.  Definition of quality assurance
    • Be sure to note the distinction between quality control and quality assurance.
    • What is the product with which EPA quality assurance programs are
      conceived?
                                    21

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2. Elements of quality assurance
   • The elements have been placed on the wheel in such a way that the quality
     assurance coordinator can select those applicable to his or her particular
     program.
   • The eight elements reviewed here should be considered from the very
     beginning in the development of a program. They are as follows:
     (1)  document control and revisions
     (2)  policy and objectives
     (3)  organization
     (4)  training
     (5)  audit procedures
     (6)  quality  reports to management
     (7)  quality  assurance manual
     (8)  quality  assurance plans for projects and programs
   • The 23 quality assurance elements can be grouped into four general
     categories:
     (1)  management activities
     (2)  measurement activities
     (3)  routine systems for program operation and support
     (4)  statistical techniques
3. Document control and revisions
   • Note the indexing format of the Volume I excerpts included here. Also note
     the indexing format in Volume III. The format  provides a means of tracking
     and updating entries in QA manuals  and plans.
   • The purpose of document control is to provide the latest procedures to all
     concerned.
   • The last page of this lesson is an outline of Volume III.  We will discuss this
     in depth later in this course. The manner in which Volume HI is
     documented is very important for its use.
4. Quality assurance policy and objectives
   • The QA policy of an organization must have the support of upper-level
     management if the QA program is to be effective. Note the mernos
     reproduced in Reading Assignment 1.
   • When reading the discussion of this element, note that data objectives
     should be specified for:
           completeness
           precision
           accuracy
           representativeness
           comparability
     However, cost should be kept in mind.
                                      22

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 5. Organization
    • Quality assurance is normally a separate function. The separation helps pre-
      vent bias and provides easier access to upper-level management.
    • A QA coordinator should be appointed and his function spelled out in a
      position description.
 6. Training
    • You cannot produce high quality data with people who do not know how to
      do their jobs. It is the responsibility of management to see that the job is
      done right.
 7. Audit procedures
    • Audit procedures should be implemented as quickly as possible when setting
      up a QA program.
    • Audits are one of the best ways of checking the quality of data.
 8. Quality reports to management
    • Feedback is very important for managers. Anything that affects management
      decisions should be included in the report.
    • Reports should be understood at a glance.  When possible, use charts and
      graphs to present data, rather than tables.
 9. The quality assurance manual
    • Note that a quality assurance  manual is general. It covers all of the Q/ pro-
      grams and methods used by an organization.
10. The quality assurance plan
    • Note that the quality assurance plan is method specific. It gives the specific
      QA requirements for a sampling procedure.
    • In this sense, the EPA QA Volume I provides guidance for the development
      of an organization's QA manual.  Volume III provides guidance for the
      development of source sampling QA plans  for  EPA Reference Methods A
      through 8.
11. Final note: Although not included in the excerpts here, it is important to men-
    tion the QA cycle. The cycle is shown below.


                                           Plan

                Take corrective action                     Implement
                                          Assess
    The effect of applying quality assurance techniques should result in the
    development of an on-going corrective action system. Once a QA plan is
    written and implemented, assessment procedures point out necessary corrective
    action which, in effect, revises the plan. The cycle continues in this manner,
    providing quality source sampling data.
                                      23

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                                   EPA-600/9-76-005
                                       January 1976
    QUALITY ASSURANCE HANDBOOK
                    FOR
AIR POLLUTION  MEASUREMENT SYSTEMS

          Volume I — Principles
           U.S. ENVIRONMENTAL PROTECTION AGENCY
             Office of Research and Development
         Environmental Monitoring and Support Laboratory
           Research Triangle Park, North Carolina 27711
                     25

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                                             Section No. 1.3
                                             Revision No. 0
                                             Date  May 1, 1975
                                             Page 1 of 2


1.3  DEFINITION OF QUALITY ASSURANCE(1~4)

     Quality assurance and quality control have been defined

and interpreted in many ways.  The more authoritative usages

differentiate between the two terms by stating that quality

control is "the system of activities to provide a quality

product," whereas quality assurance is "the system of activities

to provide assurance that the quality control system is

performing adequately."  In other words, quality assurance

is quality control for quality control.

     Quality control may also be understood as "internal

quality control;" namely, routine checks included in normal

internal procedures; e.g., periodic calibrations, duplicate

checks, split samples, and spiked samples.  Quality assurance

may also be viewed as "external quality control," those

activities that are performed on a more occasional basis,

usually by a person outside of the normal routine operations;

e.g., on-site system surveys, independent performance audits,

interlaboratory comparisons, and periodic evaluation of

internal quality control data.

     In this Handbook, the term quality assurance is used to

include the above meanings of both quality assurance and

quality control.

     While the objective of EPA's air programs is to improve

the quality of the air, the objective of quality assurance

for air programs is to improve or assure the quality of

measured data on pollutant concentrations.  Thus the "product"
                             26

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                                             Section No. 1.3
                                             Revision No. 0
                                             Date  May 1, 1975
                                             Page 2 of 2
with which quality assurance is concerned is data.

     Since air pollution measurements are made by numerous

agencies and private organizations at a large number of

field stations and laboratories, quality assurance is also

concerned with establishing and assessing comparability of

data quality among organizations contributing to data bases.

1.3.1  REFERENCES

1.   Juran, J.M.  Quality Control Handbook, 3rd Ed. McGraw-
     Hill, 1974.  Section 2.

2.   ASTM.  Designation E-36, "Standard Recommended Practice
     for Generic Criteria for Use in the Evaluation of
     Testing and/or Inspection Agencies."

3.   ASQC.  Standard A3-1971 (ANSI Standard Zl.7-1971),
     "Glossary of General Terms Used in Quality Control."

4.   Feigenbaum, A.V.  Total Quality Control, Engineering
     and Management.  McGraw-Hill, 1961.
                            27

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                                             Section No. 1.4
                                             Revision No. 0
                                             Date May 1, 1975
                                             Page  1 of  3
1.4  ELEMENTS OF QUALITY ASSURANCE

     A quality assurance program for air pollution measure-

ment systems should cover a number of areas or elements.

These elements are shown in Figure 1.4.1 in a "Quality

Assurance Wheel."  The wheel arrangement illustrates the

need for a quality assurance system that will address all

elements and at the same time will allow program managers

the flexibility to emphasize those elements that are most

applicable to their particular program.  Quality assurance

elements are grouped on the wheel according to the orga-

nization level to which responsibility is normally assigned.

These organizational levels are the quality assurance coor-

dinator (normally a staff function), supervisor (a line

function), and the operator.  Together the supervisor and

quality assurance coordinator must see that all these elements

form a complete and integrated system and are working to

achieve the desired program objectives.

     The three-digit numbers shown on the wheel show the

location in Section 1.4 where a description of the element

is provided.  Each element is described in three subsections

as follows:

     1.   ABSTRACT - A brief summary that allows the program

          manager to review the section at a glance.

     2.   DISCUSSION - Detailed text that expands on items

          summarized in the ABSTRACT.
                            28

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                                                            Section No.  1.4
                                                            Revision  No.  0
                                                            Date  May  1,  1975
                                                            Page 2 of  3
It«tUtlca) An
•f »>C> 1.4.11
                                                                        .V*
                                     29

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                                           Section No. 1.4
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page  3' of  3
     3.   REFERENCES - List of resource documents used in

          preparation of the discussion.  In addition, where

          applicable, a list of resource documents for

          recommended reading is shown under BIBLIOGRAPHY.

     The DISCUSSION subsection is designed to be relatively

brief.  In those cases where a topic would require con-

siderable detailed discussion, the reader is referred to the

APPENDIX.
                             SO

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Procurement
Quality Control
    -°«fc
Statistical
Analysis of Data
                                      SI

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                                              Section No.  1.4.1
                                              Revision No.  0
                                              Date May 1,  1975
                                              Page 1 of  5
 1.4.1  DOCUMENT CONTROL AND REVISIONS

 1.4.1.1  ABSTRACT

     A quality assurance program should include a system for

 documenting operating procedures and revisions in the pro-

 cedures.  The system used for this Handbook is described and

 is recommended.

 1.4.1.2  DISCUSSION

     A quality assurance program should include a system for

 updating formal documentation of operating procedures.  The

 suggested system is the one used in this Handbook and described

 herein.  This system uses a standardized indexing format and

 provides for convenient replacement of pages that may be

 changed within the technical procedure descriptions.

     The indexing format includes, at the top of each page,

 the following information:

                         Section No.

                         Revision No.

                         Date (of revision)

                         Page

A digital numbering system identifies sections within the

text.  The "Section No." at the top of each page identifies

major three-digit or two-digit sections, where applicable.

For example, Section 1.4.4 represents "Quality Planning" and
                             32

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                                              Section No.  1.4.1
                                              Revision No.  0
                                              Date May 1,  1975
                                              Page 2 of 5


 Section 1.4.5  represents  "Training."   "Revision  No."  repre-

 sents  the  most current version of the  section in question,

 where  the  first version is  represented as  "0."   "Date"

 represents the date  of the  latest revision.   "Page  No."

 includes not only  the number of  the specific page,  but also

 the  total  number of  pages in this section.  An example of

 the  page label for the first page of "Quality Planning" in

 Section 1.4.4  follows:

                     Section No.  1.4.4

                     Revision No. £

                     Date  May 1, 1975

                     Page 1  of 6

 For  each three-digit level, the  text begins on a  new page.

 This format groups the pages together  to allow convenient

 revision of the  section.  Each time a  new page is added or

 expanded within  a  section,  the number  of the preceding or

 original page  is included on the new page, and a  letter is

 added to it.   For example,  if Page 4 of 8 were revised and

 expanded to include  an extra paragraph, the overflow would

 appear  on  a page designated 4a.  The original Page  4 would

 then be removed  from the Handbook and  replaced by revised

 Page 4  and Page  4a.  This allows expansion within a section

without retyping the section or renumbering all of  the

pages.

     The Table of Contents follows the same structure as the

text.   It contains a space  for "Revision No." and "Pages"

-------
                                           Section No. 1.4.1
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 3 of 5
within each section heading.  When a revision to the text is
made, the Table of Contents page would be updated by re-
typing, or by striking out the old revision number and
printing the current revision number.  For example, the
Table of Contents page detailing Section 1.4 might appear as
follows:
                                   Pages  Revision  Date
1.4.1  Document Control and          5       0      5/1/75
        Revisions
1.4.2  Quality Assurance             5       0      5/1/75
        Policy and Objectives
1.4.3  Organization                  7       0      5/1/75
A revision to "Organization" would change the Table of Con-
tents to appear as follows:
                                   Pages  Revision  Date
1.4.1  Document Control and          5       0      5/1/75
        Revisions
1.4.2  Quality Assurance             5       0      5/1/75
        Policy and Objectives
1.4.3  Organization                  7       1      7/1/75
     A Handbook distribution record has been established and
will be maintained up to date so that future versions of
existing Handbook sections and the addition of new sections
may be distributed to Handbook users.  In order to enter the
user's name and address in the distribution record system,
the "Distribution Record Card" in the front of Volume I of
                            34

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                                           Revision No. 1.4.1
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 4 of 5
this Handbook must be filled out and mailed in the pre-

addressed envelope provided with this volume of the Handbook.

 (Note:  A separate card must be filled out for each volume

of the Handbook).  Any future change in name and/or address

should be sent to the following:

     U.S. Environmental Protection Agency
     Environmental Monitoring and Support Laboratory
     Quality Assurance Branch
     Research Triangle Park, N.C. 27711

     Attn:  Distribution Record System


     Changes may be made by the issuance of (1) an entirely

new document, (2) replacement pages or, (3) an errata sheet

or by pen and ink posting on the original document.  The

recipient of these changes should remove and destroy all

revised pages, sections, etc. from his copy and/or make pen

and ink corrections as noted.

     The document control system described herein applies to

this Handbook and it can be used, with minor revisions, to

maintain control of quality assurance procedures developed

by users of this Handbook and quality assurance coordina-

tors.  The most important elements of the quality assurance

program to which document control should be applied include:

          1.   Sampling procedures.

          2.   Calibration procedures.

          3.   Analytical procedures.
                           35

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                                           Section No. 1.4.1
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 5 of 5
          4.    Data collection and reporting procedures.

          5.    Auditing procedures.

          6.    Sample shipping and storage procedures.

          7.    Computational and data validation procedures.

          8.    Quality assurance manuals.

          9.    Quality assurance plans.

1.4.1.3  REFERENCE

1.   Industrial Hygiene Service Laboratory Quality Control
     Manual.   DHEW, PHS, National Institute of Occupational
     Safety and Health, Cincinnati, Ohio.  Technical Report
     No. 78,  1974.  Section VII.

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Statistical
Analysis of Data
Procurement
Quality Control
                                     37

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                                            Section No. 1.4.2
                                            Revision No. 0
                                            Date May 1, 1975
                                            Page 1 of 5
1.4.2  QUALITY ASSURANCE POLICY AND OBJECTIVES

1.4.2.1  ABSTRACT

     1.   Each organization should have a written quality

assurance policy that should be made known to all organization

personnel.

     2.   The objectives of quality assurance are to produce

data that meet users' requirements measured in terms of

completeness, precision, accuracy, representativeness and com-

parability and at the same time reduce quality costs.

1.4.2.2  DISCUSSION

     Quality assurance policy - Each organization should

have a written quality assurance policy.  This policy should

be distributed so that all organization personnel know the

policy and scope of coverage.

     Quality assurance objectives  '  - To administer a

quality assurance program, the objectives of the program

must be defined, documented, and issued to all activities

that affect the quality of the data.  Such written objectives

are needed because they:

     1.   Unify the thinking of those concerned with quality

assurance.

     2.   Stimulate effective action.

     3.   Are a necessary prerequisite to an integrated,

planned course of action.
                             58

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                                           Section No. 1.4.2
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 2 of 5
      4.    Permit  comparison of completed performances

 against  stated objectives.

 The  objectives of a quality assurance system as described in

 this Handbook are to produce data that are complete, pre-

 cise,  accurate, representative, and comparable.

      Data  can be  considered to be complete if a prescribed

 percentage of the total possible measurements is present.

 Precision  and accuracy represent measures of the data

 quality.   Data must be representative of the condition being

 measured.   Ambient air sampling at midnight is not representa-

 tive  of  carbon monoxide levels during rush hour traffic.  Sta-

 tionary  source emission measurements are not representative if

 measured at reduced load production conditions when normal oper-

 ation  is at full  load.   Data available from numerous agencies

 and private organizations should be in consistent units and

 should be  corrected to the same standard conditions of tempera-

 ture and pressure to allow comparability of data among groups.

     Figure 1.4.2.1 shows three examples of data quality

with varying degrees of precision and accuracy.   These

examples hypothesize a true value that would result if an

accurate measurement procedure were available and an in-

 finitely large number of measurements could be made under

specified conditions.   If the average value coincides with

the true value (reference standard), then the measurements

are accurate.   If the measurement values also are closely

clustered about the true value, the measurements are both

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                                                 Section No.  1.4.2
                                                 Revision No.  0
                                                 Date   Nay  J,  T>',"S
                                                 Page  3 of  5

                                                  Precision ( i)
                 True Value  of
                 Concentration
Measured
Average
                                 Bias •
    Example of Positive Biassed  (Inaccurate) but Precise
                             True Value
                         —       and
                          Measured Average

        Example  of Accurate  (No Bias)  but Imprecise Measurements
                                              Precision (r1
                             True Value
                          —      and
                           Measured Average
              Example of Precise and Accurate Measurement?
Downtime (D)
System
Operation



Diagnostic
and
Maintenance
*— Time '








Down                        Jailing Periods

    Example Indicating a Measure of Completeness of Data  U/(D *  u)
  Figure 1.4.2.1   Examples of data with varying degrees  of
                     precision,  accuracy,  and  completeness
                                40

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                                           Section No.  1.4.2
                                           Revision No. 0
                                           Date May 1,  1975
                                           Page 4 of 5
precise and accurate.  Figure 1.4.2.1 also shows an example

of completeness of data.

     Each laboratory should have quantitative objectives set

forth for each monitoring system in terms of completeness,

precision, and accuracy of data.  An example is included

below for continuous measurement of carbon monoxide (non-

dispersive infrared spectrometry) to illustrate the point.

     1.   Completeness - For continuous measurements,  75

percent or more of the total possible number of observations

must be present.  A summary of a minimum number of observa-

tions by time intervals (i.e., yearly, monthly, and hourly)

is shown in Figure 1.4.17.1 (Data Validation).

     2.   Precision - Determined with calibration gases,

precision is +0.5 percent full scale in the 0 through 58
    3       4
mg/m  range.

     3.   Accuracy - Depends on instrument linearity and the

absolute concentrations of the calibration gases.  An

accuracy of +1 percent t>f full scale in the 0 through 58
    3                       4
mg/m  range can be obtained.

     For further discussion of completeness, precision,

accuracy and comparability, see the following:

     1.   Completeness and comparability, Section 1.4.17.

     2.   Precision and accuracy, Appendix G.

     Employment of the elements of quality assurance dis-

cussed in Section 1.4. should lead to the production of data

that are complete, accurate, precise, and comparable.
                            41

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                                           Section No. 1.4.2
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 5 of 5
1.4.2.3  REFERENCES

1.   Juran, J.M., (ed.).  Quality Control Handbook.
     McGraw-Hill, New York, 1962.  Sec. 2, pp. 4-8.
2nd Ed.
2.   Feigenbaum, A.V.  Total Quality Control.  McGraw-Hill,
     New York, 1961.  pp. 20-21.
3.   Juran, J.M., and Gryna, F.M.  Quality Planning and
     Analysis.  McGraw-Hill, New York, 1970.  pp. 375-377.

4.   Nehls, G.J., and Akland, G.G.  Procedures for Handling
     Aerometric Data.  Journal of the Air Pollution Control
     Association, 2_3 (3) :180-184, March 1973.

5.   National Primary and Secondary Ambient Air Quality
     Standards.  Federal Register, 3£(B4): 8194-8195,
     April 30, 197IT(Note:  Copy available in Volume II of
     this Quality Assurance Handbook.)
                            42

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Statistical
Analysis of Data
Procurement
Quality Control
                                    43

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                                             Section No. 1.4.3
                                             Revision No. 0
                                             Date  May 1, 1975.
                                             Page 1 of 7
1.4.3  ORGANIZATION

1.4.3.1   ABSTRACT

     1.   Organizing a quality assurance function includes

establishing objectives, determining the amount of emphasis

to place on each quality assurance element, preparing a

quality assurance plan, identifying quality assurance problems

to be resolved, and implementing the quality assurance plan.

     2.   Quality assurance is normally a separate function

in the organization.

     3.   Quality assurance has input into many functions of

an air pollution control agency.   (See Figure 1.4.3.2 for

details.)

     4.   The basic tools for quality assurance implementation

are:

          a.   Organization chart

          b.   Job description.  (See Figure 1.4.3.3 for job

description for the Quality Assurance Coordinator.)

          c.   Quality assurance plan

1.4.3.2   DISCUSSION

     Organizing the quality assurance function  - Because of

the differences in size, workloads, expertise, and experience

in quality assurance activities among agencies adopting the

use of a quality assurance system, it is useful here to

outline the steps for planning an efficient quality assurance

system.
                            44

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                                             Section No. 1.4.3
                                             Revision No. 0
                                             Date May 1, 1975
                                             Page 2 of 1
      1.    Establish  quality assurance objectives  (precision,

 accuracy,  and  completeness) for each measurement  system

 (Section 1.4.2).

      2.    Determine  the quality assurance elements appro-

 priate  for the agency  (Figure  1.4.).

      3.    Prepare a  quality assurance plan  (normally on a

 project basis)  for all measurement systems  (Section 1.4.23).

      4.    On the basis of the  quality assurance plan, iden-

 tify  quality assurance problems which must be resolved.

      5.    Implement  the quality assurance plan.

      Location  of the quality assurance function in the

 organization   - If practical,  one individual within an

 organization should  be designated the Quality Assurance (QA)

 Coordinator.   The QA Coordinator should undertake activities

 such  as quality planning, auditing, and reliability.  The QA

 Coordinator should also have the responsibility for coor-

 dinating all quality assurance activity so that complete

 integration of the quality assurance system is achieved.

 The QA Coordinator should, therefore, gain the cooperation

 of other responsible heads of  the organization with regard

 to quality assurance matters.

     As a general rule, it is not good practice for the

quality assurance function to be directly located in the

organization responsible for conducting measurement pro-

grams.  This arrangement could be workable, however, if the

person in charge maintains an objective viewpoint.
                            45

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                                           Section No. 1.4.3
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 3 of 7
     Relationship of the quality assurance function to

other functions - The functions performed by a comprehensive

air pollution control program at the state or local level

are shown in Figure 1.4.3.1.   The relationship of the

quality assurance function to the other agency functions is

shown in Figure 1.4.3.2.  The role of quality assurance can

be grouped into two categories:

     1.   Recommend quality assurance policy and assist its

formulation with regard to agency policy, administrative

support (contracts and procurements), and staff training.

     2.   Provide quality assurance guidance and assistance

for monitoring networks, laboratory operations, data reduc-

tion, instrument maintenance and calibration, litigation,

source testing, and promulgation of control regulations.

     Basic tools for quality assurance implementation are;
                                4
     1.   The organization chart  - The quality assurance

organization chart should display line and staff relation-

ships, and lines of authority and responsibility.  The lines

of authority and responsibility, flowing from the top to

bottom, are usually solid, while staff advisory relation-

ships are depicted by dashed lines.

     2.   The job description  - The job description lists

the responsibilities, duties, and authorities of the job and

relationships to other positions, individuals, or groups.  A

sample job description for a Quality Assurance Coordinator

is shown in Figure 1.4.3.3.
                             46

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                                              Section No. 1.4.3
                                              Revision No. 0
                                              Date  May 1, 1975
                                              Page  4 of  7
Management Services
        Agency policy
        Administrative and clerical support
        Public information and community relations
        Intergovernmental relations
        Legal counsel
        Systems analysis, development of strategies,
          long-range planning
        Staff training and development

Technical Services

        Laboratory operations
        Operation of monitoring network
        Data reduction
        Special field studies
        Instrument maintenance and calibration

Field Enforcement Services

        Scheduled inspections
        Complaint handling
        Operation of field patrol
        Preparation for legal actions
        Enforcement of emergency episode procedures
        Source identification and registration

Engineering Services

        Calculation of emission estimates
        Operation of permit system
        Source emission testing
        Technical development of control regulations
        Preparation of technical reports, guides, and
          criteria on control
        Design and review of industrial emergency episode
          procedure:
     Figure 1.4.3.1  List of functions performed by comprehensive
                     air pollution control programs
                              47

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                                                         Section No.  1.4.3
                                                         Revision  No.  0
                                                         Date   May 1,  1975
                                                         Page  5 of 7
             Manaqem3nt  Services
    n
    m
    a
    •O
    c
    a
    u
    a
    •o
    •H

    t7>

    §
                     Quality assurance
                     Agency
                     Administrative and clerical support:
                                            contracts ^
                                            procurement •
        Public information and  community relations
        Intergovernmental relations -^
        Legal counsel
        Systems analysis, development of strategies,
          long-range planning
        Staff trainmg and development .^
             Technical  Services
                                                               •o »
                                                               o n>
                                                               (-• o
                                                                              (3
                                                                             Mi D
                                                                             O O.
C 3
>-• &
Cu
n- B)
H- IB
O 0)
3 H-
  01
  rr
        Laboratory operations
        Operation of monitoring  network
        Data  reduction
        Special field studies
        Instrument maintenance and calibration
Field Enforcement Services
        Scheduled inspections
        Complaint handling
        Operation of field patrol
        Preparation of legal actions
        Enforcement of emergency episode procedures
        Source  identification and  registration
             Engineering Services
                     Calculation of emission estimates
                     Operation  of permit system
                     Source emission testing
                     Technical  development of control regulations
                     Preparation of technical reports, guides, and
                       criteria on control
                     Design and review of industrial emergency episode procedures
Figure  1.4.3.2
       Relationship of the quality  assurance function
       to  other air pollution  control  program  functions
                                       48

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                                             Section No.  1.4.3
                                             Revision No.  0
                                             Date  May  1,  1975
                                             Page  6 of  7
TITLE:  Quality Assurance Coordinator

Basic Function

     The Quality Assurance Coordinator is responsible for the
conduct of the quality assurance program and for taking or
recommending measures.

Responsibilities and Authority

1.   Develops and carries out quality control programs, including
     statistical procedures and techniques, which will help
     agencies meet authorized quality standards at minimum
     cost.

2.   Monitors quality assurance activities of the agency to
     determine conformance with policy and procedures and
     with sound practice; and makes appropriate recommendations
     for correction and improvement as may be necessary.

3.   Seeks out and evaluates new ideas and current developments
     in the field of quality assurance and recommends means
     for their application wherever advisable.

4.   Advises management in reviewing technology, methods, and
     equipment, with respect to quality assurance aspects.

5.   Coordinates schedules for measurement system functional check
     calibrations, and other checking procedures.

6.   Evaluates data quality and maintains records on related
     quality control charts, calibration records, and other
     pertinent information.

7.   Coordinates and/or conducts quality-problem investigations.
     Figure 1.4.3.3  Job description for the Quality Assurance
                     Coordinator
                             49

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                                            Section  No.  1.4.3
                                            Revision No.  0
                                            Date May 1,  1975
                                            Page 1 of  1
     3.   The quality assurance plan - To implement quality

assurance in a logical manner and identify problem areas,

quality assurance plans are needed.  These are normally

prepared on a project basis.  For details on preparation of

quality assurance plans, see Section 1.4.23.

1.4.3.3   REFERENCES

1.   Feigenbaum, A.V.  Total Quality Control.  McGraw-Hill,
     New York.  1961.  Chapter 4, pp. 43-82.

2.   Covino, C.P., and Meghri, A.W.  Quality Assurance
     Manual. Industrial Press, Inc., New York.  1967.
     Step 1, pp. 1-2.

3.   Walsh, G.W., and von Lehmden, D.J.  Estimating Manpower
     Needs of Air Pollution Control Agencies.  Presented at
     the Annual Meeting of the Air Pollution Control Asso-
     ciation, Paper 70-92, June 1970.

4.   Juran, J.M., (ed.).  Quality Control Handbook, 2nd
     Edition. McGraw-Hill, New York.  19627Section 6,
     pp. 242.

5.   Industrial Hygiene Service Laboratory Quality Control
     Manual.  Technical Report No. 78, National Institute
     for Occupational Safety and Health, Cincinnati, Ohio.
     1974.

     BIBLIOGRAPHY
1.   Brown, F.R.  Management;  Concepts and Practice.
     Industrial College of the Armed Forces, Washington,
     D.C.  1967.  Chapter II, pp. 13-34.
                            50

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                        »^<2
                        2. »> V
Statistical

Analysis of Data
Procurement

Quality Control
                                  51

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                                           Section No. 1.4.5
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 1 of 8
1.4.5  TRAINING
1.4.5.1   ABSTRACT
     All personnel involved in any function affecting data
quality  (sample collection, analysis, data reduction, and
quality assurance) should have sufficient training in their
appointed jobs to contribute to the reporting of complete
and high quality data.
     TM training methods commonly used in the air pollution
control field are the following:
     1.   On-the-job training  (OJT).
     2.   Short-term course training  (normally 2 weeks or
less).
     3.   Long-term course training (quarter or semester in
length).
     A list of recommended short-term course training is
shown in Figure 1.4.5.1.
     Training should be e\ aluated in terms of the trainee
and the training per se.  The following are techniques
commonly used in the air pollution control field to evaluate
•training.
     1.   Testing (pre-training and post-training tests).
     2.   Proficiency checks.
     3.   Interviews (written or oral with the trainee's
supervisor and/or trainee).
                            52

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                                            Section  No.    4.5
                                            Revision No.  J
                                            Date May 1, 1975
                                            Page 2 of 8
1.4.5.2   DISCUSSION
     All personnel involved in any function affecting data
quality  (sample collection, analysis, data reduction, and
quality assurance) should have sufficient training in their
appointed jobs to contribute to the reporting of complete
and high quality data.  The Quality Assurance Coordinator
should be concerned that the required training is available
for these personnel and, when it is not, should recommend to
management that appropriate training be made available.
                       1 2
     Training .objective '  - The training objective should
be to develop personnel to the necessary level of knowledge
and skill required for air pollution measurement systems
(ambient air and source emissions).
     Training methods and availability - Several methods of
training are available to promote achievement of the desired
level of knowledge and skill required.  The following are
the training methods most commonly used in the air pollution
control field; a listing of available training courses for
1975-1976 is given in Figure 1.4.5.1.
     1.   On-the-job training (OJT) - An effective OJT
program could consist of the following:
          a.   Observe experienced operator perform the
different tasks in the measurement process.
          b.   Study the operational portion of the method
as described in the pollutant-specific portion of this
Handbook, and use it as a guide for performing the operations.
                            53

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                                           Section No.  1.4.5
                                           Revision No.  0
                                           Date May 1,  1975
                                           Page 5 of  8
          c.   Perform operation under the direct super-

vision of an experienced operator.

          d.   Perform operations independently but with a

high level of quality assurance checks, utilizing the evalua-

tion technique described later in this section to encourage

high quality work.

     2.   Short-term course training - A number of short-

term courses (normally 2 weeks or less) are available that

provide knowledge and skills to implement more effectively

an air pollution measurement system.  Some of the courses

are on the measurement methods per se_ and others provide

training useful in the design and operation of the total or

selected portions of the measurement system.

     3.   Long-term course training - Numerous universities,

colleges, and technical schools provide long-term (quarter

and semester length) academic courses in statistics, analy-

tical chemistry, and other disciplines.  The agency's train-

ing or personnel officer should be contacted for information

on the availability of long-term course training.

     Training evaluation - Training should be evaluated in

terms of (1) level of knowledge and skill achieved by the

operator from the training; and (2) the overall effective-

ness of the training, including determination of training

areas that need improvement. If a quantitative performance

rating can be made on the operator during the training
                           54

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                                           Section No. 1.4.5
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 6 of 8
period  (in terms of knowledge and skill achieved),  this

rating may also provide an assessment of the overall effective-

ness of the training as well.

     Several techniques are available for evaluating the

operator and the training per se.  One or more of these

techniques should be used during the evaluation.  The most

common types of evaluation techniques applicable to training

in air pollution measurement systems are the following:

     1.   Testing - A written test before (pretest) and one

after  (post-test) training are commonly user] in short-term

course training.  This allows the trainee to see areas of

personal improvement and provides the instructor with infor-

mation on training areas that need improvement.

     2.   Proficiency checks - A good means of measuring

skill improvement in both OJT and short-term course training

is to assign the trainee a work task.  Accuracy and/or

completeness are commonly the indicators used to score the

trainee's proficiency.  The work tasks could be of the

following form:

          a.   Sample collection - Trainee would be asked to

list all steps involved in sample collection for a hypothe-

tical case.  In addition, the trainee could be asked to

perform selected calculations.  Proficiency could be judged

in terms of completeness and accuracy.
                            55

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                                           Section No. 1.4.5
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 7 of 8
          b.   Analysis - Trainee could be provided unknown

samples for analysis.  As defined here, an unknown is a

sample whose concentration is known to the work supsr^isor

 (OJT) or training instructor  (short-term course training)

but unknown to the trainee.  Proficiency could be judged in

terms of accuracy.

          c.   Data reduction - Trainees responsible for

data reduction could be provided data sets to validate.

Proficiency could be judged in terms of completeness and

accuracy.

     If proficiency checks are planned on a recurring basis,

a quality control or other type chart may be used to show

progress during the training period as well as after the

training has been completed.  Recurring proficiency checks

are a useful technique for determining if additional train-

ing may be required.

     3.   Interviews - In some cases, a written or oral

interview with the trainee's supervisor and/or trainee is

used to determine if the training was effective.  This

interview is normally not conducted until the trainee has

returned to the job and has had an opportunity to use the

training.  This technique is most often used to appraise the

effectiveness of a training program  (OJT or short-term

course) rather than the performance of the trainee.
                            56

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                                           Section No.  1.4.5
                                           Revision No.  0
                                           Date May 1,  1975
                                           Page 8  of 8
1.4.5.3   REFERENCES
1.   Feigenbaum, A.V.  Total Quality Control.  McGraw-Hill,
     New York.  1961.  pp. 605-615.

2.   Feigenbaum, A.V.  Company Education in the Quality
     Problem.  Industrial Quality Control, X(6):24-29, May
     1974.                                 ~

     BIBLIOGRAPHY

1.   Juran, J.M., (ed.).  Quality Control Handbook.  2nd
     edition. , McGraw-Hill, New York, 19671Section 7, pp.
     13-20.

2.   Reynolds, E.A.   Industrial Training of Quality Engi-
     neers and Supervisors.  Industrial Quality Control,
     X(6):29-32, May 1954.

3.   Industrial Quality Control, 23_(12) , June 1967.  (All
     articles deal with education and training.)

4.   Seder, L.A.  QC Training for Non-Quality Personnel.
     Quality Progress, VII(7);9.

5.   Reynolds, E.A.   Training QC Engineers and Managers.
     Quality Progress, III(4):20-21, April 1970.
                            57

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                *
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                                             Section No. 1.4.16
                                             Revision No. 0
                                             Date May 1, 1975
                                             Page 1 of 4
1.4.16  AUDIT PROCEDURES

1.4.16.1  ABSTRACT

     1.   Performance audits are independent checks made by

the supervisor or auditor to evaluate the quality of data

produced by the total measurement system (sample collection,

sample analysis and data processing).  Performance audits

are normally a quantitative appraisal of quality.

     2.   A system audit is an on-site inspection and review

of the quality assurance system used for the total measurement

system (sample collection, sample analysis, data processing,

etc.).  Quality assurance plans discussed in Section 1.4.23

should be used as the basis for conducting a system audit.

System audits are normally a qualitative appraisal of quality.

1.4.16.2  DISCUSSION

     Performance audit - Performance audits refer to indepen-

dent checks made by the supervisor or auditor to evaluate

the quality of data produced by the total sampling and

analysis system.  Performance audits generally are categorized

as follows:

     1.   Sampling audits.

     2.   Analysis audits.

     3.   Data processing audits.

These audits are performed independent of and in addition to

normal quality control checks by the operator/analyst.

Independence can be achieved by having the audit made by  a
                             60

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                                    Section  No.  1.4.16
                                    Revision No.  0
                                    Date  May 1,  1975
                                    Page  2 of 4
different operator/analyst from the one conducting the

routine measurements or, in the case of sampling or analysis,

by the introduction of audit control standards into the

sampling or analysis system and the subsequent plotting of

results on control charts by the supervisor.  The use of

audit control standards should be applied without the

knowledge of the operator/analyst, if possible, to insure

that recorded results reflect normal operating conditions.

     Performance audits made by a different operator/analyst

from the one conducting the routine measurement may be

conducted in several ways.  The following are examples of

the most common type of audits.

     1.   Sampling audit - The auditor uses a separate set

of calibrated flowmeters and reference standards to check

the sample collection system:

          a.   Flow rate devices.

          b.   Instrument calibration.

          c.   Instrument calibration gases, when applicable.

     2.   Analysis audits - The auditor is commonly provided

a portion or aliquot of several routine samples for analysis.

     3.   Data processing audits - Data reporting commonly

involves a spot-check on calculations and data validation

may be checked by inserting in the data processing system a

dummy set of raw data followed by review of these validated

data.
                           61

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                                           Section 1.4.16
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 3 of 4
     A major problem in audit design is determining the
auditing frequency and the lot size (number of samples
required to estimate population concentration with a spec-
ified percentage confidence).
     After the auditing schedule has been implemented, the
audit results should be plotted on control charts to give
the supervisor a visual picture of changes in the perform-
ance so that corrective actions may be taken when necessary.
A discussion of recommended control chart types, instruc-
tions on construction, and criteria for interpretation are
included in Appendix H, "Control Charts."
     System audit - A system audit is an on-site inspection
and review of the quality assurance system used for the
total measurement system  (sample collection, sample anal-
ysis, data processing, etc.) for each monitoring sensor.
Whereas performance audits are a quantitative appraisal,
system audits are normally a qualitative appraisal.
     The quality assurance plans for projects and programs
discussed in Section 1.4.23 should be used as the basis for
conducting a system audit.  For convenience, some of the
items recommended for a QA plan are repeated here:
     1.   Organization and responsibility - Is the quality
assurance organization operational?
     2.   Sample collection - Are written sample-collection
procedures available and are these followed as written?
                           62

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                                           Section No. 1.4.16
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 4 of 4


      3.   Sample analysis - Are written analysis procedures

available and are these followed as written?

      4.   Data validation - Is a list of criteria for data

validation available and is it used?

      5.   Calibration - Are written calibration procedures

available and are these followed as written?  In addition, a

review should be made of procedures used to establish

traceability of calibration standards to standards of higher

accuracy and of the calibration schedule and data by mea-

surement sensor.

      6.   Audits - Are control charts for performance audits

reviewed?

      7.   Interlaboratory tests - Are results from inter-

laboratory testing reviewed?

      8.   Preventive maintenance - Is the preventive main-

tenance schedule being followed as recommended in the QA

plan?

     Other items for consideration in a system audit are

shown in Section 2.0 of Volume II, Ambient-Air Specific Methods

and Section 3.0 of Volume III, Stationary-Source Specific

Methods.

     A system audit may be made at any time during the life

of a project but is normally conducted before or just after

monitoring has been initiated.

-------

-------
Procurement
Quality Control
Statistical
Analysis of Data""^
 pa*a
       X?
    ^         *

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                                           Section No.  1.4.21
                                           Revision No.  0
                                           Date May 1,  1975
                                           Page 1 of 5
1.4.21  QUALITY REPORTS TO MANAGEMENT

1.4.21.1  ABSTRACT

     Quality facts to be reported should be defined and

methods for summarizing and reporting data should be deter-

mined.

     Quality facts usually reported are:

     1.   Percentage duplication or replication of deter-

minations.

     2.   Instrument or equipment downtime.

     3.   Percentage voided samples versus total samples.

     4.   Quality cost in terms of prevention, appraisal,

and correction costs.

     5.   System audit (on-site inspection) results.

     6.   Performance audit results.

     7.   Interlaboratory test results and, where appro-

priate, intralaboratory test results (precision and accu-

racy) .

     8.   Status of solutions to major quality assurance

problems.

     The Quality Assurance Coordinator should consult with

line staff to determine the necessary reporting require-

ments.  Reports should be obtained from source documents.

Reports should have a baseline for comparison and should be

easy to interpret.  Similar reports should be combined if

possible.
                            66

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                                           Section No. 1.4.21
                                           Revision No. 0
                                           Date Hay 1, 1975
                                           Page 2 of 5
 1.4.21.2  DISCUSSION
     Quality  assurance  facts to be reported may vary widely

 from one  air  pollution  control agency to another, depending

 on size and organization of the agencies.  The quality

 reports listed  in the abstract represent the kinds of in-

 formation commonly needed by management.

     The  details or  sources of such facts are obtained from

 other  sections  of the Handbook as follows:

          Facts
1.  Percentage of duplication or repli-
    cation of determinations.

2.  Instrument or equipment downtime.

3.  Percentage of voided samples versus
    total samples.

4.  Quality costs  (prevention, appraisal,
    and correction costs).

5.  System audit  (on-site inspection)
    results.

6.  Performance audit results.

7.  Interlaboratory test results and,
    where appropriate, intralaboratory
    tests results  (precision and
    accuracy).

8.  Status of solutions to major quality
    problems.
Source

Methods (Vols. 2 and 3)


1.4.20  (Vol. 1)

Methods (Vols. 2 and 3)
1.4.17  (Vol. 1)

1.4.14  (Vol. 1)


1.4.16  (Vol. 1)


1.4.16  (Vol. 1)

1.4.15  (Vol. 1)
1.4.13  (Vol. 1)
     Principles of reporting to management - The following

are general principles that should be considered:

     1.   In order to determine what periodic reports are

needed or desired by management, the Quality Assurance
                               67

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                                           Section No. 1.4.21
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 3 of 5
Coordinator should discuss with superiors and staff members
what reports need to be published on a regular basis to
provide information required for rational decision-making.
     2.   In order to minimize errors in transmission,
translation, and interpretation, facts used in reports to
management should be obtained from source documents when
possible.
     3.   Facts should be presented in summary form.  When
not presented graphically, the report should provide ab-
stracts of essential points.
     4.   Reports should compare current data with some
base.  The basic standard of comparison can be:
          a.   Based on previous performance  (historic).
          b.   Based on engineering judgment.
     5.   The report should be understood at a glance.  If
the report is not presented graphically, essential points
should be reduced to a single page, preferably double-
spaced.  An example of a graphic report is shown in Figure
1.4.21.1.  Figure 1.4.14.1 for quality costs  (in terms of
prevention, appraisal, and corrective costs) is anothei
example of graphic presentation.
     Where applicable, quality control charts should be used
to report results from performance audits, intralaboratory
tests and, when performed on a recurring basis, interlabora-
tory test results.
                            68

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                                   Section No. 1.4.21
                                   Revision No.  0
                                   Date   May 1,  1975
                                   Page  4 of 5
tf3a\/
                                            c
                                            OJ

                                            0)
                                            en
                                            10
                                            c
                                            10


                                            o
                                            4J
                                            0
                                            a
                                            a
                                            (0
                                            >-i
                                            o
                                           01
                                           M
                                           3
    Q3QIOA
             69

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                                           Section No. 1.4.21
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 5 of 5
1.4.21.3

1.
     REFERENCES
2.
Juran, J.M.,  (ed.).  Quality Control Handbook.  2nd ed.
McGraw-Hill, New York.  1962.  Sec. 12, pp. 26-32.

BIBLIOGRAPHY

Juran, J.M., and Gryna, F.M.  Quality Planning and
Analysis.  McGraw-Hill, New York.  1970.

Spear, M.E.  Charting Statistics.  McGraw-Hill, New
York.  1952.
                             70

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Procurement
Quality Control
   £3?-*.
Statistical
Analysis of Data
 t)»ta
                              71

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                                             Section No. 1.4.22
                                             Revision No. 0
                                             Date May 1, 1975
                                             Page 1 of 2
1.4.22  QUALITY ASSURANCE MANUAL

1.4.22.1  ABSTRACT

     1.   A quality assurance manual is a manual of general

requirements needed to assure quality.  Specific require-

ments for each project are contained in a quality assurance

plan.

     2.   Each state and local air pollution control agency

and others involved in air program research and monitoring

activities need a quality assurance manual.  These organiza-

tions should use the "Elements of Quality Assurance" de-

scribed in Section 1.4 of this Handbook as a guide in

developing their own manuals.

1.4.22.2  DISCUSSION

     Quality assurance manual content - A common practice foi

quality assurance in industry is for each company concerned

with the design, development, and manufacturing of a product

to prepare a quality assurance manual.  This manual states

the company's general philosophy and requirements with

respect to quality assurance by functional activities that

are associated with the quality of the product.  The spe-

cific requirements for each product  (or group of products)

are contained in a quality assurance plan.

     State and local air pollution control agencies and

others need a quality assurance manual - Each state and

local air pollution control agency and others involved in
                             72

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                                           Section  No.  1.4.22
                                           Revision No.  0
                                           Date  May 1,  1972
                                           Page  2 of 2

air program research and monitoring activities need a

quality assurance manual.  The manual should define manage-

ment's position on quality assurance and provide guidelines

that should be followed by subordinates in preparing quality

assurance plans.  These organizations should use the "Ele-

ments of Quality Assurance" described in Section 1.4 of this

Handbook as a guide in developing their own manual.
                            78

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Procurement
Quality Control
Statistical
Analysis of Data"~~i
                                    75

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                                           Section No. 1.4.23
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 1 of 7
1.4.23  QUALITY ASSURANCE PLANS FOR PROJECTS AND PROGRAMS

1.4.23.1  ABSTRACT

     1.   A quality assurance plan (QA plan) is specific

quality assurance requirements prepared for a project or

program for the elements discussed in Section 1.4 of this

Handbook.

     2.   QA plans should be prepared for both inhouse and

contract projects.

     3.   The depth of a QA plan is influenced primarily by:

          a.   Intended use of the data.

          b.   Whether the project is new or on-going.

     4.   An example format for a QA plan is given.

1.4.23.2  DISCUSSION

     Definition of quality assurance plan (QA plan) - The

specific requirements prepared by or for a project officer

(single project) or a program manager*  (group of similar

projects) to ensure quality data from each air measurement

system are called a QA plan.

     Quality assurance plans for inhouse and contract

projects - A QA plan should be prepared and implemented to

include each air pollution measurement system in an inhouse

or contract project.  The plan should be prepared by the

project officer for inhouse projects and for the project

officer's review and approval for contracts.  The Quality
* For simplicity the terms project officer and project will
  be used throughout the discussion.
                            76

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                                           Section No. 1.4.23
                                           R°vision No. 0
                                           Late May 1, 1975
                                           Page 2 of 7


Assurance Coordinator should be involved in the review of

the QA plan prior to implementation.  The plan should be

based on project objectives and should be consistent with

management's general requirements on quality assurance that

are specified in the quality assurance manual  (see Section

1.4.22).

     Quality assurance elements in a QA plan - All quality

assurance elements discussed in Section 1.4 should be con-

sidered in the preparation of the QA plan.  However, dif-

ferent projects will require emphasis on different elements.

Factors that will have the most influence on the QA plan

design are:

     1.   Intended use of the data - Monitoring for enforce-

ment or the establishment of air pollution criteria levels

(normally for health effects) will result in closer scrutiny

of the project from a quality assurance standpoint than

projects in which legal actions may not be involved; e.g.,

research on the development of a new monitoring instrument.

     2.   New project versus improvement in an on-going

project - Improving quality assurance on a current project

normally means that the operators are on the job and the air

measurement equipment is in operation.  For on-going pro-

jects, the quality assurance elements that are particularly

beneficial to consider in the QA plan are:

          a.   Organization (Section 1.4.3); namely, the

project quality organization and responsibility.
                          77

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                                           Section No. 1.4.23
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 3 of 7
          b.   Sample collection (Section 1.4.8), includes

sampling handling and storage requirements.  Include a copy

of all procedures, or if standard procedures are used, a

reference to these will suffice.

          c.   Sample analysis  (Section 1.4.9).  Include a

copy of all procedures, or if standard procedures are used,

a reference to these will suffice.

          d.   Data reporting (Section 1.4.10).

          e.   Data validation  (Section 1.4.17), including

specific criteria that are to be applied for validation of

data.

          f.   Audit procedures  (Section 1.4.16) including

specific performance audits that are to be performed during

routine project operations.

          g.   Calibration (Section 1.4.12), including

description of procedure for establishing traceability,

description of calibration standards, and a schedule for

calibration.  Include a copy of all calibration procedures,

or if standard procedures are used, a reference to these

will suffice.

          h.   Preventive maintenance  (Section 1.4.7),

including a schedule for maintenance.

          i.   Interlaboratory  tests  (Section 1.4.15),

including a list of any planned or anticipated participation

in interlaboratory tests.
                            78

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                                           Section No. 1.4.23
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 4 of 7
          j.   Quality reports to management  (Section

1.4.21), including the information content of the reports

and the frequency of reporting.

     Project officers or managers for new projects will need

to consider all elements mentioned previously for on-going

projects and, in addition, should probably pay special

attention also to the following areas:

          a.   Pretest preparation (Section 1.4.6).  For new

monitoring projects, a preliminary visit to select sampling

sites for ambient air monitoring and source emission moni-

toring will normally be required.  Criteria or factors used

to select the sample collection sites should be listed.

          b.   Training  (Section 1.4.5).  Commonly, new

projects may result in the hiring of new personnel or the

assignment of current personnel to different work tasks for

which training may be required.  Anticipated training should

be listed.

          c.   Procurement quality control (Section 1.4.11).

A new project may mean procurement of new equipment and

reagents.  Equipment and reagents that should be placed

under procurement quality control should be listed and, if

available, acceptance limits should also be included.

          d.   Reliability (Section 1.4.20).  When equipment

reliability is important, the equipment should be listed and

reliability limits provided.
                             79

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                                           Section No. 1.4.23
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 5 of 7
          e.   Configuration control (Section 1.4.19).  Any

plans for configuration control on large projects should be

summarized.

     Quality assurance plan document control and distribu-

tion - The preparation of a QA plan requires that the

project officer consider all quality assurance elements

listed previously and plan for those elements that will have

the most quality impact in the project.  The result of this

planning is the QA plan per se.  The QA plan represents the

project officer's best judgment on the quality assurance

level required for the project.  Therefore, the QA plan

should be readily available to all project personnel with

distribution copies made available to those personnel most

affected by the plan.  The plan should be in a document

control format in order to maintain a historical record of

major revisions in the project quality assurance program.

     Quality assurance plan format - The format used for the

QA plan will vary from project officer to project officer.

The following format is suggested, primarily to highlight

points for consideration by the project officer in preparing

the plan.

     1.   Table of Contents.  Show in document control and

revision format similar to the Handbook table of contents.

     2.   Project Description.  Give a brief project descrip-

tion including references to be consulted for more details.

     3.   Organization and Responsibility.  Give a table or
                            80

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                                           Section No. 1.4.23
                                           Revision No. 0
                                           Date May 1, 1975
                                           Page 6 of 7
chart  showing key individuals or groups involved in the
project quality assurance activities.
     4.   Project Quality Assurance Program.  The following
is a minimum that should be contained in QA plans in regard
to the elements of quality assurance:
          a.   Pretest preparation.  Include criteria or
factors used to select sample collection sites.  For ambient
air monitoring, a map of the site with the location of air
pollution and meteorological sensors should be included; and
for source emission monitoring, a flow diagram of the
process to be tested and a diagram  (with dimensions) of the
stack  or duct to be tested, plus pretest engineering data on
stack  velocity, stack temperature, etc.
          b.   Sample collection.  Include a copy of each
sensor sample collection procedure.  For manual sample
collection, include a procedure for sample handling and      <
storage requirements.  If standard procedures are used,
reference to these procedures will suffice (e.g., EPA Method
5 - Stationary Source Emission Monitoring for Particulates).
          c.   Sample analysis.  Include a copy of all
analytical procedures.  If standard procedures are used,
reference to these procedures will suffice.
          d.   Data reporting.  Include a copy of all forms
for reporting data and an example calculation for each
pollutant measurement.
          e.   Data validation.  Include a list of criteria
that should be used to validate data.
                            81

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                                           Section No. 1.4.23
                                           Revision No.  0
                                           Date May 1, 1975
                                           Page 7 of 7

          f.   Calibration.  Include a copy of all calibra-

tion procedures.  If standard procedures are used, reference

to these procedures will suffice.  By sensor, provide:    (1)

a schedule for calibration; (2) description of type of

standard; and  (3) procedure planned to establish trace-

ability of calibration standards to available standards of

higher quality.

          g.   Audits.  Include a plan for performance and

system (on-site inspection) auditing.  For performance

audits, recommend a frequency for an initial audit by

sensor.

          h.   Interlaboratory tests.  Any planned or antic-

ipated participation in interlaboratory tests should be

listed.

          i.   Preventive maintenance.  Include a copy of

preventive maintenance procedures for sensor and auxiliary

equipment.  Where vendor preventive maintenance procedures

are available, reference to these will suffice.  A pre-

ventive maintenance schedule should be recommended.

          j.   Other.  Any other quality assurance elements,

e.g., procurement quality control, configuration control,

training, etc., that are applicable to the project should

also be included.

     5.   Forms.  Any forms that are not included in part  4a

through 4g should be included.

     6.   Distribution list.  A complete list of all organiza-

tions and persons to whom the QA plan has been distributed

should be included.
                              82

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         You have completed your reading for Assignment 2. Do
         the review exercises which follow and check your answers
         after you complete them. The correct answers are given
         on the page following the review exercises.
       Reading Assignment 2 Review Exercises
Quality control is:
a. a system of management equivalent to a quality assurance system.
b. a system of data management used to ensure correct reporting of test
   results.
c. the system of statistical procedures used to ensure data quality.
d. the system of activities used to provide a quality product or result.
Quality assurance is:
a. the system of activities used to provide assurance that the quality control
   system is performing adequately.
b. the system of activities used to statistically determine confidence levels for
   air quality data.
c. the system of activities used to provide a quality product.
d. the system of activities used to provide assurance that air quality is
   improving.
The quality assurance wheel illustrates:
a. the elements that should be considered when planning a quality assurance
   program.
b. the costs associated with quality assurance programs.
c. mandatory requirements for any quality assurance program.
d. the management structure of the EPA Quality Assurance Division.
The objectives of a quality assurance program should be to produce data
that are:
a.   	
b.   	
c.   	
d.   	
e.   	
                                  83

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 5. The data illustrated below are:
                                        True value

    a.  both precise and accurate.
    b.  precise but not accurate.
    c.  both imprecise and inaccurate.
    d.  accurate but not precise.
 6. The quality assurance coordinator of a source testing organization should:
    a.  be the newest employee on the sampling team.
    b.  be a test team leader.
    c.  be independent from other organizational programs.
    d.  report to the laboratory supervisor.
 7. List the three most common training methods used in the field of air pollution
    control.
    a.
    b.
    c.
 8. List at least three techniques that can be used to check the effectiveness of a
    training program.
    a.   	
    b.   	
    c.
 9. An auditing procedure is one of the elements of a QA program that should be
    implemented as soon as possible. What are two types of audits that could be
    set up in a source sampling QA program?
    a.
    b.
10. What is the difference between a performance audit and a system audit?
    a. A performance audit is qualitative, whereas a system audit is quantitative.
    b. A performance audit is quantitative, whereas a system audit is qualitative.
                                      84

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11.  Which one of the following statements would not be true of a performance
    audit?
    a.  An aliquot of an unknown standard is submitted for lab analysis.
    b.  The source tester is required to solve a sample problem  on his nomograph
       before testing.
    c.  The sample-collection procedures are checked off as the test is done.
    d.  The dry-gas meter of the Method 5 train is checked using an EPA audit
       device.
12.  Which one of the following statements would not be included in a QA report
    to management?
    a.  Aliquots of the recovered Method 6 sample sent to ACME labs agreed with
       2% of those determined by the test contractor.
    b.  Laboratory analysis indicated a 30% disagreement with the EPA NO, audit
       sample stated value.
    c.  Inaccuracies in determining AH values from a nomograph were avoided in
       Tests 2 and 3 by using a calculator.
    d.  The nozzle was attached to the probe and then connected to the sample
       case in the normal manner.
IS.  What is the difference between a  quality assurance plan and  a quality
    assurance manual?
                                     85

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                         Answers to
         Reading Assignment 2 Review Exercises
1.
2.
5.
4.




5.
6.
7.


8.


9.

10.
11.
12.
a
©
GD
a.
b.
c.
d.
e.
a
a
a.
b.
c.
a.
b.
c.
a.
b
a (
a
a
b c (a;
bed
bed
complete
precise
accurate
representative
comparable
b 0 d
b©d
on-the-job
short-term
long-term
written tests
proficiency checks
interviews
performance audit
system audit
5)
b ©d
b c (d)
IS.  A quality assurance manual is general and covers the QA programs and
    methods used by an organization, whereas a quality assurance plan is method
    specific.
                                86

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                         Lesson  B
                  Volume III  Overview
Lesson Goal

The goal of this lesson is (a) to show you how to use Volume III and (b) to review
for you some aspects of source sampling before proceeding with the specific QA
procedures developed for each method.

Lesson Objectives

After completing this lesson, you should be able to:
    1.  describe how Volume III of the QA Manual is organized with respect to
      reference methods and topics.
    2.  explain how you can develop other manuals from Volume III.
    3.  define the responsibilities of the source tester.
    4.  list at least four activities involved in planning a source test.
    5.  understand the procedures outlined in EPA Reference Method 1 for locating
      sampling points in rectangular and circular ducts.
    6.  outline how one can check for the presence of cyclonic flow.
    7.  locate in Volume III a listing of suggested equipment for a source-test team.
    8.  use proper labeling procedures for source-test reagents and samples.
    9.  discuss why chain-of-custody procedures are important in compliance test
      cases.
  10.  summarize EPA Reference Methods 2 through 8.

Materials

Assignment 3
  Table of Contents of Volume III and pages 1 through 4 of Volume III, Purpose
  and Overview of the Quality Assurance Handbook
Assignment 4
  First three parts of Section 3.0 of Volume III, including:
    3.0  Summary
    3.0.1 Planning the Test Program
    3.0.2 General Factors Involved in Stationary Source Testing
    3.0.3 Chain-of-Custody Procedure for Source Sampling
Assignment 5
  • Section 3.1  Summary and Method Highlights for Method 2
  • Section 3.1.12 Data Forms for Method  2
                                    87

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       Reading Guidance—Assignment 3
Volume III of the US EPA Quality Assurance Handbook contains a great deal of
accumulated material. At first glance, it may seem more than one can deal with,
but on closer examination, you will find that much of Volume III contains
reference material, check sheets, or data forms.
  The handbook contains a great deal of information that you would normally
have to look up in periodicals, books, or EPA reports. The handbook brings
together much scattered information and gives detailed procedures which in many
cases amplify those given in the Code of Federal Regulations. Volume III expands
on the methods required, what is suggested, and what is not required.
             Begin your reading of Volume III by reviewing the Table
             of Contents, pages 1 of 4 through 4 of 4, and Purpose and
             Overview  of the Quality Assurance Handbook, which
             follows, pages 1 of 5 through 5 of 5.
  Many points in the reference methods can be subject to interpretation. Different
agencies have established their own interpretations of many of these points. In fact,
if we consider several agencies, there may be five or six ways of doing the same
thing. Volume III presents detailed and consistent procedures so that ambiguity
can be held to a minimum. The procedure that was elected may or may not be
better than some of the others that are possible. Ideally, the methods will be made
more uniform throughout the agencies through the use of Volume III.
  Volume III is organized for compliance testing. If source testers closely follow the
procedures, they should get results with good reproducibility. Hopefully, the results
will be accurate; however, it is difficult to determine accuracy in source sampling
because the true value of the emissions is seldom known. The reference method
procedures may in some cases give results higher than true because of the way in
which calibrations or corrections are made. However, this is not a great problem
for agencies in terms of compliance testing  since if a source is within the emission
standard as determined by the reference method, any positive testing bias would
imply that the source is even cleaner than determined.
  When testing is performed for tuning process operations, determining efficiency
guarantees, and so on, even more  care must be taken. For example, pitot-tube—
probe assemblies would need to  be calibrated as used in the test, impinger catches
accounted for, etc.
                                     89

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  In Volume III, each reference method is divided into the following sections.
Summary
Method Highlights
Method Description
1.
2.
3.
4.
5.
6.
7.
8.
9.

10.
11.
12.
Procurement of Apparatus and Supplies
Calibration of Apparatus
Presampling Operations
On-site Measurements
Postsampling Operations
Calculations
Maintenance
Auditing Procedures
Recommended Standards for
Establishing Traceability
Reference Method
References
Data Forms
Documented as
	 1
	 2
	 3
	 4
	 5
	 6
	 7
	 8

	 9
	 10
	 11
	 12
  This makes it easy to know where to go for information about a reference
method. This organization also allows you to prepare separate manuals for specific
purposes. For example, a calibration manual can be developed by removing Sub-
sections S.I.2, 3.2.2, 3.3.2, etc., and combining them. A test team checking equip-
ment before a test could then easily find and follow the required procedures.
  Similarly, an on-site testing manual can be prepared by combining Subsections
3.1.4, 3.2.4,  3.3.4, etc. A manual for the analytical laboratory can be prepared by
using Subsections 3.1.5, 3.2.5, 3.3.5, and so on.
  The figure  on the following page shows how the seven major sections of Volume III
are organized:
                                       90

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  Each of these sections (e.g., S.I.5) contains an important summary sheet called
the Activity Matrix. The activity matrix for the procedure discussed (calibration,
on-site measurement, etc.) provides a readily referenced table of the quality
assurance activities, acceptance limits, and action requirements.
  In the section for each method, Part 10 contains the promulgated reference
method as it appears in the Code of Federal Regulations, Part 11 contains a list of
references,  and Part 12 contains a compilation of clean data forms which can be
reproduced and used by the testing team.
             You have completed your reading for Assignment 3. If
             you are satisfied that you understand this material, go on
             to Reading Assignment 4. It begins on the following
             page.
                                      92

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       Reading Guidance—Assignment 4
            Continue your reading  of Volume III. To review some
            general aspects of source testing, read the first four parts of
            Section 3.0, including:
              Summary
              S.O.I Planning the Test Program
              5.0.2 General Factors Involved in Stationary Source
                   Testing
              S.O.S Chain-of-Custody Procedure for Source Sampling
  This reading assignment incorporates a review of the purposes and the planning
of a source test. This part of Volume III also contains a discussion of a number of
general factors involved in source testing.
  The discussion and check-off sheets of Section 3.0.1, pages 1 through 8, provide
information which when used, may help the tester avoid problems when conducting
the actual test.
  Note that EPA Reference Method 1 appears in Section 3.0.1, pages
8 through 19, as part of the discussion on planning the test program. Since site
selection is fairly general for all of the reference methods, the authors of the hand-
book felt that it would more appropriately be discussed here than separately.
  Note that in Figure 1.4 (page 9 of 19) the minimum number of traverse points
are different for velocity measurements and paniculate matter measurements.
Recent studies have determined that for velocity measurements, a greater number
of sampling points do not necessarily give greater reproducibility or accuracy. For
this reason fewer traverse points are specified for velocity measurements.
  Note: In Figure 1.4, the graphs for nonparticulate traverses were mislabeled on
the May 1, 1979 Revision 0. The upper dashed line is for stack diameters greater
than 0.61 m (24 in.). The lower is for stack diameters from 0.30 to 0.61 m
(12-24 in.).
  Since an even matrix arrangement of traverse points will give more representative
data,  the balanced matrix approach for rectangular ducts was incorporated into
the August 18, 1977 revisions to the reference methods.
  Measuring gases or paniculate matter where  cyclonic flow is present is indeed a
problem. Paragraph 1.2.3, on page 14 of Section 3.0.1, tells  how to detect cyclonic
flow. If cyclonic flow is present, you should try to either sample at a better location
or straighten the flow. Various methods have been proposed for measuring under
such conditions. They do, however, take considerable time to perform, and it has
                                     93

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not been generally shown that the data produced will be representative. The
following references can provide additional information on these procedures:
         Baker, D.W. and Sayre, C.L. "Decay of Swirling Turbulent Flow
      of Incompressible Fluids in Long Pipes." Flow: Its Measurement and
      Control in Science and Industry,  Volume 1,  Part 1, Flow Character-
      istics, Instrument Society of America, 1974.
         Mason, K.W. Location of the Sampling Nozzle in Tangential
      Flow. M.S. Thesis, University of Florida, Gainesville, Florida, 1974.
         Chigier, N.A. "Velocity Measurement  in Vortex  Flows." Flow: Its
      Measurement and Control in Science and Industry,  Volume 1, Part 1,
      Flow Characteristics, Instrument Society  of America, 1974.
         Lundgren, D.A., Durham,  M.D. and Mason, K.W. "Sampling of
      Tangential Flow Streams." Am. Ind. Hgy. Assoc.J., 39:640, 1978.
         Peeler, J.W.  "Isokinetic paniculate sampling in non-parallel flow
      systems—cyclonic flow," paper prepared by Entropy Environmentalists,
      Inc. for the US Environmental Protection Agency,  EPA Contract
      #68-01-4148, 1977, 27 p. (Contact EPA,  DSSE for  copies).
         Phoenix, F.J. and Grove, DJ. "Cyclonic flow—characterization
      and recommended sampling approaches," paper prepared by Entropy
      Environmentalists, Inc. for the US Environmental Protection Agency,
      EPA Contract #68-01-4148, November 1977, 14 p. (Contact  EPA,
      DSSE for copies).
  The discussion on General Factors Involved in Stationary Source  Testing contains
a convenient checklist  of the sampling tools and equipment that a source test team
may need on a job.  It is a good compilation to use if your team has not already
devised one of its own.
  Paragraphs 2.2 and 2.3 of Section 3.0.2 are important  reminders to samplers. In
the rush of completing a job, or especially when problems crop up, the proper
documentation of readings often is neglected. When data forms are used,  they
should be properly completed. The identification of samples is extremely important
and is discussed in more detail in the next section on Chain of Custody.
  Section 3.0.3 describes chain-of-custody procedures that should be implemented
in the testing organization. Such procedures should be set up before the test is
done, and each individual involved should be aware of his responsibilities  in the
chain.
  The labels and forms shown in Figures 3.1 through  3.5 are examples recom-
mended for your program. These or similar forms should be used in your organiza-
tion to properly document the handling of compliance samples.
  Chain-of-custody procedures are used to document who did what to a sample,
and when and how they did it. The  chain of custody starts with the preparation of
anything that becomes an integral part of the sample (such as a filter) and con-
tinues through to the disposal of the sample.
  Note: We will not cover Section 3.0.4 in this course since it is more directly
applicable to quality assurance activities related  to continuous emission monitoring.
                                      94

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You have completed your reading for Assignment 4. If
you are satisfied that you have mastered this material, go
on to Reading Assignment 5. It begins on the following
page.
                        95

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       Reading  Guidance—Assignment 5
             Read Section S.I  Summary and Method Highlights for
             Method 2. If you  would like a review of other reference
             methods before proceeding  with  this correspondence
             course, review the Summary of Sections S.S through 5.7.
This reading assignment is intended as a review of the reference methods. Do read
all of Section 3.2, Summary and Method Highlights (9 pages). Each of the other
reference method sections is organized in the same fashion. In fact, the Method
Highlight sections for the other methods discussed in Volume III all say about the
same thing.
  But note the format.  Section S.I briefly gives an overview of what will  be dis-
cussed about the method. Just after this overview, blank check sheets are  provided
for you to reproduce and use. We recommend that they be used in the test pro-
gram to properly document procedures. Note that blank data forms are provided
in Pan 12.0, at the end of each discussion of the method. Considerable controversy
surrounds the use of the check sheets and data forms in a source test program.
Remember that the forms and quality assurance procedures given in Volume III
are recommended. Their use is not part of a promulgated Federal regulation. An
agency should avoid requiring that these forms or procedures be used rather than
other forms or procedures currently used by established testing firms.  Many testing
organizations had already adopted their own procedures for assuring quality data
before Volume III was published. In many cases, their procedures may be as good
as or better than those given in Volume III. In other cases, they may not. Volume
III provides the first compilation of a standard set of QA methods for source
testing. The procedures  given in Volume III are recommended, but do not
necessarily preclude equivalent or more stringent techniques.
  The numbering scheme for blank data forms is given in Section S.I. 12.
            Read Page 1 of 8, Section S.I. 12 Data Forms.
            Review pages 2 of 8 through 8 of 8, Section S.I.12.
  This scheme is consistent for each reference method throughout the manual.
Note that not all of the Volume III data forms are included in Section 12 of each
method. Others are located in the Method Highlights sections or elsewhere in the
text. The form numbers are not printed on those placed in the Method Highlights
sections. These are, however, identified and referenced in each of the Data Forms
sections (Section 12).
                                     97

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            If you would like a quick review of Reference Methods 3
            through 8, read the Summary and Method Highlights of
            Sections 3.3, 3.4,  3.5, 3.6, 3.7, and 3.8.
             You have completed your reading for Assignment 5. Do
             the review exercises for Assignments 3, 4, and 5. They
             begin on the following page. When you have completed
             them, check your answers with those given on the page
             following the review exercises.
 Reading Assignments 3, 4,  and 5 Review  Exercises
1.  Super Stack Testers (SST) has been providing manual stack testing services for
   industrial clients for two years. The company has been doing well and now has
   a staff of nine people. It normally can send two test teams at a time into the
   field, and in a pinch  can send out three. SST has recently had the opportunity
   to bid on several sampling jobs, but the jobs require that the company have an
   established quality assurance program.
     Carl, the president of the company, has decided that separate manuals
   should be prepared for each function of his testing company. A calibration
   manual is especially needed. To make a calibration manual from  Volume III,
   which sections would you abstract?
   a. 3.1.1, 3.2.1,  S.S.I	5.7.1
   b. 3.1.1, 3.1.2,  3.1.3,...,3.1.12
   c. 3.1.2, 3.2.2,  3.3.2	3.7.2
   d. 3.1.9, 3.2.9,  3.3.9	3.7.9
2.  Since Carl's turnover  rate  for lab technicians is high, he also wants to develop
   a manual that could be used to assure quality data from his analytical lab.
   Which sections of Volume III could he abstract to do this?
   a. 3.1.8, 3.2.8,  3.3.8	3.7.8
   b. 3.1.12, 3.2.12, 3.3.12	3.7.12
   c. 3.5.5, 3.6.5,  and 3.7.5
   d. 3.1.5, 3.2.5,  3.3.5	3.7.5
                                     98

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3. Mike has just recently joined the staff and is to accompany a team on a job in
   which Method 7 samples are to be taken. Mike has done Method 7 before, but
   wants to review the procedures to make sure that he can follow all of them cor-
   rectly. Which section of Volume III should he review?
   a. 3.5
   b. 3.6
   c. 3.6.4
   d. 3.0
4. What does Section 3.0 of Volume III contain?
   a. a review of how to do Methods 2 through 8
   b. statistical procedures for determining test accuracy
   c. a discussion of how to plan and  document a source test
   d. a discussion of quality assurance requirements for continuous emission
      monitoring
5. What are  the responsibilities of the source tester?
   a. to follow standard testing procedures and document each step of the work
   b. to get the data as quickly as possible and get home
   c. to get a sample from the stack, no matter how
   d. to fill in all the check lists and data forms of Volume III
6. When planning a Method 5 source  test, which one of the following activities
   would not be performed?
   a. determine applicable emission control regulations
   b. determine sampling site and sampling points
   c. determine process information
   d. determine SRM values
7. Dennis,  a  team leader of SST, has been having trouble with everyone else
   borrowing his tools. In  order to make sure he has everything he needs on a
   stack test,  he developed a checklist  from the tools and equipment listing given
   in Volume III. Where is this listing?
   a. in Section 3.0.1
   b. in Section 3.0.2
   c. in Section S.O.S
   d. in Section 3.0.4
8. Dennis is planning a Method 5_ test  at Sheer Power Company. Platforms and
   ports are in a breeching six equivalent duct diameters downstream from a
   bend and two from the stack. What are the minimum number of points
   required for a  Method 2 traverse and for a Method 5 traverse?
   a. 12 for Method 2; 12 for Method 5
   b. 16 for Method 2; 24 for Method 5
   c. 12 for Method 2; 24 for Method 5
   d. 24 for Method 2; 16 for Method 5
                                     99

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 9. Which one of the following depicts a balanced matrix for 12 traverse points in
    a rectangular duct?
    a.                            „	     c.






























Ports

j


    b.




u




u




u




u




u




u
d.
10. When checking for cyclonic flow, no reading will be obtained on a pitot tube
    manometer if:
    a. the direction of gas flow is perpendicular to the plane of the pitot tube face
       openings.
    b. the direction of gas flow is parallel to the plane of the pitot tube face
       openings.
11. True or False? The Federal reference methods require that a degree-indicating
    level be used when determining the angles of rotation of cyclonic flow.
12. Admissible data in a court case must show that the sample was:
    a. collected properly.
    b. handled properly.
    c. analyzed properly.
    d. all of the above
13. Mike, when labeling the filters for his first Method 5 test with SST, carefully
    put the run numbers 1 cm from the edge of the filters. After the test, he could
    identify the filters  from runs 1 and 3, but could not find the number on the
    filter from the second run. What happened?
    a. Acid in the stack erased the number.
    b. He probably inadvertently put in a filter he did not label.
    c. The filter was put in the holder with the number  on the face side.
    d. It never could have happened.
                                      100

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14. SST has been using/efr pens to label their plastic collection bottles, but the
    bottles are beginning to look pretty messy because the ink does not come off
    afterwards. Mike has decided to buy some tick-and-stick labels to use instead.
    Will this work?
    a. Yes. It is a great idea because labels that you can lick are inexpensive.
    b. Yes. It is a great idea because you have sample identification and can reuse
       your bottles, too.
    c. No. Water-soluble labels do not stick well on plastic. He should have bought
       self-adhesive labels instead.
    d. No. Sample bottles do not have to be identified because you can remember
       which is which anyway.
15. Which of the following would be included in chain-of-custody procedures?
    a. Method 5 filters
    b. Method 7 absorbing solution
    c. Method 5 probe wash
    d. signature of test team leaders
    e. all of the above
    f.  none of the above
16. Consider the format of Section S.I, which discusses  Method 2—Determination
    of Stack Gas Velocity and Volumetric Flow Rate. Where can blank check
    sheets for  the method be found?
    a. in Section S.I.12
    b. in Section S.I after the discussion on Method Highlights
    c. at the end of Sections 3.1.1, S.I.2, S.I.5,  etc.
    d. at the end of Volume III
17. The activity matrices provide a means of quickly reviewing the operations and
    quality assurance activities involved in the different phases of a reference
    method. How many activity matrices are given for Reference Method 2?
    a. 1
    b. 12
    c. 8
    d. 6
18. Give the titles  of the forms listed below:
    a. M2-1.2 	
    b. M2-2.5 	
    c. M2-8.1 	
    d. M2-S.2 	
19. Give the form number for the following data forms:
    a.  Method 2 Stack Temperature Sensor Calibration Data Form.
    b.  Method 2 Gas Velocity Data Form	
    c.  Method 2 Pretest Sampling Checks_
    d.  Method 2 Posttest Sampling Checks.
                                      101

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                  Answers to
Reading Assignments 3, 4, and 5 Review Exercises
1.
2.
S.
4.
5.
6.
7.
8.
9.
10.
11.
12.
IS.
14.
15.
16.
17.
18.



19.



a
a
a I
a
(a)
a
a 1
a 1
a
a (
T
a
a
a
a
CO'
a
a.
b.
c.
d.
a.
b.
c.
d.
b
b
5
b
b
b
S
(b
b
J
(CJ
c (
) c
Q
c
c (
) c
) c
0
)
d
d)
d
d
d
d)
d
d
d

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b
b
b
b
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b
c (
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c
) c
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d)
d
d
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d
d
Procurement Log

Pitot
Tube Calibration Data
Method 2— Auditor's Checklist
Pretest Preparations




M2-2
M2-4
M2-S
M2-5
.10
.1
.1
.1
                      102

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Pretest Operations
 Lesson C — Procurement of Equipment
           Reading Assignment 6
           Reading Assignment 7
           Reading Assignment 8
 Lesson D—Calibration of Equipment
           Reading Assignment 9
           Reading Assignment 10
 Lesson E — Presampling Operations
           Reading Assignment 11
                103

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                         Lesson   C
            Procurement of  Equipment
Lesson Goal

The goal of this lesson is for you to be able to purchase source sampling equipment
which will perform in the field and will meet the specifications given in Federal
regulations.

Lesson Objectives

After completing this lesson, you should be able to:
  1. use a procurement log to track the status of purchased equipment.
  2. use the activity matrices given at the end of each Subsection 3	1 as aides
     when checking purchased equipment.
  3. measure pitot tube misalignment angles for the determination of tube
     acceptability.
  4. leak check a differential pressure gauge.
  5. list at least two desirable design qualities of an Orsat analyzer.
  6. describe how to check the acceptability of a sample probe.
  7. check common laboratory equipment such as impingers, vacuum pumps,
     thermometers, graduated cylinders, barometers, etc., for acceptability.
  8. check the acceptability of acetone and isopropanol used in source sampling.
  9. check reagent grades of chemicals used in reference method analytical
     procedures.

Materials

Assignment 6
  • Section 3.1.1, Procurement of Apparatus and Supplies in Section  3.1
    Method  2—Determination of Stack Gas Velocity and Volumetric Flow Rate
Assignment 7
  • Section 3.2.1, Procurement of Apparatus and Supplies in Section  3.2
    Method 3—Determination of COt, O», Excess Air, and Dry Molecular Weight
  • Section S.S.I, Procurement of Apparatus and Supplies in Section  3.3
    Method  4—Determination of Moisture in Stack Gases
  • Section 3.4.1, Procurement of Apparatus and Supplies in Section 3.4
    Method 5—Determination of Paniculate Matter from Stationary Sources
                                   105

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Assignment 8
  • Section 3.5.1, Procurement of Apparatus and Supplies
    Method 6—Determination of Sulfur Dioxide Emissions from Stationary Sources
  • Section S.6.1, Procurement of Apparatus and Supplies
    Method 7—Determination of Nitrogen Oxide Emissions from Stationary Sources
                                     106

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       Reading Guidance—Assignment  6
             Begin your reading of Lesson C with Section 3.1.1 —
             Procurement of Apparatus and Supplies, Method 2.
             Read pages 1 of 15 through 15 of 15.
Figure 1.2 is provided to assist in documenting procurement actions. For those
involved in purchasing equipment and air analyzers, an excellent discussion on pro-
curement quality control is given by M.J. Kopecky and B. Rodger (Wisconsin
Department of Natural Resources) in Quality Assurance for Procurement of Air
Analyzers, ASQC Technical Conference Transactions; 1979, Houston, Texas.
American Society for Quality Control. 1979:35-40.
  Many of the quality assurance activities given in Volume III for the procurement
of apparatus and supplies merely deal with inspecting the purchased items  after
they are received. This section is useful since it points out what you should look for
or, in some cases, how you  can properly check to see that you received a quality
product for your money. Since less experienced testers may not be aware of all of
the things to look for, the activity matrices of Table 1.1, etc., can be useful and
convenient  guides.
  Note, on pages 4 and 5 of Section 3.1.1, the many measurements one can make
on a pitot tube. Method 2 gives geometric standards for the assignment of  a coeffi-
cient, Cp = 0.84, for a bare  Type S pilot tube. The EPA did not, however,  specify a
measurement technique to determine the various angles and dimensions associated
with a Type S tube's construction. Volume III describes a technique discussed by
T.R. Clark, W. Mason and P. Reinermann, III (PEDCo. Environmental),  Source
Evaluation  Society Newsletter, Volume V, No. 1,  1980.
  Note that the data sheet  (Figure 1.7) has the acceptance criteria on it.
  In the field, the worst case misalignments would be similar to those shown in
Figure 1.4.  A 10° misalignment angle should be obvious to the eye, but if there is
doubt as to acceptability for smaller angle misalignments, the tube should  be
measured.
  Care should be taken in specifying a Cf = 0.84 for a pitot tube attached to a
probe or to anything else where aerodynamic interferences may occur.  Even a one-
inch separation of the tube from the probe may not necessarily eliminate all such
interferences. In such a case, the true Cf will normally be lower than 0.84. By
assuming a  value of 0.84, the velocity and volumetric flow rate will be larger than
true, giving a positive bias to the data. For accurate data, the tube-probe assembly
should be calibrated in a wind tunnel.
                                    107

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  Differential pressure gauges, liqi d-filled manometers, or magnehelics should be
checked upon receipt for leaks. Page 12 of Section 3.1.1 offers a procedure for
doing this.
  Take note of other apparatus used. Liquid-filled bulb thermometers should be
checked periodically for liquid separation. Thermocouple systems should be
checked frequently for consistency in reading—problems are hard to check visually,
but if the LED readout says the ambient air temperature is 150°F, you have a
problem.
             You have completed your reading for Assignment 6. Do
             the  review  exercises  which follow;  then check your
             answers. The correct answers are given on the page
             following the review exercises.
           Reading Assignment 6 Review Exercises
1.  Carl had to order a new pitot tube for Method 2 traverses since Mike dropped a
   meter box on the old one. Carl got a deal from Fast-Weld Products in Hialeah,
   Florida. Carl filled out Purchase Order SST-238, on June 6, 1981 for pitot tube
   model #FWB-S951. The catalogue cost was $68.00. Fill in the form on page 3
   of 15, Section 3.1.1, with this information.
2.  When Carl received the tube on August 29, 1981, Fast-Weld sent along a cer-
   tification stating that "The Type S pitot model #FWB-S951 No. 68 was
   calibrated and determined to have a C, value equal to 0.899 ±0.001 in." Fast-
   Weld charged SST  $35.00 for the calibration and an additional $19.76 for
   taxes, shipping, and handling. Log this information into the procurement form.
3.  Carl gave the tube to Mike so that he could check the design parameters.
   Something about the tube looked odd.  By using the measurement methods
   described in Section 3.1.1,  he found the following:
       D, =0.373 in.     a, = 6°       a, = 0°      0 = 5°
       PA= 0.398 in.                               -y=100
       PB= 0.402 in.     0, = & = 0
   Look at pages 8 of 15 and  9 of 15 of Section 3.1.1 to see how Mike determined
   the  values for a, ft, and y.
   Calculate the value of z.
   a. z = 0.139 in.
   b. z = 0.069 in.
   c. z = 0.070 in.
   d. z = 0.052 in.
                                     108

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4. Calculate the value of w.
   a.  w = 0.698 in.
   b.  w = 0.139 in.
   c.  w = 0.070 in.
   d.  w = 0.052 in.
5. Based upon the values given and calculated in Exercise 5, what should be done
   with the probe?
   a.  It should be judged acceptable and should be used in the field with the cer-
      tified value of 0.840.
   b.  It should be judged acceptable, but the Cp value should be corrected by sub-
      tracting 5% of the certified value.
   c.  It should be judged acceptable, but should be recalibrated by SST in a wind
      tunnel.
   d.  It should be returned to the vendor.
6. A 10-inch oil-filled inclined manometer was purchased to determine Ap values
   across the pitot tube. When it was received, Mike leveled it and zeroed it. He
   then blew into the positive leg of the manometer and sealed it at a reading of
   4.5 in. HjO. Over a minute, no change in the reading was  observed. What con-
   clusions should be made?
   a.  The fluid flow is blocked.
   b.  The manometer leaks.
   c.  The positive side of the manometer is leak free.
   d.  The negative side of the manometer is leak free.
                                      109

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                    Answers to
       Reading Assignment 6 Review Exercises
i.
Item description
Pitot tube
Pilot tube
Model FWB-3951
Quantity
1
1
Purchase
order
number
764308
SS7-238
Vendor
Ace Metal
Fast-Weld
Date
Ordered
9-6-79
6-6-81
Received
9-29-79

Cost
86.00
68.00
Disposition
In service
Order
pending
Comments


2.


Item description
Pitot tube
Pitot tube
Model FWB-S951
Calibration
Taxes and
handling


Quantity
1
1




Purchase
order
number
764308
SS7-238






Vendor
Ace Metal
Fast-Weld




Date

Ordered
9-6-79 .
6-6-81




Received
9-29-79
8-29-81

8-29-81

8-29-81


Cost
86.00
68.00

35.00

19.76


Disposition
In service
Rec'd.






Comments

No. 68
C, = 0.899 ±
0.001 in.


3. 0 b  c  d
4.  a  b fcj d
5.  a  b  c @
6.  a  b (T) d
                         110

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       Reading Guidance—Assignment  7
This reading assignment covers the procurement of apparatus and supplies for
Methods S, 4, and 5. By now, you have either figured out the organization scheme
of Volume III or else are saying unkind things about this correspondence course.
Instead of carrying the whole of Volume III around with you when doing these
lessons, you might want to take Volume III apart and combine all of the procure-
ment sections, all of the on-site measurement sections, etc. This course deals with
each of these topics separately. Separating the sections will take about 15 minutes
to do, and it will save you time because it will eliminate the need for you to
continually leaf through the volume.
  Of course, when you are finished with all of the lessons, you can recombine the
sections and have the handbook organized as it was originally.
            Continue your reading with Section S.2.1 — Procurement
            of Apparatus and Supplies, Method S. Read pages 1 of 15
            through 15 of 15.
  In Section 3.2.1 on Procurement of Apparatus and Supplies for EPA Method 3,
pay primary attention to the discussion of the Orsat analyzer, starting with
paragraph 1.3.1 on page 8 of 15. In particular, note the Desirable Design Qualities
given on page 11 of 15 and the method for leak-checking a new apparatus,  given
on page 10 of 15.
  You might often have wondered what is in the various solutions of the Orsat
analyzer. Volume III provides this information for you. The discussion on Orsat
reagents is given on page 12 of 15 in Section 3.2.1.
  You should note that the Orsat method of determining Oj and CO» is the EPA
Reference Method. Alternate methods, such as the Fyrite or continuous Ot or CO2
analyzers may be used to determine molecular weight. However, when using Ot or
COZ measurements for reporting emissions in units of the standard (i.e., lbs/106
Btu heat input for combustion sources), Orsat data is used. Other methods,
however, may be used for this purpose if approval is first obtained from the
administrator.
            Continue your reading with Section 3.3.1 — Procurement
            of Apparatus and Supplies, Method 4. Read pages 1 of 9
            through 9 of 9.
                                    Ill

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  Section 3.3.1 covers the apparatus that is needed for EPA Reference Method 4—
Determination of Moisture in Stack Gases. By now, you should have noticed the
organization in the procurement sections 3	1. First,  a schematic of the sampling
train is discussed, then procurement logs are discussed. The section proceeds with a
discussion of individual items and tells exactly what equipment is needed to do the
reference method. Descriptions of pumps, thermometers, manometers, etc., are
generally the same throughout the reference method  discussions, so if you
thoroughly read about this apparatus once,  you can just skim over these parts in
subsequent reading assignments.
  Carefully read the discussion of the probe. Since you must have a heated probe
for the moisture determination,  special care should be taken to inspect it for elec-
trical continuity and for leaks.
  Note the method of checking  a  Greenburg-Smith impinger for leaks.  It is given
on page 5 of 9 in Section 3.3.1.
  Paragraph 1.1.9 on page 7 of 9 in Section 3.S.I refers to the measurement of
moisture in saturated gas streams. The exhaust gas from wet scrubbers or certain
industrial processes may be saturated with water vapor and may even contain
entrained water droplets. In  such  cases, the condensation technique of Method 4  is
not applicable. Instead,  one  merely measures the stack gas temperature and looks
up the moisture percentage on a psychometric chart  or in saturation vapor pressure
tables. It is recommended, however, that the temperature sensor used have an
accuracy of ±  1 °C (± 2 °F) when applying this method. This is in  contrast to an
accuracy requirement of 1.5% of the minimum absolute stack temperature for nor-
mal stack temperature measurements.  At 40°C (100°F), a 1.5% accuracy of the
absolute  temperature would  give a range of ±8.4%, and this would lead to greater
ambiguity in reading the saturation vapor pressure tables.
  Obtaining a temperature sensor with an accuracy within ± 1 °C (2 °F) should not
be too difficult since the temperature range for this technique will generally be
below 100°C (212 °F).
             Continue your reading with Section 3.4.1 — Procurement
             of Apparatus and Supplies, Method 5. Read pages 1 of 15
             through 15 of 15.
  Section 3.4.1 covers the procurement of apparatus and supplies for EPA
Reference Method 5. You have had to read a lot of material to get to this point,
but this may be the most important section for you if you are planning to purchase
a Method 5  sampling train. Ten years ago,  many people used to construct their
own Method 5 trains. Now, over half a dozen commercial firms sell sampling
equipment.  Although the catalogue prices may seem high, it is usually cost-
effective, just in terms of labor hours,  to purchase commercial equipment. You can
consult trade journals such as Pollution Equipment News, Journal of the Air Pollu-
tion Control Association, and Pollution Engineering for the names of vendors of
this equipment.
                                     112

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  First, obtain the vendor literature on your instrumentation. Then cross-check the
equipment specifications against the QA requirements given in Section 3.4.1. Since
most commercial systems meet these requirements, you might consider other fac-
tors, such as ease of handling and ease of repair. Ask around and see what other
stack testers are using and what they like and do not like about different types of
apparatus. The more information you have,  the better decision you will be able to
make. Refer to the article by Kopecky, discussed on page 107 of this course, for
further guidelines on procurement quality control.
  The probe discussion is much the same as  that given for Method 4, but do read
the probe nozzle discussion (page 5 of 15, Section S.4.1) carefully.
  Carefully read Section 1.1.8 on page 7 of 15.  Note  that the metering system
should be checked for leaks upon receipt.
  Sections 1.2, 1.3,  and 1.4 cover the supplies that will be needed for performing a
Method 5 test. The recommendations are based upon experience with sampling
under field conditions.
             You have completed your reading for Assignment 7. Do
             the  review  exercises which  follow;  then check  your
             answers. The correct  answers are given on  the  page
             following the review exercises.
          Reading Assignment 7 Review Exercises
    Which one of the following would not be a proper criterion for selecting a
    sampling probe?
    a.  The probe material should be inert to the stack gas constituents.
    b.  The probe should be resistant to temperature effects at sampling conditions.
    c.  The probe should provide for some means of filtering out paniculate
       matter.
    d.  The probe should be traceable to an NBS standard probe.
    What is normally used to reduce the pulsation effect of diaphragm pumps on
    rate meters and volumetric flow meters?
    a.  surge tanks
    b.  baffles
    c.  glass wool
    d.  slider valves
                                     113

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3. At what pressure should a Tedlar®  bag used in Method 3 be leak checked?
   a.  5 to 10 cm (2 to 4 in.) vacuum
   b.  5 to 10 cm (2 to 4 in.) H,O
   c.  15  psi (1 atm)
   d.  1 cm (0.39 in.) H2O
4. List the reagents used for the three absorbing solutions in an Orsat analyzer.
   a.  CO,	
   b.  O»  	
   c.  CO 	
5. Why should the volume reference mark be on the capillary tube of an Orsat
   analyzer and not on the larger-diameter glass burette?
   a.  Precision in reading is increased if it is on the capillary.
   b.  Accuracy in reading is increased if it is on the capillary.
   c.  both of the above
   d.  none of the above
6. Bob, a member of SST's test team, was leak checking a new Orsat analyzer.
   After  displacing the burette liquid to obtain a reading of 25 ml, he closed the
   manifold valve and waited 4 minutes. What change in the meniscus level
   would indicate that the apparatus is acceptable?
7. Of what is the confining solution of an Orsat analyzer composed?
   a.  water colored with red food dye
   b.  water, sodium sulfate, sulfuric acid,  and methyl orange
   c.  antifreeze
8. Four steps are given in  Volume III for checking a probe heating system.
   •  connect probe to pump
   •  connect heater and turn on
   •  turn on pump and adjust flow rate
   •  maintain temperature
   Answer the following:
   a.  For how long do you warm up the probe?	
   b.  At  what flow rate do you pump?	
   c.  What temperature is to be maintained?	
9. How do you check a standard Greenburg-Smith impinger?
   a.  fill inner tube with water and check dram rate
   b.  check visually for flaws or cracks
   c.  pressurize at two atmospheres and check with Snoop®
   d.  both a and b
   e.  a,  b, and c
                                    114

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10. What valu*- is subtracted from a sea-level barometric reading for each increase
    of SO m (loJ ft) in altitude?
    a. 2.5 mm Hg
    b. 760 mm Hg
    c. 0.76 mm Hg
    d. 250 mm Hg
11. What precision is required for a thermometer used to measure the temperature
    of a saturated stack gas?
    a. ± 1.5% of stack temperature in °C
    b. ± 1.5% of stack temperature in °R
    c. ±2% of stack temperature in °C
    d. ± 2 °F (1 °C) of stack temperature
12. What should you do to a nozzle after it is received from the manufacturer?
    a. Bang it on a table to see if it will keep its tolerances.
    b. Measure the nozzle diameter with a ruler to see if you agree with the
       manufacturer's value.
    c. Engrave it for identification and inventory purposes.
    d. Throw it in the tool box, so you will not forget it for tomorrow's test.
13. Mike ordered filters, for use in the Method  5 train, from Roger's High School
    Chem Lab Supply Company. Would these be acceptable for Method 5 testing?
    Yes	
    No	
    Why or why not?
14. What grade of acetone should be used for cleaning the apparatus used for
    Method 5 testing?
                                      115

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                           Answers to
         Reading Assignment 7 Review Exercises
 1.
 2.
 3.
 4
 a b  c (^
T) b  c  d
Cx
 a Hy c  d
 a    CO2 —KOH or NaOH solution
 b.
    c.
          O2—pyrogallic acid or chromous chloride solution
          CO—cuprous chloride or cuprous sulfate solution
 5.  a  b (c^ d
 6.  A change of <0.2 ml
 7.  a (b) c  d
 g  a     2 or 3 minutes	
    b.
          0.02 mVmin (0.75 ftVm)
 9.
10. 0 b
    c     1000C(212°F)minimum
    a  b  c
          c  d
11.  a  b  c 0
12.  a @0 d
IS.  No, because they may not give the required collection efficiency and may
    deteriorate at the elevated sample case temperatures.
14.  ACS grade
                                 116

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       Reading Guidance—Assignment  8
Reading Assignment 8 covers primarily Methods 6 and 7. The discussion of the
sampling equipment is much the same as that given in previous discussions of
Methods 3,4, and 5. Pay close attention to details of the equipment and supplies
used in the analytical procedures.
  In particular, certain grades of reagents are required in the laboratory analysis.
A review of the different types of chemical grades is given below.
  Technical or commercial grade. Chemicals labeled technical or commercial
grade are of indeterminate quality and should be used only where high purity is
not of paramount importance. In general, technical or commercial grade chemicals
are not used in analytical work.
  Chemically Pure, or C.P. grade. The term, Chemically Pure, has little definite
meaning. Such reagents are usually more refined than are the technical grades, but
no specifications define what is meant by the term. Thus, it is prudent to avoid the
use of C.P. reagents in analytical work. If this is not possible, testing the reagent
for  contaminants of importance and running frequent reagent blanks may be
necessary.
  U.S.P. grade. U.S.P. chemicals have been found to conform to tolerances
specified in the United States Pharmacopoeia. The specifications are designed to
control the presence of contaminants dangerous to health; thus, chemicals passing
U.S.P. tests may still be quite heavily contaminated with impurities that are not
physiological hazards.
  Reagent grade. For the most part,  the analytical chemist uses reagent grade
chemicals in his work. These  have been tested and found to conform to the
minimum specifications set down by the Reagent Chemicals Committee of the
American Chemical Society. In addition to meeting these requirements, the results
of the analysis are, in some instances, printed on the label. Thus reagent grade
chemicals fall into two categories: namely, those that simply pass the tests and
those for which the actual results of the tests are additionally supplied.
  Primary standard grade. These are substances that are obtainable in extraor-
dinarily pure form. Primary standard grade reagents are available commercially;
these have been carefully analyzed and the assay value is printed on the label. An
excellent source for primary standard chemicals is the National Bureau of
Standards.
            Begin  by  reading  Section  S.5.1—Procurement  of
            Apparatus and Supplies, Method 6. Read pages 1 of 15
            through 15 of 15.
                                    117

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  Note paragraph 1.1.9 on page 7 of 15 in Section S.5.1. This paragraph presents
a method of checking a metering system for leaks. You have not read about this
yet, since for Reference Methods 4 and  5,  leak checking procedures are discussed in
the calibration Sections 3.3.2 and 3.4.2  (Subsections 2.1), respectively. Read
carefully the procedure given here so that  you can recognize the method when
similar descriptions are presented in the larger discussions on calibration
procedures.
  On page 10 of 15 of Section 3.5.1, a discussion of analytical laboratory supplies
begins. Although selecting such supplies may  appear straightforward, you should,
when doing routine testing, take care to assure that the laboratory and its supplies
remain clean and uncontaminated.
  The problem of contaminated isopropanol  has led to many cases of inconsistent
and invalid data. The preparation and testing of blanks is an important practice in
any analytical laboratory.
             Continue your reading with the discussion of Method 7
             procurement on page 4 of IS of Section 3.6.1.
  Note the specifications for the collection flask.
  Also, note the requirements for the evaporating dishes given on page 8 of IS of
Section 3.6.1.
  Method 8 is very similar to Method 5. It is not necessary to read Section 3.6.1 at
this time unless you have an immediate interest in the procurement of the
analytical reagents used in the method.
             You have completed your reading for Assignment 8. Do
             the review exercises which follow; then check  your
             answers. The correct answers are given on the  page
             following the review exercises.
          Reading Assignment 8  Review Exercises
1.  Which one of the following is not a criterion for rejecting a new dry gas
   meter?
   a.  The meter face is broken.
   b.  Readings are less than 3% of that determined with a spirometer.
   c.  The meter dial frequently sticks.
   d.  The meter is painted green instead of gray.
                                     118

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   What should be the capacity of the silica gel drying tube used in Method 6?
   a. 5 to 10 g silica gel
   b. SO to 50 g silica gel
   c. 100 to 150 g silica gel
   d. 6 to 16 g silica gel
   On a Held test, Mike realized that he had not prepared the isopropanol solution
   for the Method 6 impingers. He did have a bottle of ACS grade 100%
   isopropanol, so he quickly made the 80% solution by diluting with tap water.
   Was this a good thing to do?
   Yes	
   No	
   Why or why not?


   If your answer was "no", what would you have done  instead?
4. What types of reagents are to be used in Method 6?
   a.  ACS grade
   b.  PBS grade
   c.  NBS grade
   d.  C.P. grade

(Review exercises continue on page 120.)
                                     119

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5. The figure below shows a Method 7 train assembly. What is missing that would
   normally be on the Method '  ystem?             s^^\.

                                                          m
Glass wool
  filter
                  1—L
 Probe
ib
                                 Three-way
                                 flask valve
                                                                 • Manometer
                                                  Three-way
                                                 pump valve
                                                                  Pump
   a. orifice meter
   b. thermometer
   c. flask shield
   d. pitot tube
6. How many volumetric flasks, and what sizes, would have to be ordered for a
   Method 7 experiment?
   a. one 100-ml flask; two 1000-ml flasks; several 50-ml flasks
   b. ten 100-ml flasks; five 1000-ml flasks
   c. three 1-L flasks
7. What do you need to make phenoldisulfonic acid solution?
   a. phenol,  water, and disulfonic acid
   b. phenol and sulfuric acid
   c. sulfone, phenolidene, and distilled water
8. In what wavelength range must a spectrophotometer used in Method 7 be
   capable of  measuring?
   a. 210 to 214 nm
   b. 3.5 to 4.6 fan
   c. 2000 A  to SOOO A
   d. 400 to 415 nm
                                     120

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                           Answers to
         Reading Assignment 8 Review Exercises
1. a b c (d)
2. a (b) c d
S. Yes
No x
    Sulfates may be introduced from the tap water.
    Purchase distilled water in a supermarket, or better yet, go to a local university
    or hospital and ask for some distilled water from a laboratory. A sample of the
    water should be retained for analysis as a blank.
4.  0 b   c  d
      ~  ^^
            d
                                 121

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                        Lesson  D
              Calibration of Equipment
Lesson Goal

The goal of this lesson is for you to understand the procedures that are to be
followed when calibrating equipment used in source sampling and analysis.

Lesson Objectives

After completing this lesson, you should be able to:
  1. describe how to set up a pitot tube calibration apparatus.
  2. perform the calculations used in reporting the pitot tube calibration
     coefficient, Q,.
  3. tell how to calibrate a thermometer, barometer, and differential pressure
     gauge.
  4. explain the procedure that is to be followed when checking the Orsat
     apparatus.
  5. explain, using a diagram,  how to calibrate a dry gas meter with a wet test
     meter.
  6. explain how to check the calibration of a wet test meter.

Materials

Assignment 9
  • Section 3.1.2, Calibration of Apparatus in Section 3.1
    Method  2—Determination of Stack Gas Velocity and Volumetric Flow Rate
  • Section 3.2.2, Calibration of Apparatus in Section 3.2
    Method  3 — Determination of COX, Oj, Excess Air, and Dry Molecular Weight
Assignment 10
  • Section 3.3.2, Calibration of Apparatus in Section 3.3
    Method  4—Determination of Moisture in Stack Gases
  • Section 3.5.2, Calibration of Apparatus in Section 3.5
    Method  6—Determination of Sulfur Dioxide Emissions from Stationary Sources
                                   123

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       Reading Guidance—Assignment 9
It is very important to use properly calibrated equipment when stack sampling.
Lesson D will emphasize the procedures that can be used to calibrate and check the
following types of equipment:
  1. pitot tubes
  2. dry gas meters and wet test meters
  5. thermometers, barometers, differential pressure gauges
  4. spectrophotometers
  The first reading assignment covers the calibration of the pitot tube, a check of
the Orsat apparatus, and methods for calibrating ancillary source sampling equip-
ment such as temperature sensors and barometers.
             Begin by reading Section 3.1.2—Calibration of Apparatus,
             Method 2. Read pages 1 of 21 through 21 of 21.
  In Lesson C, you reviewed the design criteria for assigning a Cp value of 0.84 to
a pitot tube. Section S.I.2, pages 1 of 21 to IS of 21, provides a method for
obtaining a laboratory-referenced value for Cp. Considerable experimental work has
shown that  by placing a pitot tube on a probe-nozzle assembly, the Cp value can
decrease. The interference-free criteria of % in. between pitot tube and nozzle may
not in all cases guarantee that the Cp will still be equal to 0.84 in this assembly. A
review of interference effects for several types of pitot-tube—probe  assemblies is
given in Williams, J.C. and Dejarnette, F.R., A Study on the Accuracy of Type-S
Pitot  Tubes EPA 600/4-77-030, June 1977.
  Note that if the true value of Cp is equal to 0.80  (for example), then when the
tube is attached to a probe, if a value of 0.84 is assumed instead, the following
error arises  when determining the stack gas velocity:
                           v,(true) = 0.80 K,
                        v,(assumed) = 0.84 K,
                         vXtrue)     0.80
                          assumed)   0.84

                           v/true) = 0.95 v.(assumed)
                                    125

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  The true velocity would therefore be lower than that obtained if the tester had
assumed a value of 0.84. This is an example of positive bias in stack sampling. If
the pollutant emissions were to be reported on a Ibs per hour basis, i.e.,
                           pollutant mass rate = c,v,A,
Where:    c, = the concentration of the pollutant
           A,= the area of the stack or duct
then the reported values would be higher than true and could possibly indicate a
violation when in fact there was none.
  The above illustration was given to underscore the importance of calibration in
obtaining accurate test data. It is often worth the effort to recheck calibrations if
there is a question about their validity.
  Paragraph 2.1.2 shows how you can construct a test setup for calibrating a pitot
tube. The major expense is the fan. You should  use a fan large enough to reach
representative stack velocities (see page 4 of 21—bottom of page).
  When performing this calibration, it is very important to properly align the
standard and Type S pitot  tubes, as discussed on page 6 of 21.
  Read the calibration procedure of paragraph 2.1.3 carefully. Note that standard
and Type S tube readings are  taken alternately.
  Paragraph 2.1.4 points out problems  that can occur if you attempt  to calibrate a
probe assembly if the test duct area is small relative to the probe. Correction fac-
tors for blockage effects are given in Figure 2.9 on page 14 of 21.
  Subsection 2.2 gives simple and straightforward procedures for calibrating
temperature sensors. Keep  in mind that when your temperature readings are used
in sampling calculations, they must be converted into absolute temperatures. Small
errors in degrees Celsius or degrees Fahrenheit may be relatively unimportant once
values are converted to kelvin  or degrees Rankine.
             Turn to Section 5.2.2, Calibration of Apparatus used for
             Method S—Determination of COlt  Of, Excess Air, and
             Dry Molecular Weight. Read Subsection 2.1 which gives
             a procedure for checking the performance  of both the
             operator and the Orsat analyzer.
             You have completed your reading for Assignment 9. Do
             the  review  exercises which follow;  then  check your
             answers. The correct answers are given on the page
             following the review exercises.
                                       126

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          Reading Assignment 9 Review Exercises
1. Carl obtained the following data in the calibration of Fast-Weld's No. 68 Type S
   pilot tube in a wind tunnel. Calculate the Cp(,) value where Cp(ad) = 0.99 (use
   form M2-2.5 in Section S.I. 12).
A-side calibration
Ap.,,,.
0.072 in. H,O
0.065
0.070
Ap,.
0.116 in.
H,O
0.120
0.118
B-side calibration
Ap,,,,.
0.060 in. H,O
0.060
0.065
Ap,
0.120 in.
H,O
0.122
0.118
2. Calculate the average DEV between CP(J) and Cp for both the A and the B sides
   of the pitot tube. Does the average deviation come within the Volume III
   criteria?
3. From the data in 1, calculate CP(A)-CP(B). Does the value meet the Volume
   III requirements?
4. It is highly recommended in  Volume III that an ASTM reference thermometer
   be purchased for thermometer and thermocouple calibrations. What would be
   the number of an ASTM thermometer that could be used for such calibrations?
                        or
   The calibration of temperature sensors is a relatively simple task, but Bob often
   neglected it. How would he compare a thermocouple's response to that of an
   ASTM reference thermometer at a temperature of 2SO°C?
   a. use boiling water
   b. use crushed ice in Dewar flask
   c. calibrate it at the stack
   d. use cooking oil
   Orsat values that are high compared to a standard indicate:
   a. leaking valves.
   b. spent absorbing reagent.
   c. poor operator technique.
   d. a worsening greenhouse effect.
                                    127

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7. In the analysis being performed in the figure below, what should the average Ot
   value for three replicates be?
        Reference mark
     CO
  absorbing
   pipette
absorbing
 pipette
   a. 20.9±2%
   b. 20.8±0.7%
   c. 21.5±0.9%
   d. 20.1±0.1%.
                       Leveling bottle


                       Gas bubbling
                       through water
                                                                     Aspirator bulb
SR
                                                       -  Air
                                                       entering
                                                       analyzer
                                        128

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                          Answers to
        Reading Assignment 9 Review Exercises
1, 2, and S.
                         Pilot tube calibration data
Calibration pitot tube: type
Type S pitot tube ID number
Calibration: Hate
sizp (OD)
68 (
, 	 performed
TD number
~(rin = 0.99
hy Carl
A-side calibration
Ap,,,,.
cm (in.)
H,O
0.072 in.
0.065
0.070







Ap,
cm (in.)
H,O
0.116 in.
0.120
0.118







Average
C,(j)"
0.780
0.729
0.762







0.757
DEV*
0.023
0.028
0.005







0.019
      •c.
        '<*>
                 Ap.
      *DEV m C,,,, - C, (must be S 0.01)

       C,(A)-C,(B) = 0.047 (must be £0.01).

       Quality Assurance Handbook M2-2.5
B-side calibration
Ap,,,.
cm (in.)
H,O
0.060 in.
0.060
0.065


Ap..
cm (in.)
HtO
0.120 in.
0.122
0.118


Average
Q(*>"
0.700
0.694
0.735


0.710
DEV*
0.010
0.016
0.025


0.017
                                129

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    The average values of DEV for both the A and the B sides exceed the
    recommended value of 0.01. The value of Cp(A)-Cp(B) = 0.047, exceeds the
    recommended value of 0.01. The calibration requirements for the pitot tube
    are not met and the pitot tube should not be used.

4.  ASTM 63C or ASTM 63F
5.  a  b  c
6.  a  b ^cj d
7.  a (b) c  d
                                    ISO

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      Reading Guidance—Assignment  10
EPA Methods 4, 5, and 6 use dry gas meters for determining volumetric flow
through the sampling train. The discussion on the calibration of the dry gas meter
is the same for Methods 4 and 5 (Sections S.S.2 and S.4.2 in Volume 3). Section
3.5.2 contains some additional information concerning the calibration of the wet
test meter.
  The wet test meter is an  intermediate standard commonly used to calibrate dry
gas meters. Wet test meters are used for this purpose because of their high
accuracy (better than ±1%). However, because of their bulk, weight, and
equilibration requirements, they are seldom used outside a laboratory setting.
  Since it is often difficult  to locate information about wet test  meters, a brief
review of their operation is  given here (abstracted from  APTI Course 435
Atmospheric Sampling—Student Manual EPA 450/2-80-004, September 1980).

Wet Test Meter

The  wet test meter consists  of a series of inverted buckets or traps mounted radially
around a shaft and partially immersed in water (c). The location of the entry and
exit gas ports is such that the entering gas fills a bucket, displacing the water and
causing the shaft to rotate because of the lifting action of the bucket full of air.
The  entrapped air is released at the upper portion  of the rotation and the bucket
again fills with water. As it turns, the drum rotates index pointers that register the
volume of gas passed through the meter (b).
  After the meter is leveled, the proper water level is achieved by using the filling
funnel, fill cock, and drain cock (a) to bring the meniscus of the water in touch
with  the tip of the calibration index point. The calibration gas  should be passed
through the meter for one hour to saturate the water with the gas. The water in
the meter should be at the  same temperature as the surrounding atmosphere. If
any water is added, sufficient time must be allowed for  complete equilibration.
                                    1S1

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             (a)
(b)
(c)
      Calibration point
       for water level
 Drain cock
                 V_
                   Drain plug
  Water manometer


      Thermometer    ^ Rotating partitioned drum


                               Gas outlet


                                Direction of
                                  rotation
                                                                     Water
                                                                      level
                               Gas inlet
                                     Leveling screws
  If a wet test meter is used to measure a dry gas stream, a significant error is
introduced if the measured volume is not corrected to dry conditions. The correc-
tion can be made by using the following expression:
                               V = V
                                •c — v«
Where:    P6 = atmospheric pressure
           Pw = vapor pressure of water at room temperature
           Ve = corrected volume at room temperature
           Vm.M = measured volume at room temperature
  It may be easier, however, to first saturate the test gas stream by passing it
through a bubbler before it enters the wet test meter.
             Begin by reading Section S.3.2—Calibration of Apparatus,
             Method 4. Read pages 1 of 19 through 19 of 19.
  Four methods of checking the initial calibration of a wet test meter are given in
paragraph 2.1.1 on page 1 of 19, Section S.S.2. The second method suggests using
any primary air or liquid displacement method. A spirometer, mercury-sealed
piston, or simple displacement bottle all can be used for this purpose. It may be
difficult, though, to find a large enough displacement bottle to handle the volume
requirements of the wet test meter. The calibration section for Method 6, given in
Section 3.5.2, gives a step-by-step procedure for the displacement bottle method.
                                       1S2

-------
             Read paragraph 2.1.1  of Section 3.5.2 at this point,
             before proceeding with the actual calibration procedures
             for the  sample train. We would like to round out the
             discussion of wet test meters by including that part of the
             Method 6 discussion here.
Calibrating the Sample Meter System
             Now read paragraph 2.1.2, pages 2 of 19 through 12 of
             19 of Section S.3.2—Calibration of Apparatus, Method 4.
The leak-check procedures are, of course, important. Both positive pressure and
vacuum leak checks should be performed before proceeding with the calibration.
  Note that a needle valve will be needed for this calibration method.
  Note that the forms of Figure 2.3A provide for  taking data from AH values of
0.5 to 4.0 in. HtO. Higher values of AH are not routinely encountered in source
testing so a calibration ranging to 4.0 in. HtO will generally be adequate.
  Note on page 11 of 19 of Section 3.3.2, that from steps 7 and 8, each calibration
factor must be within ± 2% of the average Y value. The average Y value does not
necessarily have to be equal to 1.0.
  Note that metric data sheets are provided on page 9 of 19 of Section 3.3.2.
  A post-test calibration check is given on page 11 of 19 of Section 3.3.2.
  Temperature gauges: Briefly review the discussion of calibration techniques for
thermometers used in Method 4. Much of this material is similar to that reviewed
in the discussion of temperature sensors for Method 2.
             Continue your reading with Section 3.4.2—Calibration
             of Apparatus for Method 5.
  This section contains almost identical information to that given in the calibration
section for Method 4. It is not necessary to reread all the material, but do note on
pages 18 and 19 of 22, Section 3.4.2, calibration procedures specific to Method 5
(heater and nozzle calibrations).
             You have completed your reading for Assignment 10. Do
             the review  exercises  which  follow; then  check your
             answers.  The correct  answers  are  given  on the page
             following the review exercises.
                                      1S3

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         Reading Assignment 10 Review Exercises
1 .  In performing a positive leak check of the metering system of a Method 5 train
   before calibrating the dry gas meter, which one of the following preparatory
   steps would not be done?
   a. plug downstream tap of orifice meter
   b. plug inlet to vacuum pump
   c. vent positive side of inclined manometer attached to the orifice meter
   d. place a one-hole stopper with attached tubing to end of orifice meter
2 .  How does one perform a negative leak check on the metering system?
   a. by observing the leakage rate on the  DGM at a vacuum of 75 mm Hg
   b. by observing the leakage rate on the  orifice meter at a vacuum of 75 mm Hg
   c. by observing the leakage rate on the vacuum gauge at a vacuum of 75 mm Hg
3.  When calibrating a Method  5 metering  system against a wet test meter, Carl
   simultaneously calibrated the dry gas meter and orifice meter. When per-
   forming the calibration, what should Carl have set and what should he have
   observed?
   a. He should have set Vd and observed AH and Vw.
   b. He should have set AH and observed V«, and Vw.
   c. He should have set AH and Vw and observed Vd.
   d. He should have set Vw and observed  AH and Vd.
4.  When calibrating a dry gas meter with  a wet test meter the inlet air should be:
   a. at projected stack temperature.
   b. saturated.
   c. the same molecular weight as the projected stack gas.
   d. free of oxygen.
5.  Calculate a value for Y,-, given the following data:
   Pt = 28.63 mm Hg          AH = 0.5 in. H,O
   td=74°F                  t«,= 7S0F
   Y,= __
6.  In order to calculate the value of AH@ for an orifice meter, what additional
   information is needed beyond that given in exercise 5?
   a. K™
   b. 0
   c. Y,
   d. P.
                                     134

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7. Where in Volume III can you find a detailed procedure for calibrating a wet
   test meter?
   a.  Section 5.3.2
   b.  Section S.4.2
   c.  Section S.5.2
   d.  Section 5.6.2
8. Calibration values for Method 5 probe nozzles are obtained by:
   a  taking vendor certified values.
   b.  measuring with a ruler.
   c.  measuring with a micrometer caliper.
   d.  projecting the nozzle area on graph paper and weighing the cut-out pro-
      jected area.
                                      135

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                           Answers to
        Reading Assignment  10 Review Exercises
1.  a  b 0 d
2. 0 b  c
3.  a  b 0d
4.  a 0 c  d
           VWP6
5.  Y,=
                 -  (U + 460)
                 7
                                 5 x 28.63 x (74+ 460)
                             5.036x128.63+-^-) (73 + 460)
                                           13.6/
          5x28.63x534
        5.036x28.67x533
         c  d
                         = 0.993
6.  a ,
7.  a  b 0 d
8.  a  b (?) d
           You have now completed the material for Quiz 1.
             Take Quiz 1  under the direction of your test super-
           visor. (See page 5 of this guidebook for more detailed
           instructions.)
                                 136

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                         Lesson  E
                Presampling Operations
Lesson Goal

The goal of this lesson is for you to be able to properly prepare and pack
calibrated equipment and supplies before conducting a source test.

Lesson Objectives

After completing this lesson, you should be able to:
  1. inspect a Type S pitot tube before taking it into the field.
  2. describe the procedures for checking the Orsat analyzer before a field test.
  3. describe proper packing methods for source sampling equipment, including
     probes, glassware, and chemicals.
  4. consider the utility of using a detailed packing list.
  5. describe the procedure for checking filters used in Method 5.
  6. effectively use an activity matrix for presampling preparation.

Materials

Assignment 11
  • Section S.I.3—Presampling Operations in Section 3.1,
    Method 2—Determination of Stack Gas Velocity and Volumetric Flow Rate
  • Section 3.2.3 —Presampling Operations in Section 3.2,
    Method 3 — Determination of COt, O», Excess Air, and Dry Molecular Weight
  • Section 3.3.3—Presampling Operations in Section 3.3,
    Method 4—Determination of Moisture in Stack Gases
  • Section 3.4.3 —Presampling Operations in Section 3.4,
    Method 5—Determination of Paniculate Matter from Stationary Sources
  • Activity matrix given on page 5 of 6, Section 3.5.3 in Section 3.5—
    Presampling Operations, Method 6—Determination of Sulfur Dioxide
    Emissions from Stationary Sources
  • Activity matrix given on page 8 of 9, Section S.6.S in Section 3.6—
    Presampling Operations, Method 7—Determination of Nitrogen Oxide
    Emissions from Stationary Sources
                                   137

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      Reading  Guidance—Assignment  11
The figure below is taken from APTI Course 450 Source  Sampling for Particulate
Pollutants—Student Manual,  Aldina, GJ. and Jahnke, J.A., December 1979 EPA
450/2-79-006. It provides an overview of much of what we have studied in Volume
III so far.
                              DETERMINE NECESSITY' OF A SOURCE TEST
                               •Decide on data required
                               •Determine that tource tat will give thii data
                               •Analyze cost
                              STATE SOURCE TEST OBJECTIVES
                               •Process evaluation
                               •Process design data
                               •Regulatory compliance
                              DESIGN EXPERIMENT
                               •Develop sampling approach
                               •Select equipment to meet test objectives
                               •Select analytical method
                               •Evaluate possible errors or biases and correct
                                sampling approach
                               •Determine manpower needed for test
                               •Determine time required for test with margin for
                                breakdowns
                               •Thoroughly evaluate entire experiment
                                with regard to applicable Sole and Federal
                                guidelines
tives and
                              PRE-SURVEY SAMPLING SITE
                               •Locate hotels and restaurant! in area
                               •Contact plant personnel
                               •Inform plant personnel of letting objecti
                                requirements for completion
                               •Note shift changes
                               •Determine accessibility of sampling site
                               •Evaluate safety
                               •Determine port locations and application to
                                Methods I and 2 (12/23/71 Federal Register)
                               •Locate electrical power supply to lite
                               •Locate renrooms and food at plant
                               •Drawings, photographs, or blueprints of sampling site
                               •Evaluate applicability of sampling approach from
                                experiment design
                               •Note any special equipment needed
                 RESEARCH LITERATURE
                   •Basic process operation
                   •Tvpe of pollutant emitted
                   from process
                   •Physical state at source
                   conditions
                   •Probable points of emission
                   from process
                   •Read sampling  reports
                   from other processes
                   sampled:
                    1. Problems to expect
                    2. Estimates of variables
                       a. H2<5 vapor
                       b. Temperature at
                        source
                   •Study analytical pro-
                   cedures used for
                   processing test samples

CALIBRATE EQUIPMENT
•DGM
•Determine console AHfi
•Nozzles
•Thermometers and
thermocouples
•Pressure gages
•Orsat
•Pilot lube and probe
•Nomographs




FINALIZE TEST PLANS
•Incorporate prenirrey into experiment design
•Submit experiment design for ap-
proval by Industry and Regulatory Agency
•Set test datet and duration
j 	
PREPARE EQUIPMENT FOR TEST
•AaMinUe and confirm operation
•Prepare for shipping
•Include spare para asvi reserve equipment
1
CONFIRM TRAVEL AND SAMPLE TEAM ACCOM-
MODATIONS AT SITE
•
CONFIRM TEST DATE AND PROCESS OPERATION
•Final step before travel arriving at site


PREPARE FILTERS AND
REAGENTS
•Mark fillers with insoluble
ink
•Desiccate to constant
weight
•Record weights in per-
manent laboratory file
•Copy file for on site record
•Measure deionized distilled
HjO for impingcrs
•Weigh silica gel
•Clean sample storage
containers

                                               1S9

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  Remember that Section 3.0 (Sections 3.0.1 and 3.0.2) in the beginning of
Volume III discusses planning the test program and general factors involved in
source testing. A number of points discussed there bear on pretest preparation
discussions for the individual methods. You may wish to go back and briefly review
the contents of Section 3.0 before proceeding with this reading assignment.
             Read the Presampling Operations sections for Methods 2
             through  5.  Since  much of the material repeats, just
             review the Activity Matrices for Presampling Operations
             for Methods 6 and 7. Begin your reading with Section
             3.1.3 —Presampling Operations, Method 2. Read pages
             1 of 7 through 3 of 7.
  Note the various pretest preparation check forms provided for each of the
reference methods. The preparedness of a test team can be evaluated by noting
how completely these forms are filled out.
             Continue your reading with Sections 3.2.3, 3.3.3, and
             3.4.3 —Presampling Operations for Methods 3, 4, and 5.
  Paragraph 3.1.3 on page 3 of 6 of Section 3.2.3 is important. Before going to
the field, care should be taken that the absorbing solutions have not deteriorated.
  The presampling operations section for Method 5 contains a packing list starting
on page 3 of 20, Section 3.4.3.  This listing points out the many tools and spare
parts that a test team may need under the actual conditions at a source. The
listing has been derived from the experience of many stack testers over a period of
several years. It is inclusive for the reference methods performed by the professional
stack tester. Although all of the materials listed will not be needed for any one test,
the pack sheet allows you to consider taking the items which might otherwise be
forgotten.
  Carefully read the discussion on Method 5 filters, on page 16 of 20,
Section 3.4.3.
             Since you have already read information on presampling
             operations for probes, glassware, etc., for Methods 6 and 7,
             just review the activity matrices. For Method 6, the activity
             matrix is given on page 5 of 6, Section 3.5.3, Table 3.1.
             For Method 7, the activity matrix is given on page 8 of 9,
             Section 3.6.3, Table 3.1.
                                      140

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            If you are not familiar with the procedures for the prepara-
            tion of reagents used in Methods 6 and 7 sampling, read
            Subsection 3.2 Reagents on page 3 of 6, Section S.5.S for
            Method 6 preparations and Subsection 3.2 Reagents on
            page 4 of 9, Section 3.6.3.
            You have completed your reading for Assignment 11. Do
            the  review  exercises  which follow;  then check your
            answers. The correct answers are given on the page
            following the review exercises.
         Reading Assignment  11  Review Exercises
1.  An inspection of a Type S pilot tube before a test primarily incorporates:
   a. a visual check for damage and misalignment.
   b. the measurement of R, Pe, and A.
   c. the measurement of y, 6, and w.
   d. a check of vendor's C, certification form.
2.  True or False? Since pitot tubes and thermocouples are not fragile like glass
   probes are, they can just  be thrown in back of the van when going out on a test.
3.  List the four steps that should be taken in preparing an Orsat analyzer before use.
   a. 	
   b. 	
   c.
   d.
   SST lucked out and got a job in Hawaii. How should Mike ship the Orsat?
   a. He should put it assembled in a cardboard box and stuff paper around it.
   b. He should ship it by freighter.
   c. He should disassemble it and pack each item individually into a rigid
     container.
   d. He should carry it (assembled) with him and put it under the seat of the
     airplane.
                                    141

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5. Indicate whether or not each of the following items is noted in the packing list
   in Section 3.4.S (Method 5)?
        Yes    No
   a.  	  	    first aid kit
   b.  	  	    ice chest
   c.  	  	    tool box
   d.  	  	    calculator
   e.  	  	    glass wool
   f.   	  	    duct tape
   g.  	  	    Method 5 meter box
   h.  	  	    hard hat
   i.   	  	    500-ml graduated cylinder
6. The procedure for checking Method 5 filters is to:
   a. perform an ASTM burst test on the filter material.
   b. determine the tensile strength of 1 in. X 5 in. strips.
   c. visually check each filter for flaws or leaks.
   d. use them and see if they work.
7. True or False? It is not necessary to desiccate filters before a test since they will
   be measured at ambient conditions anyway.
8. Turn to page  5 of 6, Section S.5.3—The Activity Matrix for Presampling
   Operations,  Method 6. At this stage  of the source test, what is the predominant
   activity if acceptance limits are not met?
   a. repair or replace
   b. recalibrate
   c. return  to manufacturer
   d. repeat  the procedures
                                      142

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                           Answers to
        Reading Assignment 11 Review Exercises
1. (a) b   c  d
2.  False. Care must be taken not to damage pitot tube or thermocouple tips.
3   a   check fluid levels	
    jj   clean stopcocks	
    c   change absorbing solutions if necessary
        check for leaks
4.  a  b (cj d
5.     Yes      No
    a. _x_    	
    b.  x      	
    c.  x      	
    d. 	     x



    h.  x      	

6.  a  b (c)d
7.  False. Must desiccate to a consistent moisture level.
8. (T) b  c  d
                                 14S

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Sampling  and  Analysis
     Lesson F—On-site Measurements
             Reading Assignment 12
             Reading Assignment 13
     Lesson G —Postsampling Operations
             Reading Assignment 14
             Reading Assignment 15
                145

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                         Lesson  F
                 On-site Measurements
Lesson Goal

The goal of this lesson is for you to understand the quality assurance checks and
procedures that can be followed while conducting a source test.

Lesson Objectives

After completing this lesson, you should be able to:
    1.  use an on-site checklist to see if proper procedures are followed in a test
      method.
    2.  list at least three special precautions that should be taken when using a Type
      S pitot tube.
    S.  state when an Orsat analyzer is to be leak checked and state the criterion for
      repeating analyses.
    4.  list at least three special precautions that should be taken when performing
      Reference Method 5 for emission rate factor or excess air calculations.
    5.  state the conditions for an acceptable Reference Method 4 sample run.
    6.  discuss precautions that should be observed when determining the isokinetic
      sampling rate using a nomograph.
    7.  explain how filter blanks are used in Reference Method 5.
    8.  describe the leak-check procedure for a Reference Method 5 sampling train.
    9.  describe the probe-rinsing procedure outlined in Volume III—Section S.4.4.
  10.  describe the sample-recovery procedure used in Reference Method 6,
      including the handling of blanks.
  11.  outline the evacuation-purge-sampling procedure followed in Reference
      Method 7, and state the leak-rate requirements.

Materials

Assignment 12
  • Section 3.1.4, On-site Measurements in Section 3.1
    Method 2—Determination of Stack Gas Velocity and Volumetric Flow Rate
  • Section 3.2.4, On-site Measurements in Section 3.2
    Method S—Determination of CO2, Ot, Excess Air,  and Dry Molecular Weight
  • Section 3.3.4, On-site Measurements in Section 3.3
    Method 4—Determination of Moisture in Stack Gases
                                   147

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Assignment 13
  • Section 3.4.4, On-site Measurements in Section 3.4
    Method 5—Determination of Paniculate Matter from Stationary Sources
  • Section 3.5.4, On-site Measurements in Section 3.5
    Method 6—Determination of Sulfur Dioxide Emissions from Stationary Sources
  • Section 3.6.4, On-site Measurements hi Section 3.6
    Method 7—Determination of Nitrogen Oxide Emissions from Stationary Sources
  • Optional: Section 3.7.4,  On-site Measurements in Section 3.7
    Method 8—Determination of Sulfuric Acid Mist and Sulfur Dioxide Emissions
    from Stationary Sources
                                      148

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      Reading Guidance—Assignment  12
             Begin by reading Section 3.1.4—On-site Measurements
             for Method 2. Read pages 1 of 12 through 12 of 12.
 Paragraph 4.2 outlines Reference Method 2 procedures. Note that the data form of
 Figure 4.1 provides spaces for each parameter that will be needed to determine the
 stack gas velocity, v,. Also note the section of the form used for recording data
 from the cyclonic flow determination.
   The material in paragraph 4.2.1 on page 3 of 12 was not discussed in this
 amount of detail in the explanation of Reference Method 1 (Volume III—Section
 3.0 General Aspects, page 10 of 19). Note the two methods of measuring stack
 dimensions, and the problems that can occur with non-uniform dimensions and the
 buildup of particulate matter in ducts.
   On page 5 of 12, paragraph 4.2.3,  note the procedures given for checking for
 plugging of pitot tube openings.
   Paragraph 4.2.5 on page 7 of 12 gives a number of common sense techniques
 that can be followed to help you  perform Reference Method 2. Item 2 of this
 paragraph is particularly important, since a maximum response does not corre-
 spond to the pitot tube impact opening being aligned with the direction of flow
 (0=0° yaw). See Figure 2.6 in Section 3.1.2,  page 10 of 21.
   Paragraph 4.2.6 gives a number  of methods for measuring static pressure. You
 should be aware that in all Reference Method calculations, the static pressure is
 used on an absolute basis. For example, if the barometric pressure is 29.82 mm Hg
 and the stack static pressure was found to be  - 2.0 in. of H»O, then the value used
 in subsequent calculations would be

                            P  — P  j.   *   —
                            ii~-n"+ 15.6 ~

                                = 29.82-A?_
                                         13.6
                                = 29.67
You can see that for the small static pressures normally encountered in stack tests
(except near fans, Venturis, etc.), errors in this measurement have limited effect on
final calculations.
  The on-site measurements checklist shown in Figure 4.2 (page 10 of 12) can be
used to see if proper procedures are followed when performing the reference
method. This form, used in conjunction with the Activity Matrix of Table 4.1, can
help to check the performance of the  tester.
                                    149

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             Continue  your  reading with  Section  3.2.4 —On-site
             Measurements for Method 3. Read pages 1 of 12 through
             12 of 12.
  Note in paragraph 4.1,  the three methods of obtaining a sample for subsequent
Orsat analysis:
    •  single-point grab sampling and analysis
    •  single-point integrated sampling and analysis
    •  multipoint integrated sampling and analysis
Each method has its purpose. The significant point is that the Orsat method can
be used to determine
    1. dry molecular weight
    2. Oz concentrations  for F factor emission rate calculations
Standards requiring an F factor emission rate calculation generally specify that a
multipoint integrated sample be obtained for Orsat analysis.  For example, in
40 CFR 60 Subpart D for  fossil-fuel-fired steam generators,
    "the oxygen sample shall be obtained simultaneously by  traversing the
    duct at  the same sampling location used for each run of Method 5"
    (paragraph 60.46 fSi)
  When reading paragraph 4.1, pay particular attention to the leak-check and
purging procedures for the sample bags.
  Read paragraph 4.2.2 carefully. Note the leak-check requirements and the con-
ditions for accepting the data. When obtaining an integrated, multipoint sample,
the source tester should be sure to turn off the sample pump to the bag (if one is
used)  before switching ports. Not doing this is a common blunder and leads to the
dilution of the sample with ambient air.
  Note the special precautions that should be taken with the Orsat analyzer. These
are discussed in paragraph 4.3. An article has been written on collaborative field
studies using the Orsat analyzer. The article contains points that can supplement
Section 3.2.4. See Mitchell, W.J. and Midgett, M., "Field Reliability of the Orsat
Analyzer"/  Air Pol. Control Assoc. 21:491-495.  1976.
  Many of the problems associated with the Orsat analyzer stem from operator
error. Proper training and experience are essential if one is to obtain quality data
from this deceptively simple analytical method.
             Continue your reading with Section 3.3.4—On-site Meas-
             urements for Method 4. Read pages 1 of 10 through 10 of 10.
  Note again the on-site measurements checklist. This is given on page 2 of 10 and
provides a handy means of seeing if proper procedures were followed during the
test.
                                      150

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  Note, in paragraph 4.2, the specification of the sampling time and sampling
rate. A sampling rate of 0.75 ftVmin corresponds merely to maintaining the
system at a AH value near the AHe of the meter box.
  Paragraph 4.2.4 gives the procedures for sampling at a constant rate. Note that
item 12 on page 7 of 10 recommends that the volume taken at each point not differ
by more than ±10% from the average sample volume for all points.
            You have completed your reading for Assignment 12. Do
            the review exercises which follow and check your answers
            after you complete them. The correct answers are given
            on the page following the review exercises.
         Reading Assignment 12 Review Exercises
 1.  SST got a job to do a stack test at Superior Light and Power Co. The ports
    were located on the stack, which had a diameter of about 40 feet at that point.
    Jeff, a new member of the team, was given the job of determining the stack
    dimensions. What would be the best way of doing this?
    a. Get a 40-ft-long piece of Unistrut® insert it into the port,  and mark it off.
    b. Go to the woods  next to the plant, get a 40-ft-long tree, and do the same
      thing.
    c. Measure the outside circumference of the stack and correct for the wall/
      insulation thickness.
    d. Obtain stack blueprints from the plant engineer and read the dimensions
      from them.
 2.  Jeff inserted the pitot tube into one of the four ports at the sampling location.
    In starting the velocity traverse, he rotated the probe (yaw axis) and found that
    he could get a maximum reading on his manometer by doing this.  How should
    he proceed?
    a. He should obtain the maximum Ap value at all points of the traverse
      because Ap is at  a maximum at 0° yaw angle.
    b. He should align the probe with reference to the stack geometry if it is deter-
      mined that cyclonic flow is absent.
    c. He should align the probe to obtain maximum Ap values since the flow
      would be cyclonic.
    d. He should not use the Type S probe. He should use a Fecheimer probe for
      this particular condition.
                                    151

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S. Jeff needed to determine the stack static pressure. The static pressure was
   obviously negative because a piece of paper would quickly be sucked into the
   stack. However, when he stuck a straight tube into the port to determine p,, he
   found a pressure differential fluctuating around zero, with no more of a meter
   reading than —0.5 in. HZO. What could have been the problem?
   a.  He didn't stick the tube in far enough.
   b.  He didn't plug the port.
   c.  The cyclonic flow was creating the condition.
   d.  No problem. That's the way it was and should be recorded as such.
4. The Orsat analyzer must be leak checked before and after analysis for which
   method(s) listed below?
   a.  determination of gas composition for emission rate factor determinations
   b.  determination of gas composition for stack gas molecular weight calculations
   c.  determination of gas composition for excess air correction factors
5. When obtaining the integrated sample for subsequent Orsat analysis, Jeff had
   to  change ports four times. He hooked up  a separate probe on the side of the
   Method 5 probe  and used a separate pump to obtain the Orsat sample during
   the traverse. When switching ports, he turned off the pump for the meter box,
   but forgot about the pump for the Orsat sample. How would this affect the
   data?
   a.  The emission rate data would be higher than true.
   b.  The emission rate data would be lower  than true.
   c.  There would be no effect.

6. Three analyses are to be made of each Orsat sample. Which of the following
   would be true if the data were to be used in an F factor calculation?
   a.  repeat until any three CO» analyses differ by  15%
   d.  repeat until any three molecular weight mean values differ by  
-------
 8. A M  hod 5 meter box was used for a stack gas moisture determination. The
    AHg of the orifice meter was 1.83 in. H»O. What should the AH of the system
    be while running Method 4?
    a.  variable—adjusted to the isokinetic rate
    b.  variable—proportional to stack gas velocity
    c.  constant at any arbitrary value
    d.  constant near 1.83 in. H2O
 9. The volume taken  at each point of a Method 4 traverse should be within
    ±	of the average sample volume for all points.
    a.  2%
    b.  5%
    c.  10%
    d.  20%
10. What are the leak-rate requirements for a Reference Method 4 test?
    a.  The leak rate must be less then 2% of the average sample rate.
    b.  There are no leak-rate requirements, since sample dilution will not affect
       the results.
    c.  The leak rate must use less than 4% of  the average sample rate.
    d.  The leak rate must be greater than 4%  of the average sample rate.
                                     155

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                          Answers to
       Reading Assignment 12 Review Exercises
                    since E = Frfc,
                                 20.9-%0,
                         %OZ would be higher than true,
                         (20.9- %Oj) would be too low, and
                         therefore E would be higher than true

 7.  •   Do not allow ambient air to enter analyzer.	
    •   Follow proper sequence—Ot, COt, CO.	
    •   Saturate indicating solution with salt.
    •   Keep absorber solution from manifold.
    •   Allow 5 minutes for samples to come to temperature.
    •   Operate at constant temperature and pressure.	
 8.  a  b   c
 9.  a  b (c) d
10.  a  b
                                 154

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      Reading  Guidance—Assignment  13
                Begin by reading  Section 3.4.4—On-site Measurements
                for Method 5. Read pages 1 of 19 through  19 of 19.
Performing a source test for paniculate matter involves the techniques of Reference
Methods 1-4. The many procedures to be done require both  planning and coor-
dination. The figure below* shows how  these procedures are  interrelated, and may
help you review Section 5.4.4, On-site Measurements for Reference Method 5.
\KKI\ \l \ I  SI I I

 •\olllt pljlll jilfl

  it vol'imf* JIM'!'* %
  |N |*UIIII I
 •K.\l.» II-M  |>|JII Ollll 4ll
  nimrrm-it
 •( littk. »rjthrr forrutu
 •( (infirm |iriK«-« II|H rjlioll
  |).ii.niii l*-r* in iiinniil riMim
RKORl) Al.l. INFORMA-
TION ON I>AI A SHEETS

  •Stimuli1 tjw number
  •MuiT rtinwlc number
  •Pr«l>f leniflh

  •Niillle diameter
  •C Iatlor
  •A»umi-d HoO

  •Olix-r\rr* prewnl
  • I rjin U-jk ICM rju-

  •Inuul IX.M dul readmip
                        •«-
      1 \Kh IN I K.KAI HI
      SXMI'I I Or SI XCKCAS
      rOKOKNXl \\ALYSIS \ and temperjlure
                                 •Record duct *tatic preuure
                               USE NOMOGRAPH OR CALCULATOR TO SIZE
                               NOZZLE AND DETERMINE C FACTOR
                                 •Adjuu for molecular weight and pitoi tube C
                                 •Set K pivot point on nomograph       ^
                               LEAK TEST COMPLETELY ASSEMBLED
                               SAMPLING TRAIN fil5" Hg VACUUM AND
                               MAXIMUM LEAK RATE OF 0.02 CFM
                                             =T
                               NOTIFY ALL CONCERNED THAT TEST IS ABOUT
                               TO START
                                                                    IU Tt.RMIM APPKOX.
                                                                    IMA It MOI K II AR
                                                                    WHC.II 1 (It SIAC.k (.AS
                                                                    I'SIV. IVRI 1 t AND
                                                                    NOMO(.HAPIIS
                                                                    APPKOXIMAIt lt',0
                                                                    VAPOR (.OM'rNIOf
                                                                    S 1 AC k (.AS
                              I CONFIRM PROCESS OPERATING PARAMETERS
                         START SOURCE TEST

                           •Record start time - miliurv bate
                           •Record gat veloctt*
                           •Determine JH desired from nomograph
                           •Start pump and set orifice meter
                           differential manometer 10 desired AH
                           •Record
                              1. Sample point
                              2. Time from lero
                              3. DCM dial reading
                              4. De*ircd AH
                              5. Actual AH
                              6. All temperature* DCM, stack, sample taw.-
                           •Maintain isokinetic AH at all time*
                           •Repeat for all poinu on traverse
                                                                         MOM 1 OK PK«( MS K M I
                                                                          1 \kl SI \l rKI M
                                                                         SAMIM rs II M< tssxm
                                                                    1 \kl (OS I KOI ROOM
                                                                    IIU \
                               AT CONCLUSION OF TEST RECORD

                                •Stop time - 24 hour clock
                                •Final DGM
                                •Anv pertinent observations on sample
                               LEAK TEST SAMPLE TRAIN
                                •Test at highest vacuum (in. Hg) achieved during test
                                •Leak rale should not exceed 0.02 CFM
                                •Note location of ant leak if possible
                               REPEAT PRECEDING STEPS FOR THREE
                               PARTICULATE SAMPLES
    •Abstracted from Aldina. G.J. and Jahnke, J.A., 1979, APTI Course 450 Source Sampling for
     Paniculate Pollutants—Student Manual.  EPA 450/2-79-006. Pages 5.4 to 5.5
                                               155

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  Preliminary data on temperatures, pressures, etc. are used to set up the
nomograph. A data form that can aid in this set-up is given on page 3 of 19. The
nomograph for Reference Method 5 was developed in the early 1970s—before
hand-held calculators were widely available. At that tune, it enabled the stack
tester to quickly perform the lengthy calculations for the nozzle diameter, Dn, and
the isokinetic sampling rate.
  Today, hand-held programmable calculators are available and relatively
inexpensive (although a simple calculator with the basic math  functions and a
square root function is all that is actually needed). Numerous types of plastic slide-
rule calculators that will do these two calculations have also been developed. The
reference method does not specify that the Method 5 nomograph is required. The
tester may use either a calculator, a nomograph,  or a slide rule—it is most often a
matter of personal preference. However, it should be determined that the tester
knows how to use the calculation instrument that he chooses. The test observer or
auditor should ask the person doing these calculations to work an example problem
before the test. Any discrepancies between the known answer and the one
calculated should be resolved. Such  example problems are given in APTI Course
450 Source Sampling for Particulate Pollutants—Student Workbook, 1979. EPA
450/2-79-007, pages  53  and 57.
  Again, leak-check  procedures are very important. Read paragraph 4.2.5 care-
fully (pages 5 of 19 through 7 of 19). A common blunder of the novice j^tack tester
is improperly releasing the vacuum at the end of the leak test. If care is not  taken,
water from the impingers will back up onto the filter and the system will have to
be set up again.
  Note that a leak check is mandatory only at the end of the test.  However, the
pretest leak check is recommended,  since it might save a test if a major leak can be
detected before the testing is started.
  On page 9 of 19, paragraph 4.2.6, the nomograph is again  discussed. Note the
assumptions inherent in the nomograph. If the Cp and M, values are beyond the
limits recommended  here, corrections to the nomograph values can be made.
Equations for correction factors are  given in APTI Course 450 Source Sampling for
Particulate Pollutants—Student Workbook, 1979. EPA 450/2-79-007, page 56.
  Paragraph 4.3.1 on page 10 of 19 contains a very important point which should
be included in any quality assurance program. This is the use  of the filter blank.
The reference method itself does not require that filter blanks be saved and this
has normally not been a procedure followed by testing teams.  It might be thought
that weighing filters is a simple procedure  and that errors from the analytical
balance determinations would be small. Weighing, however, is a tedious proposi-
tion and mistakes in  weighing frequently occur.
  Also, problems with high humidity or with the transport of  the filters may raise
questions about the actual mass determination of the Reference Method 5 sample.
Setting aside three tared filters at the beginning of the test, and treating them as
actual sample filters throughout the test, provides an excellent quality control
check of the gravimetric procedures.
                                     156

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    Cleaning the sample train is  a very important part of Reference Method 5.
 Recent studies indicate that over 50% of the paniculate catch can end up in the
 probe and  not on the filter. For this reason, as much care should  be taken with the
 probe-washing procedures as with  the handling of the filters. An outline of the
 cleaning procedure is provided below to supplement the discussion of paragraph
 4.3,  pages  10 of 19 through 14 of  19.
    A good article on Method 5 clean-up procedures has been written—see Riley,
 C.E., July 1975.  EPA Method  5 Sample Clean-up Procedures. Stack Sampling
 News Vol.  5 No. 1  pp 4-7.
                                                               Toting completed
                                                                     _L
                                                     Perform final leak check on sampling train
                                                     with lacuum 2 t«t vacuum  Leak rate man
                                                     be £ 0.02 cfm.
                                       Inipect umple and record obiervatiom
  Impinger water color
  and turbiditv
                Filler appearance
                             Appearance of probe
                             and all other glauware
                                     Allow hot probe
                                     to cool sufficiently
                               Disassemble lampling train (log all information in test log)
           J_
                                                     i
    Cap nozzlr to prevent
    paniculate lou.
  1. Clean nozzle exterior
    first.
  2. Be sure cap will not
    melt to nozzle.
  3. Be sure paniculate
    Mill not mck to cap
                Separate
                probe and filter
        I   Remove impmgrr HyO     J
 Clean probe exterior
                Cap
                probe
                end
                               _L
                                   1
                  Cap filler
                  inlet and
                  outlet
                              Disassemble
                              filter
                                   J_
Bio* out
pilot tubes
Wash excess
duM off probe
sheath and
nozzle
 Careful]* remove nozzle
 and probe end caps
 Do not allow pani-
 culate to be lost
                                            Take volume then More
                                            in marked container
           Additional analysis
           optional
                                             Organic-Inorganic
                                             extraction
                                                         Store silica gel
                                                         in the same container
                                                         it was originally
                                                         weighed in
                                  [    Weigh to nearest 0.5 g     |
Filler mat placed in
clean, tared
weighing dish
Glau components air
scrubbed thoroughly with
acetone washings added
to tared probe wash beaker
              Desiccate for 24 hours
              over 16 mesh calcium
              sulfate or other
              anhydrous desiccant
 Clean probe with noizle
 in place using acetone
 and brush attached to
 stainleu steel or teflon
 handle
           _L
 Brush entire length of
 probe with acetone a S
 times into marked
 container or clean,
 tared beaker
 Remo\e nozzle and inspect it
 and probe liner
           _L
                                             i and record
                        1  Desiccate for 6 hours
                                    I
                          Weigh and record.
                          Continue to constant weight -
                          weights differ SO.5 mg
           Clean probe liner again until no
           sign of particulates can be seen in the
           acetone or on the glass
                                 Clean nozzle by rinsing with acetone
                                 I. Brush interior from blunt back ride only.
                                 2. Never force brush into sharp nozzle end;
                                   bristles will be cut contaminating sample.
                             All washings (filter glassware included)
                             added to clean, marked, tared beaker
                             Evaporate acetone at room temperature
                             and pressure
                             Desiccate and weigh to constant weight
                             as with filter
                                                   157

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  The on-site measurements checklist provides a convenient means of seeing if
many of the procedures involved in a Reference Method 5 test were performed.
This may be useful for the test observer or for the test team leader checking the
performance of his crew.
             Continue  your  reading with  Section  3.5.4—On-site
             Measurements for Method 5. Read pages 1 of 12 through
             12 of 12.
  Paragraphs 4.1 and 4.2 of Section S.5.4 are fairly straightforward. The notes
and comments given in paragraph 4.S, Sampling, should be read carefully.
  A leak-check procedure for the assembled sampling train is given in paragraph
4.S.2. The figure below is provided  to assist you in your reading.

       Vacuum gauge
                   Reference Method 6: sample train leak check.
                                     158

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  Paragraph 4.S.3 discusses sampling at a constant rate. Sampling for Sd is con-
ducted at a constant rate—not proportionally or isokinetically. The sample volume
at each reading interval should be within ±10% of the average sample volume for
each interval.
  During sampling, SOS hi the flue gas is scrubbed from the gas stream by the
80% isopropyl alcohol in the first midget impinger. The SOj passes through the
first impinger and is oxidized by the HjOz in the second and third impingers by the
following reaction:
                        SO,
                       Sulfur
                       dioxide
Hydrogen
 peroxide
-  H,SO4
    Sulfuric
     acid
             Continue  your  reading with  Section 3.6.4—On-site
             Measurements for Method 6. Read pages 1 of 11 through
             11 of 11.
  Reference Method 7 requires careful attention to both sampling and analytical
details. The following seven figures will help you follow the discussion on sampling
procedures given on pages 2 of 11  through 6 of 11, paragraph 4.3.3.
                    Flask valve
                 (evacuate position)
                                                     - Manometer
                    Pump valve
                  (evacuate position)
                                                                          To
                                                                       atmosphere
                                                      Pump to
                                                    < 3.0 in. Hg
           Reference Method 7: evacuate flask. Paragraph 4.3.3, lubparagraph 1.
                                      159

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                    Flask valve
                (evacuate position)
                                                      PA
 Pump valve
(vent position)
                                                         Pump off
Reference Method 7: initial leak check. Paragraph 4.3.3, subparagraph 2.
           L—L
           LJL
                             Flask valve
                          (purge position)
                                                 Pump valve
                                               (purge position)
                                                                  Pump off
Reference Method 7: purge. Paragraph 4.3.3, tubparagraphs 4, 5, and 6.
                                160

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*£=
~




J_J


Flask valve
( • • \
evacuate position)
1
' }
PB






jV
!
r
s
I
£
s
i
^




1
M


                                            Pump valve
                                           (vent position)
                                                             Pump off
Reference Method 7: final leak check. Paragraph 4.3.5, tubparagraphs 8 and 9.
                            Flask valve
                          (sample position)
                                                                   Manometer
     Pump valve
(intermediate position)
                                                                 Pump off
      Reference Method 7: sampling. Paragraph 4.3.3, tubparagraph 10.
                                   161

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     Flask valve
   (purge position)
Reference Method 7: sample recovery.
Paragraph 4.3.3, subparagraphs 11 and 12.
                                          Flask valve
                                      (evacuate position)
Reference Method 7: final pressure check.
                     Paragraph 4.4.1.
                          Optional Assignment
         The procedures for Method 8 are similar to those for
         Method 5. You may continue reading Section 3.7.4, On-site
         Measurements—Determination of Sulfuric Acid Mist and
         Sulfur Dioxide Emissions from  Stationary Sources on
         pages 1 of 18 through 18 of 18.
         You have completed your reading for Assignment 13. Do
         the review exercises which follow and check your answers
         after you complete them. The correct answers are given
         on the page following the review exercises.
                                  162

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        Reading Assignment 13 Review Exercises
1. Using your Reference Method 5 nomograph, Method 5 slide rule, or calculator,
   compute the isokinetic sampling rate (AH), if the Ap at the first test point is
   found to be 1.0 in. HZO. The following calibration factors and stack
   parameters were determined before sampling:
                     0^ = 0.75 cfm
                     AHe=1.85
                     Pitot tube C, = 0.85
                     tm = 80°F
                     Pm = SO.O in. Hg
                     P. = 29.6 in. Hg
                     3^ = 0
                     Bw, = 0.12
                     t, = 280°F
                     Md = 291b/lbTnole
                     Average Ap = 0.80 in. H,O
   Note: The following expressions can be used in this problem:
                    Nozzle Diameter Selection Equation

                       DB=1
                 Isokinetic Rate Equation—Working Form
               AH =
                                      -*M'
846.72DB«AHfflC,'(l-BWI)
                       Answer: AH = _ in. HtO
Ap
2.  Mike assembled the sampling train, but didn't bother to perform a leak check
   until after the test. After the test, he found a leak rate of 0.10 ftVmin. Answer
   the following questions:
   a. Is the test acceptable?  _	yes  	no
   b. Was the actual test performed isokinetically if the calculated AH values
     were set at each point?  	yes  	no
   c. Would he be able to  correct the final metered volume for the leak?
     	yes  	no
   d. Would he be able to  correct the weight of the collected paniculate matter
     for the leak?  	yes  	no
                                   165

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3. Under which of the following conditions is the use of the nomograph valid
   without compensating for nomograph assumptions?
   a.  C, = 0.79
   b.  Cp = 0.84
   c.  Md = 27.5
   d.  Md = 24.1
   e.  Q, = 0.87
4. The three filter blanks mentioned in paragraph 4.S.I on page 10 of 19
   (Section 3.4.4) should be:
   a.  saved so that they can be used to replace a filter if it gets wet during the
      leak check.
   b.  left in the desiccator in the lab.
   c.  transported along with the sample filters and weighed again at the end of
      the test.
   d.  weighed only at the end of the test, so the balance can be checked.
5. In the Method 5 sample recovery procedures, the probe should be:
   a.  rinsed only once since more rinsings waste time and  contribute to greater
      error because of increased amounts of solvent.
   b.  rinsed only once since the bulk of the paniculate matter is caught on the
      filter and any probe losses would be unimportant.
   c.  rinsed with soap and water so that it will be really clean before the next
      test.
   d.  rinsed with acetone more than three times so that all the particulate matter
      can be collected.
6. Look  at Figure 4.5 on pages 15 of 19 through 17 of 19  in Section  3.4.4 (or
   Figure 4.5 on pages 6 of 15 through  8 of 15 in Section 3.4). An agency observer
   noticed a number of things listed below. Make believe that you are the observer,
   and check off the points in Figure 4.5.
   a.  A glass liner was used.
   b.  The pitot tube coefficient was assumed to be 0.84.
   c.  One of the filters used had a tear.
   d.  The test  team had only a Vi-in.  nozzle at the site.
   e.  The pitot tube lines were checked for leaks.
   f.  A calculator was used for the isokinetic rate determinations.
   g.  Only time and volume data were put on the sampling form (Figure 4.2);
      other data were written on a note pad.
   h.  Clean-up was performed at the sampling site.
   i.  Some filter paper was left on the silicone gasket.
   j.  Probe-wash bottles were labeled  with labels similar to Figure 4.3.
                                    164

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 7. In the leak-check procedure for the Reference Method 6 assembled sampling
    train:
    a. the leak rate is determined by the amount of bubbling in the impingers.
    b. the end of the probe is capped and the leak rate determined from the dry
       gas meter.
    c. the end of the probe is capped and the leak rate determined from a
       rotameter attached to the outlet of the dry gas meter.
    d. the end of the probe is capped with a vacuum gauge and a rotameter is
       attached to the outlet of the dry gas meter.
 8. Method 6 sampling is performed:
    a. at a constant  rate.
    b. isokinetically.
    c. proportionally.
    d. by obtaining a grab sample.
 9. The contents of the first Method 6 impinger should be:
    a. discarded.
    b. retained for checking sampling errors.
    c. retained for SOJ analysis.
    d. retained for HZSO4 analysis.
10. Data taken during the Method 6 test should be:
    a. packed with the sample bottles and shipped with them.
    b. recorded in duplicate—one set  mailed  to the lab, one set hand carried.
    c. photocopied at the base lab only.
    d. given, for safe-keeping, to  the test observer.
11. The following true-false statements address  the Reference Method 7 leak-check
    and sampling procedures.
    a. True or False? When the flask is first evacuated, the flask valve is set at the
       evacuate position and the pump valve  is  set  at the evacuate position.
    b. True or False? In  the initial leak check, the flask valve is in the evacuate
       position and the pump valve is in the vent position.
    c. True or False? In  the purge procedure, the manometer fluid is level in both
       legs.
    d. True or False? In  the final leak check,  the flask valve is in the evacuate
       position and the pump valve is in the purge position.
    e. True or False? The flask is removed when the valve is in the evacuate
       position.
    f.  True or False? The flask valve is in the purge position during the final
       pressure check.
12.  The pH of the Method 7 flask sample is adjusted to a value of:
    a. 7.0 to 9.
    b. 9 to 12.
    c. 5 to 7.
    d. It is not adjusted.
                                     165

-------
                            Answers to
        Reading Assignment  13 Review  Exercises
     ,= 29(l-0.12)+18(0.12) = 27.
                              T,M,
                        ).Q)   1  W(740)(27.7)
                            0.88  K(29.6)(0.80)
      _\ /(0.0357)(0.75)(30.0)   1  -|/(740)(27.7)
             (540)(0.85)

      =  0.241 in.
   Choose a nozzle close to 0.241 in., e.g., 0.25 in.
   then:
   AH =
846.72 Dn*AHfflC,J(l-:
                                M,  T, Pm
                                          Ap
         846.72(0.25)41.85(0.85)l(0.88)

      = 2.59Ap
 2.  a.  no
    b.  no
    c.  yes
    d.  no

 3.  a QT) c  d
 4.  a  b (c  d
 5.  a  b  c
 6.  Answers on pages 167 through 169
 7.  a  b  c @
 8. 0 b  c  d
 9.  a (b) c  d
10.  a (b) c  d
                                  , 29  /540
                                   27.7 V740
                                              '29.6\
                                                   Ap
11.  a.  True
    b.  True
    c.  True

12.  a (b) c  d
                d.  False
                e.  False
                f.  False
                                  166

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6.
                                                    Section No. 3.4
                                                    Revision No. 0
                                                    Date January 15,  1980
                                                    Page 8 of  17
                         ON-SJTE MEASUREMENTS  CHECKLIST
                             (Method  5,  Figure 4.5)
       Sampling Train Schematic Drawing
       Apparatus

       Probe  nozzle:   stainless  steel  	  glass
         Button-hook  	 elbow 	  size
         Clean?
       Probe  liner:   borosilicate  y/Y?Q    quartz           other
         Clean?
         Heating system*
         Checked?
       Pitot tube:   Type  S   	   other
         Properly attached  to  probe?*  	
         Modifications
         Pitot tube  coefficient \/ O.g^ (n**tu.vn*f$~}  C frO
      Differential  pressure  gauge:   two  inclined manometers
         other 	 sensitivity
       Filter holder:   borosilicate  glass 	 glass  frit
         filter  support 	  silicone gasket 	  other
         Clean?
       Condenser:   cumber  of  impingers
         Clean?
         Contents:   1st 	  2nd	3rd      	  4th
         Cooling  system
        Proper  connections?
        Modifications
      Barometer:  mercury	  aneroid 	  other
      Gas  density determination:temperature  sensor  type 	
        pressure gauge
        temperature  sensor  properly  attached  to probe?*

      Procedure

      Recent  calibration:   pitot tubes*
        meter box*	  thermometers/thermocouples*
      Filters checked visually for  irregularities?*  4"*** :^ £t'lfa»-ei Cc~)
      Filters properly  labeled?*  	
      Sampling site properly selected?   	 	 	
      Nozzle size properly  selected?*   V^ in

      (continued)
                                     167

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                                             Section No. 3.4
                                             Revision No. 0
                                             Date January 15, 1980
                                             Page 9 of 17


(continued)

Selection of sampling time?  	
All openings to sampling train plugged to prevent pretest con-
  tamination?  	
Impingers properly assembled?  	
Filter properly centered?
Pitot tube lines checked for plugging or leaks?*   /  noV .appWt^able - <;-frtCrfih'fnr tiy-et ff>)
Care taken to avoid scraping nipple or stack wall?*
Effective seal around probe when in-stack?  	
Probe moved at proper time?
Nozzle and pitot tube parallel to stack wall at all times?*  ^HT
  Filter changed during run?  	
  Any particulate lost?
Data forms complete and data properly recorded?* Srv-rE, g/prnpldg. Cep
Nomograph setting changed when stack temp changed significafrtly ? 3

Velocity pressure and orifice pressure readings recorded
  accurately?*  	
Posttest leak check performed?*	(mandatory)
Leakage rate   	 @ in. Hg	
  Orsat analysis          from stack          integrated  HHHZI
  Fyrite combustion analysis 	  sample location 	
  Bag system leakchecked?*
  If data forms cannot be copied, record:
    approximate stack temp 	  volume metered
    % isokinetic calculated at end of each run 	
SAMPLE RECOVERY

Brushes:  nylon bristle 	  other
  Clean?
Wash bottles:  glass
  Clean?
Storage containers:  bcrosilicate glass 	.    other
  Clean?  	  Leakfree?
Petri dishes:  glass   '	  polyethylene 	  other
  Clean?
Graduated cylinder/or balance:  subdivisions <2 ml?*
  other
  Balance:  type
Plastic storage containers:  airtight?
  Clean?    	  	
Probe allowed to cool sufficiently?	
Cap placed over nozzle tip to prevent loss of particulate?*


(continued)
                               168

-------
                                             Section No. 3.4
                                             Revision No. 0
                                             Date January 15, 1980
                                             Page 10 of 17
(continued)
During sampling train disassembly, are all openings capped?
Clean-up area description: ,/ at
  Clean?  	  Protected from wind?
Filters:  glass fiber 	  type
  Silica gel:  type (6 to 16 wesh)?  new?  	 used?
  Color?                           Condition?
Filter handling:  tweezers used?  	
  surgical gloves?  	  other
  Any particulate spilled?*  	
Water distilled?
Stopcock grease:  acetone-insoluble?
  heat-stable silicone?                    other
Probe handling:  acetone rinse
  distilled water rinse
Particulate recovery from:  probe nozzle
                                         _ i
  probe fitting                       probe liner
  front half of filter holder / t^^e. p*pgy ng.ma m I^Q ") CO
Blank:  acetone __ _ >_^_____  distilled water"*
Any visible particles on filter holder inside probe?:* _
All jars adequately labeled?
-------
                         Lesson  G
               Postsampling Operations
Lesson Goal

The goal of this lesson is for you to understand the quality assurance checks and
procedures that can be followed in the postsampling/analytical operations of the
reference methods.

Lesson Objectives

After completing this lesson, you should be able to:
  1. state the procedures outlined in Volume III for the posttest checks of
     temperature sensors, barometers, and dry gas meters.
  2. compare Orsat data with estimated source combustion data as a quick check
     for gross measurement errors.
  3. use the Volume HI checklists:
           Procedure for Weighing Filters (Figure 5.5)
           Procedure for Analysis of Acetone Rinse Samples (Figure 5.6)
  4. list the standardization activities that are conducted as part of the Reference
     Method 6 analytical procedures.
  5. describe how blanks and control samples are used in the Reference Method 6
     analytical procedures.
  6. describe how control samples are used in the analytical procedures of
     Reference Method 7.
  7. describe how working standards are used in the analytical procedures of
     Reference Method 7.

Materials

Assignment 14
  • Section 3.1.5, Postsampling Operations in Section S.I
    Method 2—Determination  of Stack Gas Velocity and Volumetric Flow Rate
  • Section 3.2.5, Postsampling Operations in Section 3.2
    Method 3—Determination  of COj, O», Excess Air,  and Dry Molecular Weight
  • Section 3.3.5, Postsampling Operations in Section 3.3
    Method 4—Determination  of Moisture in Stack Gases
  • Section 3.4.5, Postsampling Operations in Section 3.4
    Method 5—Determination  of Paniculate Matter from Stationary Sources
                                   171

-------
Assignment 15
  • Section 3.5.5, Postsampling Operations in Section 3.5
    Method 6—Determination of Sulfur Dioxide Emissions from Stationary Sources
  • Section 3.6.5, Postsampling Operations in Section 3.6
    Method 7—Determination of Nitrogen Oxide Emissions from Stationary Sources
  • Optional: Section 5.7.5, Postsampling Operations in Section 3.7
    Method 8—Determination of Sulfuric Acid Mist and Sulfur Dioxide Emissions
    from Stationary Sources
                                     172

-------
     Reading Guidance—Assignment 14
            Begin by reading Section 3.1.5—Postsampling Operations
            for Method 2. Read pages 1 of 3 through 3 of 3.
Checking equipment after a test often seems unnecessary and tedious to someone
who is eager to get home or proceed with an analysis. The postsampling checks of
thermometers, barometers, etc., have been specified so that they can be done
quickly, but yet indicate whether or not there might be a problem. For example,
temperature sensor checks merely specify comparing the stack or meter ther-
mometer readings to the ambient temperature.
  Note that if the pitot tube is damaged and recalibrated, corrections can be made
for the velocity determinations made after the damage occurred. This is true for
velocity traverses. If the pitot tube of a Method 5 probe is damaged, the isokinetic
rate calculations would be in error and the tester would not have been sampling
isokinetically after the damage occurred.
            Continue your reading with Section 3.2.5 —Postsampling
            Operations for Method 3. Read pages 1 of 2 through 2 of 2.
                                  173

-------
  There are a number of ways of estimating theoretical CO* or Ot emission con-
centrations from combustion sources. A convenient nomograph that can be used
for this purpose is shown below (Smith,  W.S. and Gruber, C.W. Atmospheric Emis-
sions from Coal Combustion—An Inventory Guide. Springfield, Va. NTIS
No. PB-170-851, 1966).
      70-
      60-
   „  SO-
      30-
      20-
             •10

a
2
1

\ •

60.
_ 35-
j i »-
° : '*-
S : 10-
" I 5-
i i 2-
kHiGH VOLATILE]
BITUMINOUS -*
LOW VOLATILE/
BITUMINOUS 1
SEMIANTHRACITE1
v
ANTMMCITE-
COKE-
• METHANE
-AVERAGE NATURAL GAS
-ETHANE
- PROPANE
-BUTANE
-PENTANE
• 'GASOLINE
• KEROSENE
•No. 2 FUEL OIL
• No. « FUEL OIL
-NO. S FUEL OIL
• No . 6 FUEL OIL
1- BUNKER -C" OIL

V MEDIUM VOLATILE
r BITUMINOUS

ySUBBITUMINOUS
7 AND LIGNITE

I
•n
fe>
S
I
v>
3
i
i

M
£
0
I

tn
UJ
£
S

If the fuel type and one other parameter are known (such as %O,, %COZ, or
% excess air), a line can be drawn between them and approximate values for the
other parameters determined.
  Another convenient way of checking Orsat data is by using F factor relationships.
The Fd factor represents the ratio of the volume of dry flue gases generated in a
combustion process, to the calorific value of the fuel combusted. The Fc factor
represents the ratio of the volume of carbon dioxide generated to the calorific value
of the fuel combusted.

The F. factor is the ratio
and is equal to
  100  Fe

20.9- %0,
  %CO,
                                     174

-------
 with the %O» and %CO, being obtained on or adjusted to a dry basis.
 F0 factors for various fuels are given in the table below.

Fuel type
Coal
Anthracite
Bituminous
Lignite
Oil
Gas
Natural
Propane
Butane

F.

1.070
1.140
1.076

1.79
1.51
1.479
Maximum deviations
from midpoint F. value
(%)

2.9
4.5
2.8

2.9
1.2
0.9
   To use this technique, Orsat values for %Ot and %COt can be substituted into
the equation above. If the resultant value differs from the midpoint F0 values by
more than the range given in the table, the Orsat analysis should be rechecked or
redone (Aldina, G.J. and Jahnke, J.A.,  1979. APTI Course 450 Source Sampling
for Particulate Pollutants—Student Manual. EPA 450/2-79-006, pages 9-5
through  9-15).
             Continue your reading with Section S.S.5—Postsampling
             Operations for Method 4. Read pages 1 of 4 through 4 of 4.
   Note that the dry gas meter is to undergo a posttest check. Refer back to page
 11 of 19 of Section S.S.2 to review this procedure. Note again that these procedures
 are just data checks and not calibrations.
   The dry gas meter is initially calibrated to a precision of 2%. On the posttest
 check, however, a 5% difference from the calibrated value is allowed before a
 recalibration is necessary.
   If a recalibration is done, the lower calibration factor is then used in the calcula-
 tions. This results in a lower gas volume collected and a higher paniculate
 concentration.
   The dry gas meter thermometer is calibrated to within 3 °C initially, but a 6 °C
 deviation is allowed before recalibration is required. In this case, if recalibration is
 necessary, the higher values are  used in the calculations.
             Continue your reading with Section S.4.5 —Postsampling
             Operations for Method 5. Read pages 1 of 15 through
             15 of 15.
                                      175

-------
  Postsampling checks of the dry gas meter, thermometers, and barometers are
similar to the procedures which you have read about for Methods 2, 3, and 4. Do,
however, read Subsection 5.2—Analysis (Base Laboratory) carefully. Figure 5.5 on
pages 10 of 15 and 11 of 15 and Figure 5.6 on pages 12 of 15 through 14 of 15
give step-by-step procedures for the handling and analysis.
  The filter blanks should be treated the same as the sample filters—from the
beginning through the final weighing. Weighing filters can be a tedious procedure.
The use of blanks can help uncover inadvertant errors which might not otherwise
be detected.
  The evaporation of acetone rinses may seem like a simple procedure. But many
test teams have often had difficulty meeting the residue requirements for the
acetone blanks (< 0.001% of total acetone weight). This problem may not be due
to contaminated acetone, but rather, to dust from the air settling into the beakers.
Watch glasses don't always help eliminate the problem.
  Some testing organizations have found it  necessary to evaporate the acetone in
glove boxes, with  filtered air intakes.
  The volume of  the acetone blank should  be approximately the same as that of
the sample rinses. If they are not the same, an error could result. Consider the
following case: compare two 250-ml beakers. Also compare 50 ml of acetone blank
in one beaker to 200 ml of sample rinse in the other.  Assume equal amounts of
dust fall  into  each beaker. If you scaled up the blank reading to correspond to
200 ml, an  error would result because you would be scaling up the dustfall in addi-
tion to any  actual residue in the acetone.
             You have completed your reading for Assignment 14. Do
             the review exercises which follow and check your answers
             after you complete them. The correct answers are given
             on the page following the review exercises.
         Reading Assignment 14 Review Exercises
1.  A pi tot tube used in a Method 2 traverse was damaged just before the test.
   Mike told Jeff to go ahead and traverse anyway, since the data could be cor-
   rected later on. If the original calibration value were Cp = 0.82, the recalibrated
   value were Cp = 0.78, and the average stack gas velocity were 41.2 ft/sec, what
   would the corrected velocity be?
   a.  39.2 ft/sec
   b.  43.3 ft/sec
   c.  32.1 ft/sec
   d.  33.7 ft/sec
                                     176

-------
2. Jeff did the Orsat analysis for the second time in his life. He told Mike that he
   got a value of -4% for COt and 6% for Ot. The plant was burning anthracite
   coal. Was Jeff correct?
   Yes	
   No	
   How do you know?
S. Jeff did the Orsat experiment over again and this time got a value of 14% for
   CO, and 5% for O,. What would the F0 factor be from  this data?
   a.  1.070
   b.  1.S80
   c.  1.492
   d.  1.1S6
4. Is the F0 factor calculated within ±2.9% of the midpoint F0 value for
   anthracite?
      No. It is 6%; but its close enough, so the data should be accepted.
      Yes. It is within the tabulated range; the data should be accepted.
      No. It is 6%; the data should be checked and/or the test redone.
      No. It is 6%; the data should be rejected and the value estimated from a
      nomograph.
   What are the precision limits and posttest deviations for the following pieces of
   equipment?
a.
b.
c.
d.

Dry gas meter thermometer
Dry gas meter correction factor
Field barometer
Stack temperature sensor
Pretest calibration
precision
±5.4°F(S°C)
±0.02Y


Posttest deviation
limit


±5 mm

   In the treatment of Method 5 acetone rinses, in no case should a blank residue
   greater than	% of the blank weight be subtracted from the sample weight.
   a. I
   b. 0.1
   c. 0.01
   d. 0.001
   Is each of the following true or false?
   a. Acetone rinses may be evaporated at room temperature only.
   b. Sample filters may be oven dried at 220°F for 2 to S hours.
   c. Acetone leakage can't be detected because you can't mark on polyethylene
     bottles.
   d. Weighing to constant weight means weighing to a difference (between two
     consecutive weighings) of £0.5 mg with a minimum of six hours of desicca-
     tion between weighings.
                                     177

-------
                         Answers to
        Reading Assignment 14 Review Exercises
1. (a) b  c  d
           —  p
        v,
    VJeorr =  p
                 y
             0.82
                   .2 = 39.2
2.  Yes. According to the figure on page 174 of this course manual, at a 6% O2
   flue gas level, the %CO» should be about 14%.
S.  a  b  c  d
           20.9-
4.
5.
7.
         %cot
      - 20.9-5
          14
                  = 1.136

Dry gas meter thermometer
Dry gas meter correction factor
Field barometer
Stack temperature sensor
Pretest calibration
precision
±5.4°F(S°C)
±0.02Y
±2. 5 mm (0.1 in.)
±1.5% at three
temperatures
Posttest deviation
limit
10.8°F(6°C)
<±5%
±5 mm
±1.5% at ambient
temperature
6.  a  b
a.  False
b.  True
c.  False
d.  True
                               178

-------
     Reading  Guidance—Assignment  15
            Begin by reading Section S.5.5—Postsampling Operations
            for Method 6. Read pages 1 of 16 through 16 of 16.
Subsection 5.1 (paragraphs 5.1.1 and 5.1.2) reviews some of the posttest calibration
checks which have already been discussed. The important pan of this reading
assignment is Subsection 5.2, Analysis (Base Laboratory).
    Subsection 5.2 provides detailed instructions for accurately performing the
barium-thorin titration method for sulfate analysis. Procedures for the standard-
ization of reagents, analysis of control samples, and analysis of the stack sample are
given. The procedures are:
    Ba(ClO4),
   Standardized
 (paragraph 5.2.4)
     H,SO4
  Standardized
(paragraphs 5.2.2
   and 5.2.S)

   (NH4),S04
 Control sample
(paragraph 5.2.5)

     H,SO4
  Stack sample
(paragraph 5.2.6)
-   BaSO4U2HClO4
                                     -    BaS04J+2 NH4C104
                                     -    BaS04U2HClO4
  After just enough barium perchlorate solution is added to precipitate the sulfate
in the sample, the next drop added will produce:
                        Ba(ClO4), - Ba~ + 2 C1O4'
                                  179

-------
If thorin indicator is in the sample solution, we then have:
                 SO,Na
             +
                             SO,Na
                                        H
                            Thorin
                            indicator
           ,H
 Pink
solution
  In paragraph 5.2.1, a note is given in the discussion about water. Distilled
deionized water meeting ASTM specifications is particularly important in this
method.
  It is highly recommended that manufacturer-guaranteed sulfuric acid be pur-
chased for the barium perchlorate standardization. Diluting concentrated sulfuric
acid and standardizing it with NaOH which has to be standardized with potassium
acid phthalate is a procedure which can take a day or more. Purchased, stan-
dardized HZSO4 need merely be diluted up to some known volume in a volumetric
flask—a procedure which takes only about 20 minutes. Also, the errors involved in
the standardization of H,SO4  made up from concentrated reagent will in the end
be much greater than the error in the value given for manufacturer-guaranteed
H,SO4.
  If you  do use purchased HSSO4 solutions, you may skip reading paragraphs 5.2.2
and 5.2.3 of this reading assignment.
  In paragraph 5.2.1, in the  preparation of the Ba(ClO4)z solution, it is noted that
the solution should be protected from evaporation. This is an important point.
Note, also, that BaCl**2 HtO may be used instead of the perchlorate, if desired.
  Paragraph 5.2.4 gives the procedures for standardizing the barium perchlorate.
The preparation and analysis of blanks is important in all analytical procedures. A
blank analysis checks the purity of your reagents. Note item S of pararaph 5.2.4 in
this regard and the limit of 0.5  ml of titrant.
  The color change in the barium-thorin titration is not as sharp as the more
familiar phenolphthalein-acid base titration. For those unfamiliar with the color
changes of the thorin indicator, some practice is necessary. In the note of
                                     180

-------
paragraph 5.2.4, Volume III gives some suggestions how this can be done. Some
other tricks that can be used in obi-ining consistent results are listed here:
       1.  Put a white sheet of paper behind the burette and sample.
       2.  Illuminate the work area or back-light the white paper with fluorescent
          light. Don't use incandescent light.
       S.  Obtain an endpoint on a control sample or blank and titrate to the same
          color in succeeding samples  by keeping the control sample close by.
The color intensity is not as important as is achieving the same color intensity for
all titrations. Consistency is the key in this regard.
  Control samples are very important  as part of quality assurance activities of an
analytical laboratory. Paragraph 5.2.5 gives the procedures for preparing and
analyzing Method 6 control samples, and gives criteria for checking the technique
of the analyst (items 10 and 11). The  analysis of control samples should be an
accepted activity in  the laboratory and should not be by-passed for the sake of
expediency.
  We finally get to  the analysis of the sample in paragraph  5.2.6. Once the analyst
shows that he can do the analysis within the accepted limits, he can then go on and
do his stack sample.
             Continue your reading with Section S.6.5 — Postsampling
             Operations for Method 7. Read pages  1 of 10 through
             10 of 10.
  The analytical procedures for Method 7, which are given in Volume III, incor-
porate the use of control samples. The analysis of control samples is not required in
the Federal Register, but is recommended in Volume III to help in validating data.
                                     181

-------
  The control samples and working standards are made up and analyzed the same
way. The difference between them comes about in the calculation procedures
which are outlined in Figure 1 on page 6 of 10 (Section 3.6.5). The working stan-
dards are used to develop a calibration curve such as that shown below.
          bo

          i
          o
          2
              600
              500
              400
              300
              200
               100
                       1.0   2.0    3.0    4.0
5.0
6.0    7.0
8.0
                                      Absorbance
                                      (at 410 nm)

  The least squares constant, K«, of the calibration curve is obtained by using the
formula given in Figure 5.1 on page 6 of 10 (Section 3.6.5). This value of K* is
then used to calculate an absorbance for each of the control samples at 100, 200,
and 300 fig. This absorbance is then compared with the actual measured absorb-
ance of the control samples. Volume III recommends that calculated and measured
values should agree to within 15%.
                                     182

-------
    In the more recent discussion on quality assurance procedures for Methods 6 and
  7 (Shigehara, R.T. and Curtis, F.  1982, "Methods 6 and 7 Quality Assurance/Con-
  trol Background Information", Source Evaluation Society Newsletter Vol. VII,
  No. 1, February 1982, pp. 15-25), it is recommended that for the working stan-
  dards, Kc be multipled by each working standard absorbance to give
                              Ke X
  and that
    The analytical procedures for Reference Method 7 are quite straightforward.
  However, to obtain good precision and accuracy in the method, it must be per-
  formed by an experienced and meticulous analyst.
    In order to make the analytical procedures of Volume III a little easier for you
  to follow, a review of the Method 7 chemical reaction sequence is provided here.

                  Reactions in sample flask at time of source test
                             NO +_HIO,->NO, + H,O
                             absorbing solution
                                         l-2 HNO,
                      formed from NO or NOt
                           in stack gas

                 Salt formation on evaporating dish — lab analysis

                          HNO, -I- NaOH-NaNO, + H,O
Nitration
  step:
                     OH
               SO,H
                    SO,H
                phenoldisulfonic
                     acid
   NaNOt
(from sample)
 	*.
   H,SO4
   (cone)
                       OH
SO,H
                       SO,H
                                                                 NO,
  Color
developing
  step:
                     OH
              SO,H
                           NO,
                    SO,H
  NH
-------
Note that in these procedures a blank solution is to be analyzed along with the con-
trol working standards and sample. The blank corresponds to the 0.0 pipetted sam-
ple alluded to in item 9 on page 3 of 10 (Section 3.6.5).
             You have completed your reading for Assignment 15.
             You may wish to read optional Section  3.7.5 —Post-
             sampling Operations for Method 8. Much of this material
             has been covered in the Method 6 discussion.
               Do the review exercises which follow and check your
             answers after you complete them. The correct answers
             are given on the page following the review exercises.
         Reading Assignment  15  Review Exercises
 1.  The barium perchlorate solution prepared for Method 6 analysis procedures is
    standardized with a sulfuric acid solution. How do you know the normality of
    the sulfuric acid solution?
    a.  You can use a manufacturer-guaranteed solution and use the value stated.
    b.  You can use a manufacturer-guaranteed solution and dilute it in a
       volumetric flask to the required value.
    c.  You can use concentrated sulfuric acid diluted in a volumetric flask and
       then standardize the solution with an NaOH solution which has been stan-
       dardized with a potassium acid phthalate solution.
    d.  all of the above
    e.  c only
 2.  What is the primary precaution that must be taken with the barium per-
    chlorate solution.
    a.  It must be kept out of the sun.
    b.  It must be protected from evaporation.
    c.  It must be used within two weeks from preparation.
    d.  It must be refrigerated.
                                    184

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S. A blank solution of 2 5-ml deionized distilled water in 100 ml of isopropanol is
   titrated with 0.01 N (nominal) barium perchlorate solution in the barium per-
   chlorate standardization procedure. If the thorin indicator turns the solution
   pink after 0.8 ml of 0.01 N barium perchlorate solution have been added,
   what should be done?
   a.  Everything is fine and you can proceed with the standardization.
   b.  The isopropanol is obviously contaminated with sulfate and must be
      replaced.
   c.  Only 0.5 ml of titrant is allowed. The distilled water is not pure enough
      and must be replaced.
   d.  The thorin indicator decomposed and must be replaced.
4. SST analysis of the third Method 6 sample from a  recent test of Brimstone
   Power was accomplished by pipetting a 20-ml aliquot of the recovered H,Oj
   impinger fraction into a 250-ml Erlenmeyer flask, adding 80 ml of 80% IPA
   and three drops of thorin indicator, and titrating to a pink endpoint. Was this
   done correctly?
   a.  No. The impinger catch was not diluted to a known volume of 100 ml in a
      volumetric flask.
   b.  No. 100% isopropanol must be used because thorin is active only in an
      80% alcohol solution.
   c.  No. 20 ml of thorin indicator  are required to give the proper color.
   d.  Yes. The procedure  was followed correctly.
5. Control samples for Method 6 analysis are prepared using:
   a.  primary standard grade BaClt*2 HSO.
   b.  primary standard grade (NH^SCV
   c.  manufacturer-guaranteed HtSO4.
   d.  primary standard grade Ba(ClO4)j.
6. What is the recommended frequency for the analysis of control samples?
   a.  two  control samples  before source sample analysis and two control samples
      after the last source  sample is  analyzed
   b.  two  control samples  anytime during the day on  which the source samples
      are analyzed
   c.  one  control sample before and one after the analysis of the source samples
   d.  two  control samples  after the last collected source sample is analyzed each
      analysis day
7. Replicate titrant volumes for a Method 6 analysis must agree within:
   a.  1 %  or  1 ml, whichever is smaller.
   b.  0.2% or 1 ml, whichever is greater.
   c.  0.1% or 2 ml, whichever is smaller.
   d.  1%  or 0.2 ml, whichever is greater.
                                    185

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 8.  In Reference Method 7, control samples and working standard solutions are:
    a.  prepared in the same manner.
    b.  analyzed in the same manner.
    c.  used interchangeably.
    d.  all of the above
    e.  a and b, only
 9.  A value of 568.0 was found for the value of K« using the Method 7 working
    standards. The Control Sample S2, corresponded to 200 jig NOZ. The
    measured absorbance of the control sample was equal to 0.321. Does this con-
    trol sample meet the recommended accuracy limit?
    a.  Yes. % difference = 8.81
    b.  Yes. % difference =18.8
    c.  No. % difference = 8.81
    d.  No. % difference =18.8
10.  Which of the following analytical sequences is correct for Reference Method 7?
         NO, reactions with peroxide in flask
         spectrophotometric determination of phenoldisulphonic acid standard
         sodium salt formation on evaporating dish
         nitration of phenoldisulphonic acid
         titration of complex
         NO, reactions with peroxide in flask
         titration of nitrate with thorin
         sodium salt formation on evaporating dish
         nitration of phenoldisulphonic acid
         formation of colored complex
         spectrophotometric determination of colored complex
         NO, reactions with peroxide in flask
         sodium salt formation on evaporating dish
         nitration of phenoldisulphonic acid
         formation of colored complex
         spectrophotometric determination of colored complex
    d.    NO, reactions with peroxide in flask
         formation of colored complex
         sodium salt formation on evaporating dish
         nitration of phenoldisulphonic acid
         spectrophotometric determination of colored complex
                                      186

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                          Answers to
        Reading Assignment 15 Review Exercises
 1.  a
10.
                  568
                      = 0.352
        Absorbance comparison error:
             0.321-0.552
                O.S52
         %=-8.81
b©d
           You have now completed the material for Quiz 2.
             Take Quiz 2 under the direction of your test super-
           visor. (See page 5 of this guidebook for more detailed
           instructions.)
                               187

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     Calculations—
Maintenance—Audits
      Lesson H—Calculations
              Reading Assignment 16
      Lesson I —Maintenance Checks
              Reading Assignment 17
      Lesson J —Auditing Procedures
              Reading Assignment 18
               189

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                         Lesson   H
                          Calculations
Lesson Goal

The goal of this lesson is for you to understand that correct calculation procedures
are essential if one is to achieve valid test results.

Lesson Objectives

After completing this lesson, you should be able to:
  1. properly round off numbers calculated in the reference methods and carry
     out calculations to the appropriate number of significant figures.
  2. list at least four types of errors that frequently occur in source sampling
     calculations.
  S. explain why it is important to use data expressed in the proper units when
     performing calculations specified in the reference methods.
  4. discuss the relative importance of data errors with respect to final calculated
     values, for a number of example calculations.
  5. discuss the use of computers or hand-held calculators in performing reference
     method calculations.

Materials

Assignment 16
  • Section S.I.6, Calculations in Section S.I
    Method 2—Determination of Stack Gas Velocity and Volumetric  Flow Rate
  • Section 5.2.6, Calculations in Section S.2
    Method S—Determination of COj, Of, Excess Air, and Dry Molecular Weight
  • Section 3.S.6, Calculations in Section 3.5
    Method 4—Determination of Moisture in Stack Gases
  • Section 3.4.6, Calculations in Section S.4
    Method 5—Determination of Paniculate Matter from Stationary  Sources
  • Section 3.5.6, Calculations in Section 5.5
    Method 6—Determination of Sulfur Dioxide from Stationary Sources
  • Section 3.6.6, Calculations in Section S.6
    Method 7—Determination of Nitrogen Oxide Emissions from Stationary Sources
                                    191

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      Reading Guidance—Assignment 16
             Begin by reading Section S.I.6—Calculations for Method
             2. Read pages 1 of 4 through 4 of 4.
This reading assignment consists of each of the short sections on calculations for
the reference methods. The first subsection, 6.0, is much the same for all of the
reference methods, so after reading it once, you can quickly skim through it on the
others.
  It is assumed that you are already familiar with the reference method equations.
The goal of this lesson is not to provide background in their derivation or to give
you practice in using them. The goal is to point out Volume III techniques that
can reduce calculation errors.
  Many source tests have been invalidated in the  past because of calculation errors
only. Considering the time, expense,  and difficulty in conducting the reference
methods, errors arising from calculations should be explicitly avoided.
  With the advent of hand-held calculators and desk-top computers, programs can
be and have been developed which can quickly perform the required reference
method calculations. See for example: Ragland, J.W. et. al. 1976. HP-65 Program-
mable Pocket Calculator Applied to Air Pollution Measurement Studies: Stationary
Sources. EPA 600/8-76-002, October 1976.
  Errors still can arise with the use of programmable calculators or computers. It is
good practice to punch in an example problem for which the answer is known to
see if the program and calculator are working properly. A number of example
calculations are given in  the calculation sections of Volume HI. Punching wrong
numbers into a calculator will give wrong results. As with all other aspects of
source sampling, care should be taken in this pan of the process.
  Note in Subsection 6.1 that a nomenclature list is provided, giving the units for
each parameter in both metric and English terms. It is important that data be
expressed in the correct units before being substituted into the method equations.
Many of the equations contain constants which are dependent upon the system of
units used. For example, the average stack gas velocity is calculated in units of feet
per second if (Ap).« is in inches of water, and K, = 85.49.
            Continue your reading with Section 3.2.6—Calculations for
            Method S. Read pages 1 of 3 through 3 of S.
                                    193

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             Continue your reading with Section 3.3.6—Calculations for
             Method 4. Read pages 1 of 8 through 8 of 8.
  Example calculations are given in Figures 6.1 A and 6.IB on pages 4 of 8 and 5 of 8
of Section 3.3.6. Note the spaces denoting the number of significant figures that
are to be used. This aid is provided for you in the calculation discussions of
Methods 3, 6, 7, and 8 in Volume III. You may wish to develop similar forms for
the other reference method calculations or for calculations not addressed in
Volume III.
  The following rules are used for determining the number of significant figures in
a number:
     1. Disregard all initial zeros.
     2. Disregard all final zeros unless they follow a decimal point.
     3. The remaining digits are significant.
  Volume III recommends carrying out calculations to one decimal figure beyond
the acquired data. Rounding off numbers is accomplished according to the
following rules:
     1. If the succeeding digit is greater than five, round off to the next highest
       number.
     2. If the succeeding digit is less than five, drop the  digit.
     3. If the succeeding digit is equal to five and the preceding number is odd,
       round off to the next even number.
     4. If the succeeding digit is equal to five and the preceding number is even,
       drop the five.
       Examples: round off to  three significant figures:
                              2.168-2.17 rule 1
                              2.153-2.15 rule 2
                              2.155-2.16 rule 3
                              2.165-2.16 rule 4
             Continue your reading with Section 3.4.6—Calculations for
             Method 5. Read pages 1 of 10 through 10 of 10.
  It is assumed that you are already familiar with the nomenclature of source
sampling. If the symbols used in the calculations are new to you, just realize that
they are similar to the words of a new language. Each symbol means something
and is accompanied by a specific set of units (metric or English). As with all
languages, the more that one uses it, the fewer mistakes he or she will make.
                                      194

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  The isokinetic variation equation given on page 8 of 10 in Section 3.4.6 is very
sensitive to roundoff error. Care should be  taken in keeping the proper number of
significant figures throughout the calculation (particularly in the value of A,, the
nozzle area, which is to be expressed in units of square feet). An example problem
addressing this situation is given in the review  exercises of this lesson.
             Continue your reading with Section 5.5.6—Calculations for
             Method 5. Read pages 1 of 6 through 6 of 6.
               Then go on to Section 3.6.6—Calculations for Method 7.
             Read pages 1 of 6 through 6 of 6.
  A recent article has reviewed types of errors which can occur in Methods 6 and
7. (Shigehara. R. and Curtis, F. February 1982. "Methods 6 and 7 Quality
Assurance/Control Background Information". Source Evaluation Society Newsletter
Volume III, No. 1.) By evaluating several hundred audit sample reports, the
authors found that approximately 10% of the reports contained some type of
mistake in the calculations. The most common problems were: using the wrong
normality for the barium standard in Method 6, using the wrong aliquot factors in
Method 7, and making decimal-point errors. Fortunately, many of these errors can
be corrected once they are detected.
  Using certified samples and having organization management conduct
independent reviews can help to assure that the calculations in the final report are
done properly.
             You have completed your reading for Assignment 16. Do
             the review exercises which follow and check your answers
             after you complete them. The correct answers are given
             on the page following the review exercises.
                                     195

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         Readinr  Assignment 16 Review Exercises
1.  How many significant figures are in each of the following?
   a.  304.0    	
   b.  9000    	
   c.  0.114    	
   d.  0.007    	
   e.  280.S    	
2.  Round off each of the following numbers to three significant figures.
   a.  714.2     	
   b.  1725     	
   c.  0.1432    	
   d.  9.135     	
   e.  9147.2    	
3. State the units for each of the following symbols.
   a.  AH, Ap, ?„„     	  	
   b.  Vm, v,, V,c       	  	
   c.  A, A.	
   d.  B,,,, Y, I	
4. Mike recorded the sampling nozzle diameter as 0.263 inches during a source
   test. He later used a value of 0.0004 ft* for the nozzle cross-sectional area in
   order to calculate percent Isokinetic (%I). What is the problem here?
   a.  There is no problem—roundoff is done correctly.
   b.  The rounded-off A* will give a %I that is 6% too high.
   c.  The rounded-off An will give a %I that is 6% too low.
   d.  The value of A,, should be expressed in in.*.
5. Because of high SOS concentrations in the source, it was necessary for Super
   Stack Testers (SST) to cut their HZOX samples for analysis. In the final report,
   the final dilution scheme was documented:




Run#l
Run #2
Run #3

Original
volume
(ml)
100
100
250

Aliquot
size
(ml)
10
10
20

Aliquot
diluted to
ml
250
100
100
Final (ample
size for
analysis
(ml)
20
10
25

Final
dilution
factor
125
100
50

Correct
dilution
factor



   What should the correct dilution factors be?
                                    196

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                           Answers to
        Reading Assignment 16 Review Exercises
1.   a
    b.
    c.
    d.
    e.
2.  a.  714
    b.   1720
    c.  0.143
   d.  9.14
   e.  9150
S.  a.  _
    b.  _
    c.  _

4.  a  b
      mm (in.) HtO
      dcm (dcf)
         dimensionless
mm (in.) HtO
m/s (ft/sec)
                                               mm (in.) Hg
                                              "ml
                            m
                            (ft*)
                         dimensionless
   %I = K4
   Therefore
%Inw) — 0.94 %I(nnat4*
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5.
Correct
dilution
factor
Runll
Run #2
Run #3
125
OK
50
                                  198

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                         Lesson   I
                  Maintenance Checks
Lesson Goal

The goal of this lesson is for you to understand the procedures recommended in
Volume III for  the routine maintenance of source sampling equipment.

Lesson Objectives

After completing this lesson, you should be able to:
  1. explain why routine maintenance is required on source sampling equipment.
  2. list at least two items which should be checked for on each of the following:
         • pilot tube
         • fiber vane pump
         • dry gas meter
         • sampling train glassware

Materials

Assignment 17
  • Section 3.1.7,  Maintenance in Section 3.1
    Method 2—Determination of Stack Gas Velocity and Volumetric Flow Rate
  • Section 3.2.7,  Maintenance in Section 3.2
    Method 3—Determination of CO», Oj, Excess Air, and Dry Molecular Weight
  • Section 3.3.7,  Maintenance in Section 3.3
    Method 4—Determination of Moisture in Stack Gases
  • Section 3.4.7,  Maintenance in Section 3.4
    Method 5—Determination of Paniculate Matter from Stationary Sources
  • Section 3.5.7,  Maintenance in Section 3.5
    Method 6—Determination of Sulfur Dioxide from Stationary Sources
  • Section 3.6.7,  Maintenance in Section 3.6
    Method 7—Determination of Nitrogen Oxide Emissions from  Stationary Sources.
                                  199

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     Reading  Guidance—Assignment  17
This is a relatively short reading assignment. The Volume III discussions on
maintenance are much the same for Reference Methods 2 through 8, so they can
be read rather quickly. Routine maintenance is an important pan of any quality
assurance program. A testing organization with a busy schedule may often neglect
such maintenance and then have problems on site. The Volume III guidelines for
maintenance are intended to provide a start for the development of your own pro-
gram. Similar procedures can be extended to laboratory balances,  spectro-
photometers, continuous monitoring equipment, impactor systems, and so on.
            Begin  by  reading  Section 3.1.7 —Maintenance
            Method 2. Then read the Maintenance Sections
                           S.2.7-Method 3
                           S.3.7-Method 4
                           3.4.7-Method 5
                           3.5.7-Method 6
                           3.6.7-Method 7
for
            You have completed your reading for Assignment 17. Do
            the review exercises which follow and check your answers
            after you complete them. The correct answers are given
            on the page following the review exercises.
        Reading Assignment 17 Review Exercises
1. How often does Volume III recommend that routine maintenance checks be
  conducted for a sampling train?
  a. quarterly or after 1000 ft* of operation
  b. yearly or after 500 ft3 of operation
  c. semi-annually or after 1000 ft" of operation
  d. every month
                                 201

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2. A fiber vane pump requires a periodic check of:
   a.  oil level.
   b.  oil appearance.
   c.  oiler jar.
   d.  all of the above
3. The dry gas meter of a sampling train should be checked for corrosion and
   excess oil:
   a.  every month.
   b.  every three months.
   c.  every year.
   d.  after every test.
4. Jeff was doing a Method 6 test when the ball in the rotameter stuck. In despera-
   tion, he stopped the run and cleaned out the rotameter with acetone. Was this
   a good thing to do?
   Yes	
   No	
   Why or why not?	
5. Jeff had been in a hurry before going out to test Acme Power. He forgot to
   bring the condensing system for his Method 5 apparatus. Not wanting to go
   back or admit his forgetfulness,  he hooked up his diaphragm pump directly to
   the probe to get his bag sample. What might be found in a routine check of the
   pump?
   a.  oil in the pump from backup oil in the jar
   b.  nothing—there should be no problem since diaphragm pumps are
      maintenance free
   c.  corrosion of the diaphragm head because of condensation and acid deposition
   d.  burned stator because of too high a motor speed
                                     202

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                        Answers to
       Reading Assignment 17 Review Exercises
1. 0 b  c d

2.  a b  c (d)

3.  a (b) c d

4.  No. Acetone could react with the plastic of the rotameter.

5.  a b (7)d
                            203

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                         Lesson  J
                  Auditing Procedures
Lesson Goal

The goal of this lesson is for you to be able to implement auditing procedures in a
source test quality assurance program.

Lesson Objectives

After  completing this lesson, you should be able to:
  1. describe what an audit is.
  2. distinguish between a performance audit and a system audit.
  3. list the functions of an auditor.
  4. describe the auditing device that can be used in Reference Method 5.
  5. tell what is in the audit samples commonly used for Reference Methods S, 6,
     and?.
  6. list at least four check items that an  auditor should observe on site for each of
     Reference Methods S, 4, 5, 6, and 7.
  7. describe how a source testing laboratory can  use audit samples in its quality
     assurance program.
  8. understand the use of percentile rankings in the EPA National Performance
     Audit Program.

Materials

Assignment 18
  • Section 1.4.16, Quality Assuance Manual—Volume I. Audit Procedures.
    Pages 59  through 63 of this correspondence course manual
  • Section 3.1.8, Auditing Procedure in  Section 3.1
    Method 2—Determination of Stack Gas Velocity and Volumetric Flow Rate
  • Section 3.2.8, Auditing Procedure in  Section 3.2
    Method S—Determination of COJ( Ox, Excess Air, and Dry Molecular Weight
  • Section 3.3.8, Auditing Procedure in  Section 3.3
    Method 4—Determination of Moisture in Stack Gases
  • Section 3.4.8, Auditing Procedure in  Section 3.4
    Method 5—Determination of Paniculate Matter from Stationary Sources
  • Section 3.5.8, Auditing Procedure in  Section 3.5
    Method 6—Determination of Sulfur Dioxide from Stationary Sources
  • Section 3.6.8, Auditing Procedure in  Section 3.6
    Method 7—Determination of Nitrogen Oxide Emissions from Stationary Sources
                                   205

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      Reading Guidance—Assignment  18
This reading assignment is the last one in this correspondence course. The subject
of auditing procedures is appropriate in completing this study of Volume III, since
a proper audit will review all phases of the source test—from the pretest prepara-
tions to the on-site measurements and final calculations. Since it probably has been
some time since you first started this course, let us begin this assignment by reviewing
Lesson A —Reading Assignment 2.
             Begin by reviewing pages 59 through 63 of this corre-
             spondence  course manual: Audit  Procedures—Quality
             Assurance Manual Volume I Section 1.4.16.
  Note especially the definitions given for performance audits and system audits.
Much of this information is general. More specific procedures for source sampling
methods are, of course, given in Volume III.
  In the past, quality assurance and the use of audit samples focused on analytical
laboratory practices. Obtaining a representative source sample for the analysis is as
important as properly performing the analysis. In a source test, the source itself
must be operating in a representative manner, the sampling site must be represen-
tative, and the test samples must be obtained in a representative manner. Perform-
ance or system audits need to be conducted for this whole setup. For this reason, in
each of the reference method Audit Procedure sections which you are about to
read, checklists are provided for the auditor or inspector. Each phase of the test,
pretest, on-site measurements, postsampling, etc., have checkpoints which the
auditor can use to evaluate the performance of the test. These points can provide a
stan for the development of your own auditing program.
             Continue your reading with Section S. 1.8—Auditing Pro-
             cedure for Method 2. Read pages 1 of 5 through 5 of 5.
  Note especially the four functions of the auditor summarized on page 2 of 5.
  Many forms and checklists have been developed for the auditor or source test
field inspector. Example forms are given throughout Volume III, one of which is
                                    207

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Figure 8.1 on page 4 of 5, Section S.I.8. Other formats which could be adopted in
your quality assurance program can be found in:
        Industrial Guide for Air Pollution Control—Handbook. June 1978.
       EPA 625/6-78-004.
        Source Sampling Administration Manual. Volume III—EPA
       Stationary Source Enforcement Series. November 1977.
             Continue your reading with Section S.2.8—Auditing Pro-
             cedure for Method S. Read pages 1 of 5 through 5 of 5.
  Certified gases can be used as audit materials for Reference Method S. Note the
discussion on page 1 of 5, Section 3.2.8, paragraph 8.1.2. Note the recommended
difference value, D, of 1% or less, given for correspondence with the audit
materials.
             Continue your reading with Section 3.3.8—Auditing Pro-
             cedure for Method 4. Read pages 1 of 4 through 4 of 4.
               Then go on to Section 3.4.8—Auditing Procedure for
             Method 5. Read pages 1 of 7 through 7 of 7.
  The audit procedures for Method 5 introduce the use of a calibrated critical
orifice. The orifice plate is incorporated into a quick-connect coupling which is in
turn inserted into the gas inlet of the meter box. The assembly is shown in the
figure below.
  Construction and calibration details of this audit device are given in: Mitchell,
W.J. et al. 1981. New Orifice Opens Way For Fast Calibration. Pollution Engi-
neering. June 1981. pp. 45-47.
  The Environmental Protection Agency has conducted a National Performance
Audit Program yearly since 1977. The program has involved sending audit samples
for Methods 6 and 7 and the critical orifice device for Method 5 to source testing
organizations across the country. The testing organizations use these audit devices
                                     208

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in their laboratories and then report their results to EPA. Part of the results of the
program are given on page 3 of 7 of Section S.4.8, paragraph 8.1.1. They show
that 90% of the testing laboratories can come within 10% of the audit standard
value. More detailed results of these surveys are given in  the following:
         Fuerst, R.G. et al. A summary of the Interlaboratory Source Per-
      formance Surveys for EPA Reference Methods 6 and 7—1977. EPA
       600/4-79-045. August 1979.
         Fuerst, R.G. and Midgett, M.R. A summary of the Interlaboratory
       Source Performance Surveys for EPA Reference Methods 5, 6, and 7—
       1978. EPA 600/4-80-029. May 1980.
         Fuerst, R.G., Streib,  E.W., and Midgett, M.R. A Summary  of the
       EPA National Source Performance Audit Program—1979. EPA
       600/4-81-029. April 1981.
  The percentile ranges are given as a guide to show what level of correlation can
be obtained using the audit devices. Note that  audit samples and devices are
intended to be used as an aid to assess the quality of source test data.  Care  should
be taken in specifying a given number for %A such  as "all audit samples analyzed
must agree within 1% of the standard value, or else  the test is rejected", since such
a specification may be meaningless with respect to the overall test accuracy.
However, if 90% of the laboratories which have analyzed audit samples agree to
within, say, 5%  of the sample's known value, a laboratory presenting a 15%
discrepancy should be questioned about its capabilities.
  We have already discussed calculation errors in Lesson H. The auditing of the
source test report for calculation errors is one of the  most important parts of any
quality assurance program. Several techniques  can be used to do this.  A common
one is for an agency or other organization to develop audit computer programs for
all of the source test calculations. The raw source test data is then fed into  the
computer and the results compared to those given in the final report.  With the
wealth of information printed over the past ten years by  the Environmental Protec-
tion  Agency on source test procedures, and with the  advent of inexpensive pro-
grammable calculators, there should be no excuse for calculation errors occurring
in the reports of a professional source testing organization.
             Continue your reading with Section S.5.8—Auditing Pro-
             cedure for Method 6. Read pages 1 of 7 through 7 of 7.
  Ammonium sulfate solutions can be used as audit samples for Reference Method 6.
The precision of Method 6 analytical procedures can be quite good, as is reflected
in the percentile rankings on page S of 7, Section 3.5.8, paragraph 8.1.1.
  A further discussion on the results of the National Performance Audit Program
can be found in: Shigehara,  R.T. and Curtis, F. 1982. Methods 6 and 7 Quality
Assurance/Control Background Information Source Evaluation Society Newsletter.
Vol. HI, No. 1 pp.  15-25.
                                     209

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             Continue your reading with Section 3.6.8 —Auc- dng Pro-
             cedure for Method 7. Read pages 1 of 8 through 8 of 8.
  Problems with Method 7 are often the result of poor analytical technique. This is
borne out in the percentile rankings given on page 3 of 8, Section 3.6.8, paragraph
8.1.1. Only 80% of the laboratories participating in the audit program were able
to get within 15% of the known concentration of the KNOS audit samples. It is
becoming evident that the problems with Method 7 lie not so much with the
method itself, but in the capabilities of the analysts. It has been shown that
experienced personnel using quality control procedures can achieve consistently
greater precision than that which is reported in Volume III. See for example: Host,
A.J. San Diego Gas and  Electric GEM QA Program in Specialty Conference Pro-
ceedings—Continuous Emission Monitoring—Design, Operation and Experience.
Air Pollution Control Association. 1981.
             You have completed your reading for Assignment 18. Do
             the review exercises which follow and check your answers
             after you complete them. The correct answers are given
             on the page following the review exercises.
         Reading Assignment 18 Review Exercises
1. Performance audits are normally:
   a. a qualitative appraisal of data quality.
   b. a quantitative appraisal of quality.
   c. independent checks conducted by the IRS.
   d. used as the basis for conducting a system audit.
2. List two types of performance audits.
   a. 	
   b. 	
3. Which of the following might be used in a system audit?
   a.  calibrated critical orifice
   b.  Figure 8-1, page 4 of 5, Section 5.1.8
   c.  Figure 8-1, page 6 of 7, Section 3.4.8
   d.  standard aqueous ammonium sulfate solution
                                    210

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4. List four functions of a source test auditor.
   a. 	
   b. 	
   c. 	
   d. 	
5. Mike analyzed an audit sample before analyzing his Method 6 samples. He was
   later informed by EPA that his %A was 3.2%. From this information you
   know:
   a. that Mike could perform the Method 6 titration as well as or better than
      90% of the participating laboratories.
   b. that Mike could not perform the Method 6 titration as well as 90% of the
      participating laboratories.
   c. that Mike's sample had a 10% probability of being correct.
   d. that Mike's sample had a 10% probability of being incorrect.
6. Match the audit sample or device with the proper reference method.
   Method 1	                 a. (NH^SC^  standard solution
   Method 2	                 b. none
   Method S	                 c. calibrated orifice
   Method 4	                 d. 12% COt 6% O, calibration gas
   Method 5	                 e. KNOS standard solution
   Method 6	
   Method 7	
   Method 8	
7. Frank was assigned the task of observing a stack test performed by SST at Acme
   Power. The  test involved the determination of paniculate and SO, emissions. A
   number of things happened during the test. Frank used the checklists given in
   the auditing procedure sections for Methods 1 through 6 (Figures 8.1 in Sections
   3.1.8, 3.2.8, 3.3.8, 3.4.8, and 3.5.8). For each event, give the potential prob-
   lem and note whether or not the checklist would have been helpful to Frank in
   his audit.
                 Situation
                       What is the
                    potential problem?
On which checklist would
 this appear? If on none,
  where is the situation
addressed in Volume III?
    a. Test ports were at the location
      given below.
                           i

          Platform —HZ nfil D__
            Circular
              duct
           	L_
20
ft
                            50ft
                            140ft
                              Stack
      Twelve traverse points were selected.
                                     211

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                Situation
                                              What is the
                                          potential problem?
On which checklist would
 this appear? If on none,
  where is the situation
addressed in Volume III?
b. The pitot tube Cf for the Type S tube
   attached to the probe used in the
   Method 5 sampling, was assumed to have
   a value of 0.84.
c.
No equipment calibration data were
supplied to the observer.
d. The gasket on the filter holder contained
   filter fibers after the first run, but the
   technician scraped all of the fibers off
   after the second run, using a pocket knife.
   During run #2 of the Method 5 test,
   Super Stack Testers took a break from
   the sampling routine. The following
   parameters concerning the sampling train
   were observed while they were on break.
   (1)  pitot tube at a  30° yaw angle
   (2)  outlet temperature from fourth
       impinger 78 °F
   (3)  water condensation ahead of
       condenser
f.  The sample jar for the third run of the
   Method 5 test has a label stating:
   "Acme Test-SST-Sept. 12,  1979".
g. In determining the emission rate correc-
   tion factor for Acme Power and Light
   Company, the Super Stack Testers
   opted to use their Fyrite-type combustion
   gas analyzer rather than their Orsat
   analyzer because of a time limitation.
h. The analysis of the moisture content
   from Method 5 was determined by
   the following equation:
                     -f 0.025
                                         212

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                           Answers to
        Reading Assignment 18 Review Exercises
1.   a (b) c  d
2   a     measurement system audit
    jj     data processing audit
            d
         informs test team of pretest audit results
    jj     observes procedures and techniques of the
         field team during sample collection	
    c     checks records of apparatus calibration
    (j     records results of audit and reports them
         to test team management	

5. 0 b  c  d

6.   Method 1    b
          2    b
          S    d
          4    b
          5    c
          6    a
          7  _e_
          8    a
                                213

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7.
                        Item
   Potential problem?
        Checklist
     a.  Test ports were at the location
        given below.
                                  50ft
            Platform
Improper number of
traverse points selected.
Should sample at 18
points (for a circular
duct—20).
                                  140ft
Not addressed on audit
checklists. Would need
to refer back to Figures
1.3 and 1.5, Section
S.O.I, page 7 of 19 and
page 12 of 19. Should
modify audit checklist or
develop own form if
necessary.
                                    Stack
        Twelve traverse points were selected.
     b.  The pitot tube C, for the Type S tube
        attached to the probe used in the
        Method 5 sampling, was assumed to
        have a value of 0.84.
C, might not have been
equal to 0.84 and most
probably would actually
have been lower. This
would lead to higher cal-
culated flow rates and
non-isokinetic sampling.
Figure 8.1, Section 3.1.8,
page 4 of 5—Form M2-8.1
         also
Form M2-3.1 (MH), Pre-
test Sampling Checks
           or
Form M5-4.5 (MH)
On-site Measurements
Checklist (Section 3.4,
page 6 of 15)
     c.  No equipment calibration data were
        supplied to the observer.
Uncertainty as to
adequacy of equipment
for the test and values
calculated for sampling
rates, emission values, etc.
Method 2—Figure 8.1
 Section 3.1.8, page 4 of 5
 Form M2-8.1
Method 4—Figure 8.1
 Section 3.3.8, page 3 of 4
 Form M4-8.1
Method 5—Figure 8.1
 Section 3.4.8, page 6 of 7
 Form M5-8.1
Method 6—Figure 8.1
 Section 3.5.8, page 6 of 7
 Form M6-8.1
Method 7—Figure 8.1
 Section 3.6.8, page 7 of 8
 Form M7-8.1
Method 8—Figure 8.1
 Section 3.7.8, page 6 of 7
 Form M8-8.1
See also: appropriate
forms in Method High-
lights sections.	
                                             214

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                  Item
  Potential problem?
       Checklist
d.  The gasket on the filter holder contained
    filter fibers after the first run, but the
    technician scraped all of the fibers off
    after the second run, using a pocket
    knife.
Filter material on gaskets
is to be scraped off and
weighed with sample/filter.
  In the situation pre-
sented here, the results
of the first run would be
biased low. The results of
the second run would
be biased high.
Figure 8.1 Section 3.4.8,
page 6 of 7 Form M5-8.1
(note item 7—On-site
Measurements)
           also
M5-4.5 (MH) On-site
Measurements Checklist—
Section 3.4, page 8 of 15.
e. During run #2 of the Method 5 test,
   Super Stack Testers took a break from
   the sampling routine. The following
   parameters concerning the sampling train
   were observed while they were on break.
   (1) pitot tube at a 30° yaw angle
   (2) Outlet temperature from fourth
       impinger 78 °F
   (3) water condensation ahead of
       condenser
(1) An error would occur
    in velocity determina-
    tion if in this position
    when sampling. No
    problem if data not
    taken during break.
    Probe, however,
    should not have been
    left in stack.
(2) Outlet temperature
    too high. Specified to
    be 68 °F.
(3) Possible net loss in
    determination of
    % moisture when
    measuring water in
    impingers.
(1)  Not directly addressed,
    but is improper
    procedure.
(2)  Not addressed in Form
    M5-8.1, but should
    be recorded on Form
    M5-4.2.
(3)  Not addressed in
    Form M5-8.1.
f.  The sample jar for the third run of the
   Method 5 test has a label stating:
   "Acme Test-SST-Sept. 12, 1979".
Incomplete labeling;
possible misidentification
of sample in posttest
operations.
Figure 8.1 Section 3.4.8,
page 6 of 7
Form M5-8.1
(note item 7 —On-site
Measurements.)
(Note also—Form M5-4.S.)
   In determining the emission rate correc-
   tion factor for Acme Power and Light
   company, the Super Stack Testers opted
   to use their Fyrite-type combustion gas
   analyzer rather than their Orsat analyzer
   because of a time limitation.
Improper procedure.
Method requires Orsat
measurements.
Not addressed in
FormM5-8.1.
Refer to Reference
Methods 3 and 5
procedures.
h. The analysis of the moisture content
   from Method 5 was determined by the
   following equation:
                           4-0.025
Not the proper equation
for the determination of
moisture content. The
0.025 is the fraction asso-
ciated with the vapor
pressure of water at 68 °F.
Silica gel in last impinger
would give dry gas
stream.
Figure 8.1 Section 3.4.8,
page 6 of 7 Form M5-8.1
Item 12—Postsampling.
See also Section 3.4.6,
page 7 of 10—
Equation 6.3.
                                            215

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  One point of this exercise has been to indicate to you that the auditor can make use
of more than just the audit forms of Section 8 when observing a source test. The
many forms and checklists provided in Volume III in the Method Highlights sec-
tions and Data Forms sections can be used when auditing a test. As noted earlier in
this handbook, however,  these forms should be used with discretion. Requiring a
source tester to use a specific form may strain relations between the parties involved
in the test. The application of Volume III audit procedures or other procedures
should be agreed upon before any testing occurs.
             You have now completed all of the reading assignments
             for this course.
               Take the final examination under the direction of
             your test supervisor. (See page 5 of this guidebook for
             more detailed instructions.)
                                      216

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10/3/90
                                 ERRATA SHEET

       CC  414:  Quality Assurance for Source  Emission Measurement  Methods

There are now Reference Methods 3A and  3B.   For Methods 3A and 3B respectively,
see 40 CFR 60, App. A,  Meth.  3A and Federal Register  notice Vol  55, p. 05211,
Feb. 14, 1990.

For cyclonic flow,  an average 20 degree angle of rotation  is  now acceptable.
See 40 CFR 60, App. A, Meth. 1.

p. 196, Reading Assignment 16 Review Exercises.  The correct answer to question
l.a., "How many significant figures are in 0.007?" is 1 not 3. This is supported
by Rule 1 on p. 194 which states, "Disregard all  initial  zeros."

-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1,
4.
7.
9.
REPORT NO. . 2- 3. RECIf
EPA 450/2-82-003
TITLE AND SUBTITLE 5. REPO
APTT Pm"T"PQr»nnr1priPP P.nnTfif* 414 — — _
Quality Assurance for Source Emission Measurement
Methods
AUTHOR(S) 8. PEHF
James A. Jahnke
PERFORMING ORGANIZATION NAME AND ADDRESS 10. PRO
Northrop Services, Inc.
PO Box 12313 11'CON
Research Triangle Park, NC 27709 68
12. SPONSORING AGENCY NAME AND ADDRESS 13. TYP
IT C TTTwtfrknTnori«-n1 Pr-ot-an f- 1 nn Aoorifw Gu

15
16
17.


1b.
Manpower and Technical Information Branch
Research Triangle Park, NC 27711 EP

MENT-S ACCESSIOWNO.
RT DATE
ly 1982
ORMING ORGANIZATION CODE
ORMING ORGANIZATION REPORT NO.
GRAM ELEMENT NO.
TRACT /GRANT NO.
-02-3573
E OF REPORT AND PERIOD COVERED
idebook
"4SORING AGENCY CODE
A-OANR-OAQPS
. SUPPLEMENTARY NOTES
Project Officer for this publication is R. E. Townsend, EPA-ERC MD20, RTP, NC 27711
. ABSTRACT
This guidebook provides direction for Air Pollution Training Institute Course 414,
"Quality Assurance for Source Emission Measurements." It contains reading
assignments and review exercises covering the following topics:
Quality Assurance Policy and Programs
Procurement of Source Sampling Equipment
Calibration Methods
Presampling - Sampling - Postsampling Operations
Calculations
Maintenance and Audit Procedures
The Guidebook is designed for use in conjunction with "Quality Assurance Manual for
Air Pollution Measurement Systems - Volume III, Stationary Source Specific Methods"
(EPA-600/4-77-027b)
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS b. IDENTIFIERS/OPEN ENDE
Training Correspondence C
Quality Assurance Stack Sampling
Source Testing Particle Samp 1 in
Filtered Particle Sampling Gas Sampling
Gas Sampling Quality Assuranc
Calibrating
DISTRIBUTION STATEMENT .. , imited 19' SECURITY CLASS (This 1
National Technical Information Service - yn(ria.s.s^*e(*
5285 Port Royal Road 20. SECUR.TY CLASS ^,
Springfield, VA 22161 Unclassified

D TERMS c. COSATI Field/Group
ourse 14 B
14 D
g
e
leport) 21. NO. OF PAGES
222
tage) 22. PRICE
EPA Form 2220-1 (t-73J
                                                        217

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