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
-------
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
-------
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
-------
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
-------
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)
-------
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».
-------
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
-------
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.
-------
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-
-------
02
'0*?
-------
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
-------
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.
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
Procurement
Quality Control
-°«fc
Statistical
Analysis of Data
SI
-------
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
-------
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
-------
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
-------
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.
-------
Statistical
Analysis of Data
Procurement
Quality Control
37
-------
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
-------
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
-------
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
-------
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
-------
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
-------
Statistical
Analysis of Data
Procurement
Quality Control
43
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
»^<2
2. »> V
Statistical
Analysis of Data
Procurement
Quality Control
51
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
*
-------
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
-------
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
-------
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
-------
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?
^ *
-------
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
-------
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
-------
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
-------
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
-------
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
-------
Procurement
Quality Control
£3?-*.
Statistical
Analysis of Data
t)»ta
71
-------
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
-------
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
-------
Procurement
Quality Control
Statistical
Analysis of Data"~~i
75
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
------- An error occurred while trying to OCR this image.
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
©
b
b
b
b
(b
b
c (
©
©
c
) c
0
d)
d
d
*©'
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
(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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
*£=
~
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
Calculations—
Maintenance—Audits
Lesson H—Calculations
Reading Assignment 16
Lesson I —Maintenance Checks
Reading Assignment 17
Lesson J —Auditing Procedures
Reading Assignment 18
189
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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*
-------
5.
Correct
dilution
factor
Runll
Run #2
Run #3
125
OK
50
198
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
------- |