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Notice
This is not an official policy and standards document. The opinions, findings, and
conclusions are those of the authors and not necessarily those of the Environmental
Protection Agency. Every attempt has been made to represent the present state of
the art as well as subject areas still under evaluation. Any mention of products or
organizations does not constitute endorsement by the United States Environmental
Protection Agency.
Availability of Copies of This Document
This document is issued by the Manpower and Technical Information Branch, Con-
trol Programs Development Division, Office of Air Quality Planning and Standards,
USEPA. It is for use in training courses presented by the EPA Air Pollution Training
Institute and others receiving contractual or grant support from the Institute.
Schools or governmental air pollution control agencies establishing training programs
may receive single copies of this document, free of charge, from 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, 5825 Port
Royal Road, Springfield, VA 22161.
-------
JD
\
^ ^
t*W?
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AIR POLLUTION TRAINING INSTITUTE
MANPOWER AND TECHNICAL INFORMATION BRANCH
CONTROL PROGRAMS DEVELOPMENT DIVISION
OFFICE OF AIR QUALITY PLANNING AND STANDARDS
The Air Pollution Training Institute (1) conducts training for personnel working on the develop-
ment and improvement of state, and local governmental, and EPA air pollution control programs,
as well as for personnel in industry and academic institutions; (2) provides consultation and other
training assistance to governmental agencies, educational institutions, industrial organizations, and
others engaged in air pollution training activities; and (3) promotes the development and improve-
ment of air pollution training programs in educational institutions and state, regional, and local
governmental air pollution control agencies. Much of the program is nou1 conducted by an on-sitc
contractor, Northrop Services, Inc.
One of the principal mechanisms utilized to meet the Institute's goals is the intensive short term
technical training course. A full-time professional staff is responsible for the design, development.
and presentation of these courses. In addition the sendees of scientists, engineers, and specialists
from other EPA programs governmental agencies, industries, and universities arc used to augment
and reinforce the Institute staff in the development and presentation of technical material.
Individual course objectives and desired learning outcomes are delineated to meet specific program
needs through training. Subject matter areas covered include air pollution source studies, atmos-
pheric dispersion, and air quality management. These courses are presented in the Institute's resi-
dent classrooms and laboratories and at various field locations.
R. Alan Schueler
Program Manager
Northrop Services, Inc.
/James A. Jahnite
Technical Director
Northrop Services, Inc.
Jeanjf Schueneman
Chief, Manpower & Technical
Information Branch
-------
TABLE OF CONTENTS
Introductory Material
Course Description and Prerequisites 1
Background, Origin, and Philosophy 1
Educational Approach ' ' 3
Instruction for Preparation and Presentation of Course 4
PV.a/^lrl ^ o«-o _ _ 19
\j ilClvJVJ. J.O L.O .-...-.__ j_^
Course Goals and Objectives 14
Sample Agenda 21
Pre-test and Keys < 25
Quizzes and Keys 39
Post-test and Keys 61
Lesson 1 Registration and Course Information 79
Lesson 2 Introduction to Atmospheric Sampling 84
Lesson 3 Gas Measuring Instruments and their Calibration I, II 95
Lesson 4 High Volume Method 115
Lesson 5 Generation of Test Atmospheres 128
Lesson 6 Air Movers 141
Lesson 7 Problem Session I 147
Lesson 8 Principles of Gaseous Sampling 155
Lesson 9 Principles of Particulate Sampling 168
Lesson 10 Laboratory Safety Briefing 180
Lesson 11 Problem Session II 182
Lesson 12 Ambient Reference Methods for Gases 197
Lesson 13 Surveillance Networks 214
Lesson 14Site Selection 224
Lesson 15 Assuring High Quality Data 234
Laboratory Instructions 241
Siting Handout -
w
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INTRODUCTORY MATERIAL
COURSE #435 ATMOSPHERIC SAMPLING
This Instructor's Guide is to provide you as Course Moderator with assistance
in the preparation and presentation of Course #435 Atmospheric Sampling. It
will provide you with guidelines, instructions and some general information
that should facilitate your efforts in staging this course.
I. Course Description and Prerequisites
This course is an introduction to the measurement of gaseous
flow and to general techniques employed in atmospheric sampling.
Methods of calibration and use of flow rate measuring instruments
are discussed in lectures and investigated in the laboratories.
General techniques for sampling of the atmosphere as well as ref-
erence methods for sampling and analyzing criteria pollutants are
discussed in the lectures. Certain specific characteristics of gen-
eral sampling techniques (i.e., effects of storage time on bag
samples of pollutants, etc.) are investigated in the laboratories.
A scientific calculator is helpful for class and laboratory work.
Student backgrounds including general science and basic math skills
are essential.
II. Background, Origin, and Philosophy
The Environmental Protection Agency Air Pollution Training
Institute (APTI) provides courses in air pollution control
technology, ambient and source monitoring, and air quality
management. In July, 1976, Northrop Services, Inc. was con-
tracted to both present Training Institute Courses and to provide
support and technical services for the Institute as a whole.
Atmospheric sampling and other laboratory courses of particular
importance to governmental and industrial personnel concerned with
air pollution problems received early efforts of instructional
development to design the best possible training experiences for
the students. This required thorough examination of both the
materials for instruction and an examination of the characteristics
of the student audience. From such studies, the courses have been
revised and developed to provide training that enables every student
to achieve the specific course objectives.
The demographic characterization of students attending atmos-
pheric sampling classes has shown the following:
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Figure 1
Employer Course 435
Federal EPA 3%
Other Federal 8%
State Government 43%
Local Government 18% .
Industry 21%
Consultant 3%
Other 4%
Figure 2
Occupation Course 435
Administrator 2%
Chemist 17%
Engineer 18%
Ind. Hygienist 3%
Phys. Scientist 8%
Sanitarian 8%
Technician 40%
Other 3%
Figure 3
Educational
Background Course 435
High School 32%
Bachelor 50%
Master 16%
PhD 2%
Figure 4
Years
Experience Course 435
0-1 years 42%
2-4 37%
5 - 7 11%
8-10 3%
> 10 7%
Student intellectual characteristics were determined in the initial
contract year through standardized ability testing given to a total of
186 individuals in 10 different courses offered by the Institute. The
Course #435 sample produced the following percentile rank scores:
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Figure 5
Percentlie Rank
Verbal ability 74%
Numerical 56%
Spatial 38%
Reasoning 48%
Memory 41%
III. Educational Approach
The characterization studies mentioned above have indicated that
for APTI atmospheric sampling courses, the course content and instructional
methods should be explicit rather than implicit. Although formal
educational level tends to be generally high, the ability testing has
indicated the need for the course content to be presented in a careful
and logical and consistent order with the underlying principles and
relationships of given concepts being taught directly. At critical
junctures where students are required to visualize a concept, infer a
relationship, or visualize an added dimension, instruction is mediated
with the use of:
Graphic illustrations, usually in the form of 35 mm slides,
Lecture demonstrations,
In-class problem-solving,
Hands-on laboratory experience
Constant repetition and review of fundamental concepts
Course 435 is intended for personnel involved in sampling for atmos-
pheric pollutants, as well as those responsible for purchase, calibration,
and set up of atmospheric sampling equipment.
A typical person engaging in atmospheric sampling normally stays in
this type of work for 2 or 3 years before moving on to another position.
This creates a continual need to train new people entering this field
of work. Students attending #435 have ranged from high school graduates
to Ph.D.'s involved in research work. The average student (see Figures
2 and 3) has a bachelor's degree and is employed as a technician,
chemist, or engineer. In this course, the students come from industry
and governmental agencies (this provides a forum for interesting discus-
sions during the course presentations). Most of the students are also
just entering the field of air pollution, having less than one year of
experience. The approach taken in instructing Course #435 is to direct
the level of instruction towards the technical person with two to four
years of college, newly entering the field of air pollution. This
approach has succeeded, with most students gaining the knowledge they
desired through the course experience.
The variety of activities that the student experiences in Course
#435 aides in the assimilation of a great deal of knowledge. The first
day of the course is a very intensive and often stressful series of
lecture sessions. After this, laboratory experiences provide a more
balanced schedule and often are a reinforcement of the concepts developed
in Monday's lectures. The lectures for Tuesday through Thursday consti-
tute more general background to leave the students with a broader
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understanding of atmospheric sampling. Friday morning discussion sessions
are designed to provide the student with feedback on the lab experiences,
and to answer student questions for individual problem areas.
Every effort is made to answer any question asked by a student even
at the expense of some of the more advanced members of the class. In
fact, it has occurred that the simpler questions lead into details that
the class as a whole finds valuable. At the opposite end, the more com-
plex questions give the beginning atmospheric sampler an opportunity to
realize the complexities that can arise in performing atmospheric sampling.
IV. Instructions for Preparation and Presentation of Course
A. Responsibilities of Course Moderator
This course generally requires 4*g days for a complete presentation.
It can also be expected that anywhere from 10 to 16 hours of additional
preparation will be required by the individual designated Course Moderator.
Preparation and continuity are the principle responsibilities of the Course
Moderator who will coordinate all on-site activities both before and during
the course presentation. The actual tasks that are considered the direct
responsibility of the Course Moderator are:
1. Scheduling the course presentation.
2. Recruiting (hiring) and briefing instructors.
3. Preparation of classroom and teaching facilities.
4. Preparation of and distribution of course materials.
5. Presentation of introduction and other appropriate lectures.
6. Maintaining continuity throughout the course.
fc. Scheduling
The course itself is designed around a format using 16 lectures and 3
laboratory sessions, all of which are designed to fit into a 4% day time
frame of morning and afternoon sessions. All three laboratory exercises
are usually taught simultaneously with the students divided into three
groups, A, B, and C. Because the course contains a concentrated level of
involvement with rather technical material, it is recommended that no more
than eight (8) hours of class instruction be presented in one day.
The course materials contain segments, each listed below with its
recommended time and schedule placement.
Expected
Typical Time
Sequence Lesson Title Required
Day //I
Lesson //I Registration and Course Information 30 mins.
Lesson #2 Introduction to Atmospheric Sampling 1 hr. 15 mins.
Lesson #3 Gas measuring devices and
their calibration I and II 2 hrs.
Lesson #4 High Volume Method 1 hr.
Lesson #5 Generation of Test Atmospheres 1 hr. 15 mins.
Lesson #6 Air Movers 30 mins.
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Typical
Sequence
Lesson Title
Expected
Time
Required
Day
Lesson #7
Lesson #8
Lesson //9
Lesson #10
Laboratory
Session I
Day #3
Lesson
Lesson #12
Laboratory
Session II
Day #4
Laboratory
Session III
Lesson #13
Lesson #14
Lesson #15
Lesson #16
C. Instructors
Problem Session I
Principles of Gaseous Sampling
Principles of Particulate Sampling
Laboratory Briefing and Safety
Considerations
Lab 1 - Group A
Lab 2 Group B
Lab 3 Group C
Problem Session II
Ambient Reference Methods for
Gases I and II
Lab 1 Group B
Lab 2 Group C
Lab 3 Group A
Lab 1 Group C
Lab 2 Group A
Lab 3 Group B
Surveillance Networks
Site Selection
Assuring High Quality Data
Presentation of Laboratory Data
45 mins.
45 mins.
1 hr. 15 mins.
30 mins.
4 hrs.
45 mins.
2 hrs.
4 hrs.
4 hrs.
45 mins.
45 mins.
30 mins.
1 hr.
The four most important criteria in the selection of faculty for
this course are:
1. A knowledge of the current methods and procedures used in atmospheric
sampling.
2. Recent practical experience with a facility providing sampling.
3. Experience (and ability) to instruct adults using traditional
and non-traditional methods, materials, and techniques.
4. A positive attitude toward air quality management.
Before instructors are actually involved with instruction in the
classroom the course moderator should conduct thorough briefing and prepa-
ration sessions in which an overview of the entire course presentation is
given. Specific discussion of course and lesson objectives should result
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in an assurance that the instructors are well prepared and familiar with the
materials, procedures, and techniques that they will be using.
The course moderator should stress the difference in the role that
the instructor plays as compared to traditional university instruction
situations. All instructors should fully understand the function of the
course and lesson objectives and the relationship of each objective to
their particular materials and to the pre- and post-testing.
It may be particularly helpful to the instructors if they are able to
sit in on early sessions of the course presentation, so that they get a
feel for the way the students are oriented to the material and be able to
incorporate the strengths and background experiences of the students into
the various instructional sessions.
Preparation must be stressed to all prospective instructors. Thorough
familiarization with all the prepared materials is essential for even
"expert" instructors. Laboratory sessions require additional preparation
and should include a complete run-through to check out the methods and
equipment before ever presenting them to the students. Remember that
Murphy's law will always hold in a student laboratory exercise: "What
ever can go wrong, will!"
D. Physical Setting
1. Classroom a classroom of approximately 1200-1500 square feet is
. needed to accommodate 28-^30 people (24 students, 3 instruc-
tors, 1 evaluator); all students should have desks or tables-
others need chairs only
35 mm slide projector
overhead projector
screen at least 6 feet by 6 feet
chalk board, erasers and chalk
2. Lab Facilities should ideally have 3 separate rooms (can go with 2
rooms or one large room)
total of 10 people in each lab at one time
Lab 1: Hi Vol Lab 25 feet of standard lab bench top space ,
7 to 10 electrical outlets , No less than two
20 amp circuits ,
extremely noisy lab ideally should have its
own room.
Lab 2: Flow Lab 30 feet of standard lab bench top space,
6 to 10 electrical outlets, best to have two
20 amp circuits, but not necessary ,
tap water supply is nice.
Lab 3: Test Atm. 25 feet of standard lab bench top space,
6 to 8 electrical outlets (only one 20 amp
circuit necessary).
Lab exhaust hood is best (can possibly do
without),
vacuum source (^20-25 inches of mercury)-
Total of 80 feet of standard lab bench top space.
More complete and specific laboratory instructions and equipment
requirements are found in the final section of this guide.
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E. Course Materials
In addition to the course lecture and lesson outlines and the audio-
visual materials, this package contains the following material for distri-
bution to the students:
1. APTI Training Manual: "Atmospheric Sampling"
2. Student Laboratory and Exercise Manual
3. Pre-test
4. Post-test
5. Daily quizzes I, II and III
6. Course Goal and Objectives
7. List of Designated Reference and Equivalent Methods*(this publication
is updated frequently, the most recent version will be supplied)
8. "Optimum Site Exposure Criteria for S02 Monitoring" EPA-450/3-77-013 p. 31
F. Audio-Visual Materials
The visuals package accompanying these materials includes 47.4 35mm
slides. The specific lessons are as follows:
Lesson 1 No slides
Lesson 2 38 slides
Lesson 3 67 slides
Lesson 4 61 slides
Lesson 5 34 slides
Lesson 6 17 slides
Lesson 7 No slides
Lesson 8 34 slides
Lesson 9 53 slides
Lesson 10 No slides
Lesson 11 No slides
Lesson 12 62 slides
Lesson 13 32 slides
Lesson 14 55 slides
Lesson 15 21 slides
These slides are either supplied as a part of the Instructional Resource
package or are available for reproduction through the Air Pollution
Training Institute.
G. Laboratory Materials and Equipment
The following list indicates the equipment and materials required for
successful presentations of the lab sessions using the procedures
contained in the Course 435 Laboratory Manual.
*Copies can be obtained from: Office of Research and Development
EMSL (Environmental Monitoring Systems Lab)
US EPA-MD 77
Environmental Research Center
Research Triangle Park, NC 27711
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EQUIPMENT LIST - LAB #435 ATMOSPHERIC SAMPLING
LAB 1 - CALIBRATION OF A HIGH VOLUME SAMPLER
1. Portable "in the field" calibration kit (optional)
2. 2 - Pressure transducers (Dixon meters) and Hi-vol blowers.
3. 2 - Visifloat and Hi-Vol blowers (used with rootsmeters)
4. 2 - Rootsmeters with stands
5. 4 - Water manometers - capable of measuring 16 inches or more
6. 2 - Mercury manometers - capable of measuring 160 mm or more
7. 4 - Ring stands and 10-3 prong holder clamps
8. 2 - Sierra or other make constant flow controller units
9. (Optional calibrator to correspond to constant flow unit)
10. One cartridge "type" filter holder (optional)
11. 2 - Orifice units (calibrator with load plates)
12. 4 - Electrical outlet - multiplugs - (extension cords ok)
13. 2 - Reference flow devices (Ref) (Dexco, Inc.)
14. Tubing - thin walled - Tygon.
15. Miscellaneous - (A) rubber gaskets
(B) one box of clean filters (glass fiber)
(C) oil - (rootsmeter grade oil)
(D) Mercury
(E) Distilled water with added coloring - ten drops/liter
^0, e.g. fTuorescein green dye
LAB 2 - FLOW MEASURING INSTRUMENTATION
(For two identical set-ups of each)
1. 2 - Mass flowineters (0-3 liter range)
2: 2 - Displacement bottles (10 liter capacity)
3. 2 - Two liter class "A" volumetric flasks
4. 2 - Wet test meters (1 liter/rev)
5. 2 - Stopwatches
6. 2 - Vacuum pumps (capable of pulling 25" Hg vacuum)
7. 4 - Smog bubblers
8. 8 - Gas metering valves
9. 6 - Vacuum gages (0-30 "Hg vacuum range)
10. 4 - 500 ml Erlenmeyer flasks (plastic)
11. 2 - Particulate filters and holders (Teflon filters)
12. 2 - Moving soap bubble meters (graduated 0-500 ml)
13. 500 ml soap bubble solution
14. 2 - 250 ml beakers
8
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LAB 2 - FLOW MEASURING INSTRUMENTATION (cont.)
15. 10 - Metal squeeze clamps for glass sockets
16. 4 - One-holed stoppers (rubber)
17. 2 - 2-holed stoppers (rubber)
18. 2 - 500 ml washbottles
19. 10 - ring stands
20. 4 - Mounting rods (horizontal)
21. 28 - 3-prong clamps
22. 2 - rotameters (glass) (0-3£ range)
23. 2-23 gauge hypodermic needles
24. 36 - clamp holders with 45° angle thumbscrews
25. 40' - 50' of vacuum tubing (rubber)
26. 6' - thin walled tubing (rubber)
LAB 3 - STANDARD TEST ATMOSPHERES
EQUIPMENT REQUIRED*
1. Continuous S02 Analyzer - (e.g. Teco Model 43)
2. Continuous NO -N09-N0 Analyzer (e.g. Bendix 8102)
X +
3. Portable Dilution system (e.g. Bendix Model 8861D)
4. Portable permeation System (e.g. Bendix Model)
5. Misc. (a) hardware - Swagelok fittings - clamps
(b) tubing - e.g. Teflon and/or glass
(c) mixing bulbs (glass) and/or glass manifold
(d) support gases needed (1) Zero air
(2) NO bottled gas. (50 ppm)
(e) permeation tube 1 yg/min S02 @ calibrator/
permeation oven temperature
*May substitute other equipment so long as the principles put forth in
the lab write-up are demonstrated i.e., permeation/dilution system
utilized to calibrate monitor and gases and their dilution as an
alternate calibration method.
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H. Lesson Plan Use
Each lesson plan module is designed to serve as:
A. Source of lesson objectives
B. Content guide for instructor
C. Lecture outline
D. Directions for use of visual aids
E. Guidelines for approach to the lesson.
Generally the lesson plans are organized as straight outlines with
additional instructions and keys to the visuals found on the right
hand border of the page. On occasion it was felt that the instructor
might need more specific information and a more narrative format is used
for the subject matter to be adequately covered.
Each lecture plan outline is carefully timed. Instructors should give
attention to observing time schedules and "pace" of the lessons to be
given.
Instructors must be familiar with the visual aids and handout materials
before attempting to present any lesson.
The visuals are keyed using number references that are also found on the
slide. The number identifies the lecture and sequence of the slide.
Thus, L2-16 identifies a slide in lecture 2 that comes before L2-17
and after L2-15. Also, each slide is provided with a "thumb spot" that
should be in the upper right hand corner of the frame (under your thumb)
as the slide is loaded into a carousel. This should prevent slides
from being loaded backwards or upside-down.
Instructors may wish to vary slightly from the format or content for a
given lesson but should be cautioned that the schedules and lesson
objectives must be maintained. Variations should be in the direction of
greater student participation. Instructors should remember that the exams
reflect the lesson objectives as presented through these lesson outlines.
I. Grading Philosophy
The guidelines for grading student's performance in "Atmospheric Sampling"
and granting Continuing Education Units (CEU's) are as follows:
The student must:
attend a minimum of 95% of all scheduled class and laboratory
sessions;
complete and hand in copies of all laboratory data derived in
the laboratories; and
achieve an average course grade of 70% or better derived as
follows:
1) 25% from daily quizzes
2) 45% from final examination
3) 20% from laboratory reports
4) 10% from homework completion
10
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J. Other Logistics
Since the Course Moderator will need to consider a great variety of
logistic and instructional concerns, the following checklist is provided
to serve as a guide to meeting these responsibilities.
The course developers have tried to provide you with as much
information and materials as possible to enable you to present a unique
and exciting education venture.
GOOD LUCK.
11
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CHECKLIST
of Activities
For Presenting the Course
A. Pre-Course Responsibilities:
_ 1. Reserve and confirm classroom(s) and laboratories, including
size, "set-up," location and costs (if any).
_ 2. Contact and confirm all faculty (speakers) for the course(s),
including their A-V requirements. Send material (i.e., slides
and instructor's manual) to them. One or more pre-course
instructor's meetings are advisable.
__ 3. Reserve hotel accommodations for faculty.
_ 4. Arrange for and confirm food service needs (i.e., meals,
coffee breaks, water, etc).
_ 5. Prepare and reproduce final ("revise" if appropriate)
copy of the detailed program schedule.
_ 6. Reproduce final registration/attendance roster, including
observers (if any) .
_ 7. Prepare name badges and name "tents" for students and faculty.
_ 8. Indentify, order, and confirm all A-V equipment needs.
_ 9. Prepare two or three 12 in. x 15 in. signs on posterboard for
posting at meeting area.
_ 10. Arrange for and confirm any special administrative assistance
needs on-site for course, including "local" address of welcome,
11. Obtain copies of EPA manuals, and pamphlets.
12. Pack and ship box of supplies and materials one week prior
to beginning of course (if appropriate) .
13. Arrange and confirm the availability of satisfactory laboratory
equipment and facilities.
14. Set up needed equipment in the laboratory setting and make
sure all equipment and instruments are operating correctly.
15. Have run through of lab exercise with instructors.
12
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CHECKLIST (Cont.)
B. On-Site Course Responsibilities
1. Check on and determine final room arrangements (i.e., tables,
chairs, lectern, water, cups, etc).
2. Set up A-V equipment required each day and brief operator
(if supplied)
3. Post signs where needed.
4. Alert receptionist, phone operator(s) watchmen, etc., of name,
location, and schedule of program.
5. Conduct a new speaker(s) (i.e., instructor) briefing session
on a daily basis.
6. Verify and make final food services/coffee arrangements
(where appropriate).
7. Identify and arrange for other physical needs as required
(i.e., coat racks, ashtrays, etc).
8. Make a final check on arrival of guest speakers (instructors)
for the day.
C. Post-Course Responsibilities
1. Request honorarium and expense statements from faculty;
order and process checks.
2. Write thank-you letters and send checks to paid faculty.
3. Write thank-you letters to non-paid guest speakers and others
who may have contributed to the success of the course.
4. Prepare evaluation on each course (including instructions,
content, facilities, etc).
5. Make sure A-V equipment is returned.
6. Return unused materials to your office.
13
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COURSE 435
ATMOSPHERIC SAMPLING
COURSE GOAL
The goal of this course is to introduce students to the concepts of atmospheric
sampling for ambient levels of both gaseous and particulate pollutants. These
concepts include selection of sampling sites, selection of sampling methods, and
selection of calibration techniques.
COURSE OBJECTIVES
After completion of this course, the student will be able to:
a) calibrate (making all appropriate corrections for pressure drops,
ambient temperature, atmospheric pressure, etc.) the following
flow measuring devices:
1) Wet test meters
2) Rotameters
3) Critical orifices
4) Sub-critical orifices
5) Mass flow meters
6) Bubble flow meters
b) employ the devices listed in (a) to determine flow rates in various
sampling trains and through various pieces of monitoring equipment
covered during the course.
c) generate, analyze, and use controlled atmospheres of a gaseous
pollutant to calibrate or examine certain parameters of gaseous
sampling and analysis methods.
d) describe the operation of the various flow measuring devices and their
associated calibration procedures, [see (a) above]
e) describe the analytical principles involved in gaseous sampling with .
emphasis on the criteria gaseous pollutants.
f) describe the various principles and instrumentation involved in
particulate sampling.
g) describe the Federal Reference Method for particulates (TSP).
h) identify the manual procedure or measurement principle and associated
calibration procedures of the reference methods presently specified for
the analysis of ambient gaseous and particulate criteria pollutants.
i) identify the techniques used in siting monitoring stations.
j) identify the considerations involved in designing surveillance
networks.
k) identify general characteristics of Quality Assurance.
14
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1) interpret the effects of variables (i.e., flow rate, temperature,
pressure, placement of rotameter in sampling trains, direction of
flow through critical orifices, etc.) on the accuracy and precision
of atmospheric sampling and analysis.
m) select the appropriate pieces of equipment to make up a sampling
train (i.e., pumps, flow control and measuring devices, etc.) giving
consideration to such parameters as pump capacity,. interferences,
flow rate required, etc.
LESSON OBJECTIVES
Lesson 1 - Registration and Course Information and Administering Pre-Test
Lesson 2 - "Introduction to Atmospheric Sampling"
At the completion of the lecture, the student will be able to:
recall the general reasons for and types of sampling
encountered in ambient surveillance .
discuss the effects of temperature and pressure on the
volume of an ideal gas.
recognize the ideal gas law.
Define the concept of molar volume and explain its use
in atmospheric sampling.
convert gas volumes (including the molar volume) to the
conditions of standard temperature and pressure currently
specified for EPA ambient reference methods.
perform rudimentary sampling calculations such as determination
of volume sampled, amount of pollutant collected, and
conversion of yg/nr' to ppm.
Lesson 3 - Gas Measuring Devices and their Calibration
After completion of this lecture, the student will be able to:
define calibration
distinguish between primary, intermediate, and secondary gas
flow rate and volume standards
distinguish among each of the following flow measurement
instruments given operational and/or physical characteristics:
a) wet test meters
b) rotameters
c) critical or limiting orifices
d) sub-critical orifices
e) moving bubble meters
15
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Identify the general characteristics of the following flow
measurement instruments:
a) spirometers
b) displacement bottles
c) frictionless pistons
d) dry test meter
e) rootsmeters
f) pitot tubes
f) mass flow meters
Apply appropriate factors to correct volume and flow rates
for temperature and pressure
Distinguish between volume, rate and velocity meters.
Lesson 4 - "High Volume Method"
The student will be able to:
Briefly describe the components of a standard high volume
sampler
List the procedure for properly obtaining a high volume
suspended particulate sample.
Outline the procedure for calibrating a high volume
calibration orifice using a rootsmeter.
Recall and use the method for recalculating the orifice
calibration curve when different temperature and pressure
are involved.
Describe and use the procedure for calibrating a high volume
unit containing a visifloat or transducer.
Discuss briefly the audit procedure for the high volume
sampler.
Calculate the total suspended particulate concentration for
a high volume sample, given filter weights, flow rate, sampling
time.
Identify the common interferents (errors) associated with total
suspended particulate measurement using the reference high
volume method.
Lesson 5 - "Generation of Test Atmospheres"
After completion of this lecture, the student will be able to:
identify the stability problems associated with low level
cylinder gasesspecifically, SO , N02, and CO.
16
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Given the appropriate data, perform all calculations
necessary to determine the concentrations of gases
produced by permeation systems and dilution systems
Outline at least two methods for actually metering
diluent gas into a static or dynamic system .
Recognize and identify the adsorbents and apparatus
necessary to produce zero air.
Define NBS traceability in terms of Standard Reference
Materials and non-NBS standards.
Describe the construction and use of permeation tubes.
Lesson 6 - "Air Movers"
The student will be able to:
List six considerations in selecting an air mover for
a given sampling situation.
Differentiate between positive displacement and centrifugal
pumps.
t Describe the operation of the following air movers
a. Piston pump
b. Diaphragm pump
c. Vane pumps
d. Ejectors
e. Liquid displacement
Lesson 7. - Problem Session I
Lesson 8 - "Principles of Gaseous Sampling"
The student will be able to:
Distinguish between the principles of grab and integrated
gas sampling.
Identify the characteristics of adsorption, absorption, and
freezeout sampling.
List at least two common materials used as adsorbents.
List the type of samples most commonly collected by
adsorption and freezeout sampling.
Describe at least one type of analytical procedure for
quantifying gaseous pollutants'collected by adsorption.
List at least two potential problems common to adsorbent
collection and analysis of gases.
List at least two factors affecting collection efficiency
of an absorber.
Distinguish the difference between physical and chemical
absorption.
17
-------
Lesson 9 - "Principles of Particulate Sampling"
The student will be able to:
Describe three principles of particulate collection
devices: gravity, filtration, inertia, and recall
examples of each.
Identify at least two common errors in inertial collection
of particulates.
Describe the mechanism for size fractionation by inertial
sampling.
Define collection efficiency of an impaction device.
List four properties of aerosols and four properties
of collecting devices which affect the collection
efficiency of impactors.
Discuss how the following particulate samplers operate
and what each is used for:
a. Cascade Impactor
(1) Andersen Impactor
b. Cyclone Samplers
Describe the rationale for size fractionation of ambient
particulate matter.
* Define the differences between respirable and non-respirable
particulate matter.
Describe how the dichotomous sampler fractionates respirable and
non-respirable particulate matter.
Discuss some of the advantages and disadvantages of each of
the three types of filter materials.
Lesson 10 - Laboratory Briefing and Safety
Lesson. 11 - Problem Session II
Lesson 12 - "Ambient Reference Methods for Gases"
At the conclusion of this lecture, the student will be able to:
Distinguish between a Reference Method or Measurement Principle and
Calibration Procedure and an Equivalent Method for ambient air
pollutants.
List the gaseous ambient pollutants now specified as criteria
pollutants.
List the Reference Method or Measurement Principle and
Calibration Procedure currently specified for each criteria
pollutant.
Describe the operating principles of each Reference Method.
18
-------
Lesson 13 - "Elements of Surveillance Networks"
The student will be able to:
Describe the need to specify the objectives of sampling tied to
intended use of the data as the first step in designing the net-
work.
Cite the major sources of EPA guidance on monitor siting.
Discuss the composition of SAMWG and the status of its
recommendations
Defend the need for a quality assurance program.
Describe an ambient m.onitoring network including its major
subsystems.
Lesson 14 - "Site Selection"
The student will be able to:
Discuss the need to properly site pollutant monitors
Locate the documents for guidance on siting pollutant
monitors
Outline the procedure used to site monitors as described in
the guidance documents.
Locate regulations associated with monitor siting
Recognize factors involved in selecting proper siting of
monitors.
Lesson 15 - "Quality Assurance Overview"
The student should be able to:
Define Quality Assurance
State three major reasons why a quality assurance program
is important in sampling and analyzing atmospheric
pollutants.
Recognize that many different quality assurance elements are
involved in the process of producing valid data, list several
of those which are directly applicable to the individual who
samples and analyzes atmospheric pollutants.
Recognize that QA principles and specified QA methodologies
are located in Vols. I & II of the Quality Assurance Handbook
and 40 CFR Appendixes A & B.
Recall that EPA conducts an Interlaboratory Performance
Audit Survey and that participation (voluntary at present)
will be required by 1983 in accordance with SLAMS provisions.
19
-------
LABORATORY OBJECTIVES
"Lab 1: High Volume Sampler Calibration"
At the conclusion of this laboratory session the student will be
able to:
Calibrate an orifice calibration unit with a rootsmeter
Calibrate, according to the Reference Method, a hi-vol equipped
with a visi-float and a hi-vol sampler equipped with a recording
pressure transducer.
Perform a field audit on the flow calibration of a hi-vol using
a ReF (reference flow) device.
Perform a check on the constant flow performance of a constant flow
hi-vol.
"Lab 2: Flow Calibration"
At the conclusion of this laboratory session, the student will be able
to:
Calibrate a wet-test meter using a water displacement technique.
Calibrate a rotameter in a bubbler train using a mass flow
meter. The student will be able to describe the effects that
variation in AP will produce on flow measurements.
Describe how various factors affect critical orifice flow.
These factors include:
a) determination of critical vacuum
b) effects of upstream resistance
c) effects of directional placement of a common
orifice (hypodermic needle).
Calibrate a mass flow meter.
"Lab 3: Controlled Test Atmospheres"
At the conclusion of this laboratory session, the student will be able
to:
Use bottled gas/dilution, dynamic test atmospheres to prepare
a calibration curve of concentration vs. instrument response.
Use permeation tube/dilution, dynamic test atmospheres to
prepare a calibration curve of concentration vs. instrument response.
Perform all calculations necessary for the utilization of the test
atmospheres listed above.
20
-------
SAMPLE AGENDA
Name and address of
agency conducting course
(Dates of course)
435Atmospheric Sampling
Course location
Acknowledgement
of role of other
agencies, if any,
in conduct or
support of
presentation.
Name of course
director
DAY & TIME
SUBJECT
SPEAKER
MONDAY
8:30
9:00
9:45
«:00
:00
12:45
1:45
2:45
3:00
4:15
4:45
Registration and Course Information
Pretest
Introduction to Atmospheric Sampling
Gas Measuring Devices & Their Calibration I
LUNCH
Gas Measuring Devices & Their Calibration II
High Volume Method
BREAK
Generation of Test Atmospheres
Air Movers
ADJOURN
HOMEWORK:
1. Problem Set 1 (Due Tuesday at 8:30 a.m.)
2. Read Appropriate Lab Procedures
TUESDAY
8:30
Problem Session
If course is not conducted by EPA, but EPA/APTI materials are used, it would be
appreciated that an acknowledgement appear here.
21
-------
#435 - ATMOSPHERIC SAMPLING
Page 2
I
Y & TIME
SUBJECT
SPEAKER
TUESDAY (Continued)
9:15
9:30
10:15
10:25
11:40
12:30
1:00
5:00
WEDNESDAY
8:30
9:15
9:30
10:30
10:45
11:45
1:00
Quiz I
Principles of Gaseous Sampling
B R E AK
Principles of Particulate Sampling
LUNCH
Laboratory Briefing & Safety
Laboratory Session I
Lab 1 - Group A
Lab 2 - Group B
Lab 3 - Group C
ADJOURN
HOMEWORK:
1.
2.
3.
Problem set 2 (Due Wednesday at 8:30 a.m.)
Read Appropriate Lab Procedures
Complete Lab Report for Lab Session I (Due Wednesday
at 1:00 p.m. )
Problem Session
Quiz II
Ambient Reference Methods for Gases I
BREAK
Ambient Reference Methods for Gases II
L U N C H & Work Session
Laboratory Session II
Lab 1 - B
Lab 2 - C
Lab 3 - A
ADJOURN
WMEWORK:
1. Complete lab report for Lab Session II (Due Thursday @ 8:30 a.m.)
2. Read Appropriate Lab Procedures
3. Review problem sets
22
-------
#435 - ATMOSPHERIC SAMPLING
Page 3
DAY & TIME
SUBJECT
SPEAKER
THURSDAY
8:30
12:30
1:30
2:00
2:30
3:15
3:30
4:15
4:45
Laboratory Session III
Lab 1 - C
Lab 2 - A
Lab 3 - B
LUNCH
Work Session (Report for Lab Session III due
at end of this session)
Quiz III
Surveillance Networks
BREAK
Site Selection
Assuring High Quality Data
A D J C U R N
HOMEWORK:
1. Study for Final Examination. Be sure to review
pre-test, course and lecture objectives, daily
quizzes, and lab materials. Be prepared to present
lab data in class.
FRIDAY
8:30
9:30
10:30
11:30
11:45
12:00
Presentation of Laboratory Data
(Graded lab reports returned to class)
Review & Study
Final Exam
Review of Final Exam
Course Evaluation
ADJOURN
23
-------
COURSE 435
REQUIREMENTS FOR AWARD OF CERTIFICATE OF COURSE
COMPLETION AND CONTINUING EDUCATION UNITS
Three (3) Continuing Education Units (CEU's) will be awarded along with certificate
to those students who:
attend a minimum of 95% of all scheduled class and
laboratory sessions;
complete and hand in copies of all laboratory data
derived in the laboratories; and
achieve an average course grade of 70% or better derived
as follows:
1) 25% from daily quizzes
2) 45% from final examination
3) 20% from laboratory reports
4) 10% from homework completion
ALL PRE-TEST, POST-TESTS, AND QUIZZES IN THIS COURSE ARE INTENDED TO BE CLOSED-BOOK.
STUDENTS ARE NOT ALLOWED TO USE ANY ADDITIONAL MATERIAL, OTHER THAN A SCIENTIFIC
CALCULATOR. SUGGESTED TIME ALLOTMENTS FOR EACH ARE AS FOLLOWS:
PRE-TEST 45 MINUTES QUIZ 1. 15 MINUTES
FINAL EXAM 60 MINUTES QUIZ 2. 15 MINUTES
QUIZ 3. 30 MINUTES
24
-------
LESSON PLAN
D
TOPIC: REGISTRATION, COURSE
INFORMATION, AND PRE-TEST
COURSE:435-Lesson #1
LESSON TIME: 75 min.
PREPARED BY: Northrop
Services, Inc.
DATE: 1/12/79
LESSON GOAL:
LESSON OBJECTIVES:
To introduce student to the overall structure of the course.
At the end of this session the student should know:
1. That this Course 435: Atmospheric Sampling, is presented
by . (Area Training
Centers should recognize their home institution, the
Air Pollution Training Institute, and MTIB, Manpower
and Technical Information Branch of Control Programs
Development Division.)
2. The name of all instructors and their affiliation
3. Phone number where a student may receive messages
during the course offering.
4. Course goals and objectives
5. Requirements for passing the course
a. Completed registration card - Social Security Number
optional, required for CEU's} however.
b. Pre-test
c. 95% attendance - minimum
d. Daily quizzes
a. All laboratory work completed and turned in
f. Post-test
g. Minimum overall grade of 70% (See Agenda for breakdown)
h. Critique
6. Teaching approach used in this course
79
-------
7. The location of
a. Restrooms
b. Refreshments
c. Laboratories
8. Address and phone number of EPA - Air Pollution Training Institute
U.S. EPA, ERC
APTI, MD20
RTF, NC 27711
919-541-2766
FTS-629-2766
SUPPORT MATERIALS:
1. Student materials package
2. Blackboard and chalk or overhead projector
80
-------
CONTENT OUTLINE
A
Course: 435 Lesson 1
Lecture Title: REGISTRATION AND COURSE INFORMATION
NOTES
I. Introduce instructors
A. Names and affiliation
B. Experience
C. Areas of expertise
II. Institutional setting
A. If APTIexplain EPA/Contractor relationship
B. If Area Training Center explain relationship with
APTI-MTIB and acknowledge source of training materials
C. Other institutions offering this courseprovide state-
ment on their specific situation and acknowledge source
of training materials
III. Logistics of the course location - Recognize host for field
location
A. Message phone number
B. Restrooms
C. Refreshments antj Restaurants
D. Laboratory Location
E. Emergency Exits and Emergency alarm system
F. No smoking in classroom or lab
G. Parking
IV. Description of teaching methods
A. Training
1. Course directed at training students to perform
a specific skilled task.
B. Instructors
1. Will be there to help student become trained
2. Will add their experience and expertise to
the training
3. Encourage questions
C. Approach
1. Teach the basic math and sampling techniques
2. Solve new problems by applying these fundamentals
81
A simple floor
plan on chalk board
or overhead is help
ful.
-------
CONTENT OUTLINE /£
Course .435Lesson 1
Lecture Title: REGISTRATION AND COURSE
\
UJ
a
Page.
NOTES
V. Course Requirements
A. Completed registration card (Blue Card)
B. Pre-test
C. 95% attendance - minimum
D. All laboratory work completed and turned in
E. Daily quizzes
F. Post-test
G. Minimum overall grade of 70%
H. Course critique completed and turned in
VI. Materials - have students check that they have
A. APTI Training Manual: "Atmospheric Sampling"
B. Student Exercise Manual (2 problem sets and lab
exercises)
C. Agenda
D. Roster
E. Chronological Schedule of Courses
F. Note paper
G. Registration card
H. Course and Lesson Objectives
VII. Pre-test and registration
A. Explain that the pre-test
1. Tests what they know as they enter the course
2. Does not count in the final course grade
3. Will be correlated to post-test grades to measure
actual learning in the course
4. Students should not guess at answers on pre-test
B. Registration card - completely filled out
Mailing List Form - complete only if you want more
than 1 chronological schedule of courses
C. Begin the pre-test and tell students to take a break
after the test
82
-------
CONTENT OUTLINE f§
Course: 435 Lesson 1
Lecture Title: REGISTRATION AND COURSE
i
Page .3 of ^
NOTES
D. Collect all tests, registration cards, and mailing
list forms - grade tests promptly and report low,
high, and average grades.
E. At this time, it is recommended NOT to review the
exam. Answers may be given to review at a later
time after the lecture material is covered.
83
-------
LESSON PLAN
TOPIC:INTRODUCTION TO ATMOSPHERIC
SAMPLING
COURSE: 435 - Lesson #2
LESSON TlME'Apprpx. 1 hr, 15 min.
PREPARED BY: NMthrop DATEl-12-79
Services,
LESSON GOAL:
To introduce the student to the reasons, operations, types, and
methods involved in atmospheric sampling. To develop a working
knowledge of gas properties, specifically those affecting gas volume
by use of the ideal gas law.
LESSON OBJECTIVES:
The student will be able to:
1. recall the general reasons for and types of sampling encountered in
ambient monitoring.
2. discuss the effects of temperature and pressure on the volume
of an ideal gas.
3. recognize the ideal gas law and be able to use it in solving
problems in gaseous sampling.
4. define the concept of molar volume and explain its use
in atmospheric sampling.
5. convert gas volumes (including the molar volume) to the
conditions of standard temperature and pressure currently
specified for EPA ambient reference methods.
6. perform rudimentary sampling calculations such as determination
of volume sampled, amount of pollutant collected, and
3
conversion of yg/m to ppm.
84
-------
SUPPORT MATERIALS AND EQUIPMENT:
1. Objective Handout
2. Slide Projector and 35 nun slides
SPECIAL INSTRUCTIONS:
SELECTED REFERENCES:
This lecture begins with a general introduction to ambient sampling
although each general concern should be illustrated with a con-
crete example. The calculations involving the ideal gas law and con-
versions to EPA Standard conditions are used throughout the course and
students having difficulty with these calculations should work
Problem Set I carefully. Student participation should be encouraged
throughout the lecture by asking class questions and asking students
to draw on their experience (although possibly limited) to
answer questions.
Seinfeld, J. H., Air Pollution, McGraw-Hill, Inc., 1975
Barrow, G.M., Physical Chemistry, Chapt. 1 "Properties of Gases",
McGraw-Hill, Inc., 1966.
Hollowell, C. D., McLaughlin, R. D., Stokes, J. A., "Current
Methods in Air Quality Measurements and Monitoring" IEEE
Transactions on Nuclear Science, Vol. NS-72, April 1975.
85
-------
CONTENT OUTLINE £g
Course: 435-Lesson //2
Lecture Title: INTRO. TO ATMOSPHERIC SAMPLING
\
O
NOTES
Review Lecture objectives with the students
INTRODUCTION TO ATMOSPHERIC SAMPLING
I. Reason for Sampling
to obtain a true representation of the pollutant level
at a given point and time (emphasis on true)
A. Factors Affecting True Value
1. Conditions of Atmosphere at Sample Time
2. Pollutant Characteristics
B. Errors Affecting Sampling
1. Systematic Errors - errors that occur due to re-
petitive procedure - noted by biased results.
2. Random Errors - nonsystematic errors that occur
due to changes in procedure, human error, etc.
II. Sampling Operations-
A. Collection Process - gives volume of air sampled
B. Analysis - gives amount of pollutant - together they
give air pollution results - concentration of pollutant
in mass/volume of air.
C. Manual method (e.g. wet-chemical) sampling - involves two
distinct processes - the collection followed by analysis
D. Continuous Method Collection and Analysis
1. Performed simultaneously yielding a direct ppm or
o
yg/m readout.
Continuous monitoring instrumentation(e.g.
NO-NO_-NO chemiluminescent monitors, pulsed fluore-
2. X
scent SO- monitors) gives this type of value(s).
III. Components of a Sampling Train
A. Sample Collection Device or Contaminant Detector or
Collector.
B. Air Mover
86
C. Flow Measuring Device
L2-1
L2-2a
b
L2-3
Note: Ask Students
for additional
sources of systemat
or random errors.
Briefly attempt to
get positive Studen
participation.
L2-4a
L2-4b
L2-5
L2-6
L2-7
-------
CONTENT OUTLINE £X
Course: 435 - Lesson #2 \
Lecture Title: INTRO. TO ATMOSPHERIC SAMPLING
\
UJ
'J
T
2 Of.
NOTES
Illustrate these components on a typical dynamic sampling
unit.
IV. Sampling Types/Methods
A. Continuous Sample - no collection involved. Air sample
analyzed as it is collected
B. Grab Sample - taken without respect to time no flow
rates involved. (Usually less than 1 minute)
C. Condensate - condense pollutant from gaseous phase to
liquid phase for measurement.
D. Impinged Material - uses inertia of pollutant for col-
lection.
E. Sorbed Materials - collection onto or into collection
material.
V. Sample Handling Concerns
A. Loss of Materials of Interest
B. Contamination
C. Storage
D. Identification
Use specific examples to illustrate the concerns
listed. For example, exposure to high temperatures
may result in deaorption of a pollutant collected
on a solid adsorbent. Storage and temperature stability
of SO collected by the reference method. Clear identi-
fication for legal reasons etc.
VI. Sampling Representativeness, Precision, Accuracy
A. Representativeness - What type sample will best show
the representative pollutant concentration. Must consider
the time of day, averaging time, season of year, location,
etc.
B. Precision - reproducibility: refers to the extent to
which each value in a given set of measurements agrees
with the mean of the observations.
C. Accuracy - correctness refers to the extent to which a
given measurement agrees with the true but unknown
value of the quantity being measured..
! 87
L2-8
L2-9
Illustrate each
type with a current
application. Ask
class for additiona
examples.
L2-10
a
b
c
d
This is also a good
point to ask for
specific examples
from students.
L2-11
L2-12
L2-13
-------
PF CONTENT OUTLINE /S%
^^^o^^jgj i o V^Sr7 «?
^^|^^M Course. 435- Lesson #2 %^*'*^^?
ULJIBP Lecture Title: INTRO. TO ATMOSPHERIC SAMPLING ^PRO^
INTRODUCTION TO GAS SAMPLING
In Atmospheric Sampling we are primarily concerned with sampling
for and in gases. It is, therefore, necessary to understand the
basic properties of gases which affect sampling.
I. Factors Affecting Gas Properties
A. Temperature
1. Temperature Scales
a. Fahrenheit 212° boiling point HO
32° freezing point H.O
£.
b. Celsius 100° boiling point HO
0 freezing point HO
PnrjP 3 nf 7
NOTES
i^HMH^M
L2-14a
2. Absolute Temperature - temperature measured on the j
Absolute Scale - which is based on absolute zero -
a hypothetical temperature characterized by com-
plete lack of heat (no energy) and equivalent to
approx. -273.16°C or -459.67°F.
Gas properties referenced to absolute zero
(a) Rankine corresponds to Fahrenheit(°F) + 459.67
(b) Kelvin corresponds to Celsius (°C)+ 273.16
3. Standard Temperature
Since temperature affects volume of gas it is
necessary to have a standard temperature to base
all results on.
For Ambient Air Monitoring, EPA1 s Std. Temp is:
25°C or 298°K
B. Pressure
(3 Types of Pressure)
1. Barometric or Atmospheric Pressure (P ) . Weight
exerted by atmospheric air. Standard (P, )
b
(Pressure measured at sea level and 0°C) = 760mmHg 01
1 atmosphere.
2. Gage Pressure (P )
O
Pressure measured on gage in sampling system.
Difference in system pressure with respect to atmos-
pheric pressure (maybe positive or negative) .
88
L2-14b
L2-15a
L2-15b
-------
CONTENT OUTLINE /£
«ii^B«»"«""""""«"""^""""«""i^"i » v^tt^
Course: 435 - Lesson #2
Lecture Title: INTRO. TO ATMOSPHERIC SAMPLING
Page.
of^L
NOTES
,
abs
, + P
b g
L2-15C
Absolute Pressure (P , or P )
abs a
Pressure of system referenced against no pressure.
Gas properties are referenced against
absolute pressure.
Standard Pressure
EPA Standard = 760 mm of mercury or 1 atmosphere
Ideal Gas Laws
Relationship between volume and pressure, temperature, and
number of moles of gases.
A. Boyle's Law
Volume is inversely proportional to pressure
V= K(-~) or PV=K
or
P V = P_V2 @ constant temp
EXAMPLE:
L2-15d
repeat EPA std.
temp, and pressure
again.
@ constant temp, the volume of gas measured at 745 mmHg
was 200 ml, what is the volume of gas at 760 mmHg?
(l) PIVI = P2v2
(2) (745)(200) = (760)(V2)
(3) V, = (745)(200)
760
196ml
B.
Charles' Law (Charles '-Gay Lussac)
Volume is directly proportional to temperature @ con-
stant pressure
V=KT
or
_
Tl T2
89
L2-16
L2-17
L2-18
L2-19
-------
CONTENT OUTLINE /£
"^i^"""""" £ ^N^H^1
Course: 435 - Lesson #2 '
Lecture Title: INTRO. TO ATMOSPHERIC SAMPLING
Page.
Of
NOTES
c.
EXAMPLE;
@ constant pressure, the volume of a gas measured at
20°C was 200 ml. What is the Volume at 25°C?
200ml
293°K
298
(200ml) x
V^= 203ml
or
298
Note ratio >1 j
i
since you are increasing
the temperature and there-
fore increasing the volume
Avogadro's Law
Volume is directly proportional to the // moles present.
that is V=kn // moles at constant P and T.
A mole by definition, = the weight of 6.02 x 1023 Gas
molecules = MW of the gas.
1 mole S0r
64g
mole = 64pg) # moles » // grams
g-MW
Avogadro s Law further implies that:
*Equal volumes of different gases under the same con-
ditions of temperature and pressure contain the same
// of moles.
The preceding laws show the following relationship
between Volume and Temperature, Pressure, and // moles
of a gas.
Boyles Law Charles Law Avogadro's Law
V
K^ Kl
K1P V
Combine equations and
K,K0K^nT where
result is ideal gas Law
= R = ideal gas constant
so V
P
nRT
or PV = nRT (ideal gas law)
The concept of molar volume,
Molar volume : The volume that one mole of
a gas will occupy at some standard
Temperature and pressure
90
L2-20
L2-21
L2-22
L2-22a
L2-23
L2-24
L2-25
L2-26
-------
CONTENT OUTLINE /X
iMMMNnHRaHHMHHHMMM^MMHHM^MIRni^HMi 5 f^S^X
Course: 435 - Lesson //2 '
Lecture Title: INTRO. TO ATMOSPHERIC SAMPLING
/^e 6_
NOTES
if standard conditions are defined as 25 C and 1 atm Slide L2-27
or 760 mmHg
note Absolute temp.
V = nRT = (1 mole)(.08205)(298.16°K) used (Note that units
P 1 atm for R are omitted
V= 24.46 liters at EPA's STP
where R = 0.03205 I.atm
mole.deg
o
Introduce ppm, and convert yg/m to ppm example problem Slide L2-28
which is the same as
EXAMPLE PROBLEM
Sample gives results as
10.6 yg S02/m3
What is this in ppm 1
2
need to change yg/m to
-3 3
1 £ = 10 m
1 mole S0? = 64 grams
1 ymole SO- = 64 y grams
10.6 yg/m3 x 10" V . 1 p mole =.1656 X 10"3 y m°le
1 liter 64 y grams 1 liter
24. 4 6 liters = 1 mole 24.46 yl = 1 y mole
.1656 xl-
work through problei
on blackboard.
LO y mole x 24.46 yl = ^ -3 ,
1JI y mole
or
.004 ppm
EXAMPLE PROBLEM - N02 Analysis
Sampling conditions: 25°C and 760 mmHg
Flow Rate: 200 ml/min.
Sampling Time: 24 Hours
NO- cone, in Abs. Soln: 3.0 yg/ml
Volume of Abs. Soln: 50 ml
Mol. wt. of NO-: 46g/g-mole
Collection Eff: 93%
What is cone, in yg/m3 and ppm
91
-------
CONTENT OUTLINE f
Course: 435 - Lesson //2 ^
Lecture Title: INTRO< T0 ATMOSPHERIC SAMPLING
UJ
O
NOTES
(cone.) (volume)
3.0 yg/ml 50 ml = 150 ug (mass)
1440 min. = 2.88 X 105 ml (volume)
(time)
200ml/min.
(rate)
mass
150 ug
1 X 106ml
520
volume 2.88 X
3 3
corrected for 93% efficiency «FI 520 yg/m /.93 = 560 yg/m
1 umole » 46 ug
560 ug _ 1 u mole
12.2 u mole
m" 46 ug mr
24.46 ul » ymole at 25°C and 760 mmHg
« 24.46
3 .
y mole
m3 = 1 X 10
298.53 u.t
,3 .
Ixl03£
298.53
,.-. .!! ! .,1,11 I
lx!03Jl
. 298
92
remind students
that their homework
will give them some
chance to practice
this
-------
THE BASIC
OBJECTIVE OF
SAMPLING
To obtAtn trvo ropro**nt*tlon
of th* poftutMtt t«v«( it f tv»n
point to Uno
FACTORS AFFECTING
TRUE VALUE
Atmowfc.rk Condition.
FACTORS AFFECTING
TRUE VALUE
P.lkrt«rt Ch» .rt.rl.lk.
CLASSIFICATION OF ERRORS
CONTINUOUS METHOD
I CONCENTRATION I
DIRECT READOUT
f MlMrtall of M«rMl
SAMPLE H
CONCERNS
o< M.loiMI. ! Int
TCMPCRATUIIE SCALCi
ATMOSPHERIC PRESSURE
GAGE PRESSURE
ABSOLUTE PRESSURE
EPA STANDARD
PRESSURE
BOYLE'S LAW
P. =R*P total
8 pressure
of system
760 mm Hg
or
1 atmos
CHARLES' LAW
93
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94
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LESSON PLAN
TOPIC:GAS MEASURING INSTRUMENTS AND
THEIR CALIBRATION, I, II
COURSE:435 Lesson #3
LESSON TIME-' 2 Hours
PREPARED BY: Northrop DATE: 1/30/79
Services Inc.
LESSON GOAL:
To identify and understand the operating principles of various
flow measuring devices and their associated calibration procedures.
LESSON OBJECTIVES:
After completion of this lecture, the student will be able to:
1) define calibration
2) distinguish between primary, intermediate, and secondary gas
flow rate and volume standards
3) distinguish among each of the following flow measurement
instruments given operational and/or physical characteristics:
a) wet test meters
b) rotameters
c) critical or limiting orifices
d) sub-critical orifices
e) moving bubble meters
4) identify the general characteristics of the following flow
measurement instruments:
a) Spirometers
b) displacement bottles
c) frictionless pistons
d) dry test meter
e) rootsmeters
f) pitot tubes
g) mass flow meters
5) Apply appropriate factors to correct volume and flow rates
for temperature and pressure
6) Distinguish between volume, i-rate, and velocity meters
95
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SUPPORT MATERIALS AND EQUIPMENT:
35 ram slide projector - required (ATC's)
Overhead projector
Blackboard is convenient for explanations
SPECIAL INSTRUCTIONS: None
SELECTED KEY REFERENCES:
(1) Student Course Manual
(2) Gases: B. Airflow Metering Instruments,
in "Instrumentation for Environmental Monitoring - Air,"
pp. 5-12, published by Lawrence Berkeley Laboratories,
Feb., 1976.
(3) Nelson, G.O., Controlled Test Atmospheres,
pp. 21-50, Ann Arbor Science Publishers, 1971.
96
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CONTENT OUTLINE /£
Course:^35 ~ Lesson #3 v -
jr//^ . CALIBRATION OF AIR MEASURING % PRO^O<
T\T7TTT^T7O "T
Page.
NOTES
OBJECTIVES - page 2 of objective handout
Objective 3 - indicates "intimate" familiarity with those
instruments.
Objective 4 - will mention only, be able to recognize them, do not
have to be familiar with details.
I. CALIBRATION
Definition: The process of establishing the relationship
between the output of a measurement process, or
portion thereof, and that of a known input.
Calibration Approaches: (using volume meter as an example)
1. calibrate meter so that when dial reads 1 liter,
1 liter has indeed passed through the meter.
2. calibrate meter so that when 1 liter has passed
through the meter, meter reading can be multiplied b
some number (correction factor) so that adjusted
reading is 1 liter.
POINT: TO DETERMINE QUANTITATIVELY WHAT HAS PASSED THROUGH METER.
II. KINDS OF CALIBRATION STANDARDS
1. Primary - can be calibrated simply by measuring
dimensions alone.
example: glass cylinder
measure diameter, height,determine volume
by V=%ird2h
very accurate (to within ±0.1 or 0.2 percent.)
2. Intermediate - cannot be calibrated by dimensional
measurements alone but accurate to within - 0.5 percent,
must be calibrated vs. primary standard.
3. Secondary - cannot be calibrated by dimensional measure-
ments alone - must compare with primary standard. Accu-
rate to within a few percent
III. AIR MEASURING DEVICES
A. INTRODUCTION
refer student to
(objectives sheet
read objectives to
students
point out differ-
jence between Object-
jive 2 & Objective 3
L3-1
total volume meters
97
L3-2
L3-3
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CONTENT OUTLINE
Course: 435 - Lesson //3
Lecture Title ' Calibration of Air Measuring
\
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Page.
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17
NOTES
rate meters
velocity meters
1. total volume meters - measure volume
rate meters - measure flow rate
(volume per unit time: example 1/min.)
2. "rate" meter: volume meter with a timer
Classes of rate meters:
variable pressure meter: change in pressure
across constant area.
variable area meter: change in area at constant
pressure.
3. velocity meters - measure speed
(velocity: length per unit time: example:
meters/sec.)
B. VOLUME METERS - Will go over each one individually
spirometer
moving bubble meter
frictionless piston
displacement bottle
L3-4
L3-5
L3-6
L3-7
(read to students)
primary standards
intermediate standard
secondary standards
wet test meter J
dry gas meter \
rootsraeter I
1. Primary Standards
a. Spirometer known as "spirometer"
"gasometer"
"bell prover"
"drum within a drum"
(1) vertical deflection on scalar x cross-sectional area
of drum = volume
L3-8
describe spirometer
operation
L3-9
98
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CONTENT OUTLINE /£
Course ^35 ~ Lesson #3
OF AIR
Page.
NOTES
(2) Care:
Drum must be absolutely uniform in cross-
sectional area.
counter - weight system must balance out
drum so that there are no changes in gas
density inside the drum caused by weight of
bell and thus affecting pressure.
(3) Strictly a laboratory instrument, very expensive
range - 9 to 700&
2
calibration - Vird h
accuracy - (approximate) ±0.2%
advantages - very accurate
disadvantages - expensive, lab standard only,
alignment critical
uses - calibration only
(4) Calibration set-up
Typical set-up for calibration of a wet-test
meter (WTM) by a spirometer
Necessary to measure P, T in both WTM and
spirometer
WHY? Because you will want to
correct WTM readings to STP.
b. Frictionless Piston - Primary Standard
1. Constant cross-sectional area cylinder with PVC
"piston" floating in cylinder - sealed to cylinder
sides with mercury (mercury seal)
Manufacturer "air gauges" the inside of the cylinder
at 1 inch increments to test consistency of i.d. Each
system is checked against a standard frictionless
Piston before shipment.
2. Rate determined by spacing along cylinder of 2
proximity coils - when mercury seal passes lower coil
a timer is activated. When seal passes upper coil,
timer is deactivated. Upper coil is movable to
change displaced volume.
99-
L3-10
(read to students)
L3-11
L3-12
L3-13
describe operation
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CONTENT OUTLINE
Course: 435 - Lesson #3
Lecture Title: Calibration of Air Measuring
\
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Pngt> 6 r>f 17
NOTES
c.
3.
Rate of Flow = distance between coils x cross-sectional arei
tine
Laboratory Instrument
Range - 0.1 - 24 liters/minute
2
Calibration - ird h /4
Accuracy ±0.2%
Advantages - convenient, very accurate, easy to
calibrate; very little pressure drop
Disadvantages - expensive, lab only, use of mercury as
a seal, mercury toxicity
Uses - calibration only
Moving Bubble Meter - primary standard
Can be made by competent glass blower
Simple, can be constructed in your laboratory easily
Can purchase NBS traceable ones (expensive)
Can purchase cheaper ones
1. (kind of "frictionless" piston with a soap bubble as
piston)
a. Time movement of bubble between two volume marks
V = Flow = Q
t
b. Can use cut-off graduated cylinder or inverted
Burette, etc.
c. calibration usually accomplished by filling cylinder
with water, extracting known amount, and then either
use weight of water extracted x density (at lab. T) or
measuring volume of extracted water
2
d. could use V = ird h but would be inaccurate since i.d.
4
of glass is not very consistent
2. range - Useful 1ml to 1000ml/minute
calibration - by filling with a known volume of liquifi
accuracy - +0.25%
100
L3-14
L3-15
L3-16
(read to
students)
-------
CONTENT OUTLINE fg
Course. 435 - Lesson #3 \
Lecture Title: Calib. of Air Measuring Devices
advantages - low cost, easy to construct and use
disadvantages - easily broken, must have constantly wet walls,
water vapor pressure correction, only good for flowrate £U/min|"leak" of gas thru
Uses - calibration only.
3. CAUTION: Suppose you are measuring dry air with soap bubble.
Film-water used in bubble formation will evaporate into the dry
air and thus increase the volume.
Easily corrected, but subtle error that many people do not correct.
a. Correction: Use
Page.
NOTES
(explain permeation
of gas thru bubble:
bubble at < 1 ml/min
and > l£/min)
V std ,
corrected
V x correction factor
meas
correction factor = P -
» partial pressure due to water vapor
To correct to standard conditions:
T std Pb
V std = V corrected x
T meas
V std
V std
meas x
P P
b - IJ70
P std
x T std
T meas
L3- 17 a
L3-17b
P std
V meas x T std x ( b -
T meas
b. Example Problem:
P st-H
A soap bubble traversed a volume of 400ml in 0.75 minutes. If
the ambient temperature was 20°C, barometric pressure was
762.3mmHg, what was the flow rate at standard conditions?
V ,= V x Tstd x P, -P,
std meas
meas
std
H20 (at 20°C) =17.5
from "Handbook of Chemistry and Physics"
V = 400 x 298 x 762.3 - 17. 5
293
^J 760
V ... = 399ml
std,
Qstd = Vstd = 399ml - 532 ml/min
0.75 min
101-
L3-18
L3-19
L3-20
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CONTENT OUTLINE
Course: 435 - Lesson #3
Lecture Title: Calib. of Air Measuring Devices FL
ul
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Page.
of.
17
NOTES
c. Displacement Bottle - Primary Standard
1. Consists of a bottle filled with water (or some other
liquid) and a tube through which air can enter the bottle
and a tube through which the liquid is drained out. The
entering air displaces the liquid and subsequently enablejs
the measurement of the volume of liquid by having it
empty into a primary standard (volumetric flask). The
volume of air is thus equal to the volume of liquid that
emptied into the volumetric flask.
2. range - depends on volumetric flask (Class A) - usually
1-2 liters
calibration - physical determination of volume of liquid
in flask
accuracy - depends on volumetric flask CLASS A - 2000 ml:
,0.5ml in 2000"»0.1%
advantages - easy to assemble and use, inexpensive,
highly accurate
disadvantages - water must equilibrate to room conditions
before use (24 hrs.), lab only
use..;-- jcalibratlO-n -
d. Recap 4 Primary Standards discussed
SPIROMETER
FRICTIONLESS PISTON
MOVING BUBBLE METER
DISPLACEMENT BOTTLE
L3- 21a
L3-21b
L3-22
L3-23
102
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CONTENT OUTLINE
Course: 435 - Lesson #3
X>J
Lecture Title: calib. of Air Measuring Devices I
m
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NOTES
2.
Intermediate Standard
a. Wet Test Meter - intermediate standard
describe operation of WTM
level of water critical
1.SPECIAL FEATURES
sight glass - stainless steel spirometer
water manometer -gauge pressure in air space
above liquid
L3-24a
L3-24b
Thermometer - temperature of liquid
ture of gas
tempera-
2.
range - 1 £ .to 10£ /revolution
calibration - water displacement, spirometer
accuracy - +0.5%
advantages - widely used, convenient, easy to cali-
brate
disadvantages - lab only, water static temp
condition, equilibrium time
use - calibration
L3-25
Do not use WTM for flows > 3 revolutions /min; starts acting as flow limiting device.
3. CAUTION: Since 02 & N2 in air is soluble in water, it is
necessary to condition water in WTM before using it in the cali-
bration process (operate WTM for ~ 1 hour by pulling air through
it prior to use at laboratory conditions to saturate water with
<">2 & N2^' If ^ou C'ian8e from one 8as to another, you must re-
equilibrate.
Temperature of water in WTM should be at room temperature, fill ~
24 hours prior to use.
4. For calibration of wet test meter use displacement bottle
(a primary standard)
a. (DESCRIBE CALIBATION: Procedure to be
used in Lab)
103
L3-26
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CONTENT OUTLINE /£
""""I g VsPKr
Course: 435 - Lesson #3 ^
Lecture Title: Calib. of Air Measuring Devices
m
o
0/" LZ.
NOTES
1. Use class AVolumetric Flask to Collect Water
2. From laboratory data calculate percent error
if much more than + 2% error, WTM needs to be adjusted.
3. Note P., T on lab data sheet
Must correct for Ap across meter
Ap measured by U.tube manometer
V = V x Tstd x Pb ~ Ap
std meas
meas
std
L3-27a
L3-27b
If Ap measured in inches H~0, convert to P, units before subtraction
If P, is measured in mmHg, Ap converted by
Ap , mmHg
Ap, in H20 x 25.4 mmHg
13.59 in H20
in Hg
L3-28
4.
in Hg
EXAMPLE PROBLEM:
2.600& of air at 27°C, 750 mmHg were passed through a
WTM, Ap = 0.35 in H20. What is the volume of air
passed through the meter at STP?
V .-V xTstd VAP
std meas x =
meas
'std
Ap = 0.35 in H20 x 25.4mmHg = 0.65mmHg
in Hg
13.59 in H20
in Hg
V ^ , = 2.600A x 298°Kx (750 - 0.65) mmHg
std -* *^
3000K 760mmHg
= 2.600Ji x 0.99 x 0.99
V = 2.550^
std
L3-29
L3-30a
L3-30b
L3-30c
104
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CONTENT OUTLINE /X
^^^i^^""^ § ISP^
Course 435 - Lesson #3 V
-------
CONTENT OUTLINE /£
Course: 435 - Lesson #3
\
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Lecture Title: calib. of Air Measuring Devices if
nf 17
NOTES
Recap what happened in Cal. I.
C. Rate Meters
1. Introduction
a. Measure Flow (volume/time)
Variable Pressure - Secondary Standards
conventional orifice
critical/limiting orifice
Variable Area - Secondary Standards
Rotameters
2. Variable Pressure Meters
a. Orifice Meters - Secondary Standards
Explain what an orifice meter is - constriction
in a pipe
If increase Ap across orifice (constriction) flow
increases with Ap up to a maximum flow called the
critical flow (sonic flow). At this point speed
of gas = speed of sound.
Same orifice can be critical and non-critical depend-
ing on A p.
Must protect orifices from material that will clog
them.
(1) Conventional Orifice - used as flow controlling
and measuring devices - can vary Ap to get
different flows (up to a certain point).
L3-37a
L3-37b
L3-38
L3-39
106
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CONTENT OUTLINE
Course: 435 - Lesson //3
Lecture Title: Calib. of Air Measuring Devices ift*
Png* 13 nf 17
NOTES
(2) Critical or Limiting Orifice
General "Rule of Thumb" - Flow through
any orifice is critical when P upstream
= 2 x P downstream and when cross-sectiona
areas of tube is 25 times the area of the
constriction.
Critical pressure determined by:
Orifice construction
wall roughness
relative size of the orifice
cross-sectional area vs. approach cross-
sectional area
etc.
to obtain critical flow:
(1) pressurize upstream, or
(2) de-pressurize downstream side (evacuate
'Lab set-up (similar)
hypodermic needles can be used as limiting
orifices
gage inversely proportional to flow
length of hypodermic has minor effect on
flow ...
Direction of flow through a hypodermic
needle acting as a limiting orifice has
an obvious effect on its flow rate.
Kotrappa, et. al. , "Evaluation of Critical Orifices made
from sections of Hypodermic Needle" Ann Occup. Hyg.,
Vol. 20, pp 189-194, 1977.
L3-40
Note: differences
between critical
limiting orifices
include diameter,
taper, and others
L3-41
(will use this
approach in lab)
L3-42
4A.3.18 (describe
and locate compo-
nents)
L3-43
L3-44
107
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CONTENT OUTLINE
Course: 435 - Lesson #3
Lecture Title: Calib. of Air Measuring Devices ffr
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O
Page
of _ LL
NOTES
(3) range : typical ranges 0.1 £/min-10 £/min
calibration: primary standard (bubble meter, wet
test meter)
accuracy: + 3% (hypodermic needles)
advantages; inexpensive, simple, maintains constant
flow
disadvantages: only one critical flow rate possible
high pressure drop, large capacity
pump required
L3-45
use; sampling
QUESTIONS?
Ask for questions
about orifices
3. Variable Area Meter - secondary standard
Rotameter - common instrument
a. simple construction - theoretical operation complex -
basically air below float becomes dense enough
to lift float
float, tapered glass tube
3 forces acting
downward: gravity
upward: buoyancy, viscous drag
(1) Buoyancy
Buoyancy of stainless steelaerodynamic shape
(minor force in the case of a stainless steel ball)
(2) Viscous drag (affinity gas has for sides of float-
will attempt to drag sides with it as it passes
also will cause a small pressure drop on down-
stream side of ball)
o when three forces balance, ball will float in gas
o variable area because tube is tapered: as float
rises area between float and tube increases and
gas velocity decreases and viscous drag de-
creases; as float falls area between float and
tube walls decreases.
o area varies, pressure remains constant.
o typical calibration curve.
TUBE
READING
L3-46a
L3-46b
L3-47
L3-48
UNITS FLOW RATE
108
L3-49
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CONTENT OUTLINE ,
_.__._«___-«-_. i
Course: 435- Lesson #3 \
Lecture Title: qalib, of Air Measuring Devices
m
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Page
of-JL
NOTES
b. range .005 £/min - 45 £/min
calibration - primary standard, wet test meter, moving
bubble meter, mass flow meter
accuracy ±5 to ±10%
advantages - light, portable, direct flow readings,
ease of operation, useful in field.
disadvantages- correction for temperature and pressure
or calibrate under conditions to be use
use - Sampling
c. Corrections for T and P: Rotameter
Corrections for T and P: Rotameter
Correction process differs for rate meters from that of
process for volume meters
L3-50
for atmospheric
sampling applica-
tions
Volume meters^
P T
V "V x meas x std
corr meas =
std meas
Corrected Volume
flow correction differs from volume correction :
Describe to
the students how to
read a float in
a rotameter i.e
read center of
float.
L3-51
Note for students
square root used fo
flow corrections
(corrected)
Comes from Bernoulli's Theorem
better to avoid calculated corrections; calibrate at the
conditions under which you intend to use the rotameter!
in the laboratory, you will calibrate a rotameter using this
set-up
rotameter is downstream of bubblers, at reduced pressure
you will calibrate at two different upstream pressures, and
plot the calibration curves
you will essentially be investigating the effect of pressure
(T will be constant, more or less) on the flow
IMPORTANT: the rotameter should be calibrated in the con-
figuration (sampling train) in which it is used.
109
L3-52
L3-53
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CONTENT OUTLINE
Course: 435 - Lesson #3 ^
Lecture Title: Calib. of Air Measuring Devices ifr
Sfc
li of LL
NOTES
4. Velocity Meters
Not commonly used in ambient sampling, and then primarily
as calibration devices
pitot tube often used in source testing - primary
standard
a. Mass Flowmeter - secondary standard
1. Measure mass flow by transfer of heat
Components - Transducer and electronics package
Since heat transfer is sensed, mass flow is registered, not
volume flow. But volume is output electronically.
Heat transfer not affected by changes in P, T. BUT
affected by changes in gas (mass flow of helium registers
differently than mass flow of air because of different
thermal properties of helium and air).
Calibrate for the gas to be used.
b. Operation: Gas flows across heated element in transducer,
thereby cooling it. Mass flow is determined by amount of
energy required to re-heat the element to its original
temperature thru a kind of Wheatstone Bridge arrangement.
Somewhat expensive
c. range 0-50,000 SCCM (Std. cubic centimeters per minute)
calibration wet test meter, spirometer, frictionless pistor
accuracy - + 5%
response time - (5 sec. full scale)
advantages - No correction necessary over wide range of
T & P.
disadvantages - Requires electrical power, limited to non-
explosive gases, particulate buildup will
alter response, minimum threshold flow~0.5%
full scale reading
SUMMARY
IMPORTANT - air measuring instruments (for this course)
WTM
rotameter
orifices
110
L3-54
L3-55
L3-56
L3-57
L3-58
-------
CONTENT OUTLINE
Course: 435 - Lesson #3
Lecture Title: Calib. of Air Measuring Devices
Page
17
u
o
NOTES
Meters
conventional
critical
volume meters
rate meters
velocity meters
L3-59
Standards
primary
intermediate
secondary
uses
CLASS QUESTIONS
What is an example of a volume meter? rate meter? velocity
meter?
What is an example of a primary standard? Intermediate
standard? Secondary standard?
Any other questions?
Ill
-------
CAUBRATION
APPKOACHIS tot MIBRMIOS CALIBRATION STANDARDS AIR MEASURING DEVICES AIR MEASURING DEVICES
AIR MEASURING DEVICES
VOLUME METERS
MCIISUUV *>Mtmr<«
SPKOMETER
CALIBRATION",!! IP
BBCTIONLESS PISTON
MOVING BUBBLE METER COMKHONW.WATH.VAPO. rowSSES&iniow
I 400 ml in --5 mNHilrv I
-------
or, mil,O JS/4mmHg
) «vH(t
2.600-0.99-0.99
V LVM Ulcn
DRYTHtMETH
ROOTSMfTFROPtRATIOS
ROOTSMFTER
RATE METERS
Q-f
KIIK VI IIKiln I
I hvl HIM I H'tll 41 flRIIH
«l«W«IK>l«(l«M III IKiniV.l
UMmNGORJRCE
ROTA,VU1(R
«
KOTAMfTFR OUJMUTION CUIVE
CORRfCTIONS FOR
T AND P: ROTAMFTBt
113
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114
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LESSON PLAN
TOPIC: HIGH VOLUME METHOD
COURSE: 435 - Lesson #4
LESSON TIME: 1 Hour
PREPARED BY: Northrop DATE: 1/31/79
Services, Inc.
Lesson Goal: To develop an understanding of the procedures involved in
performing, calibrating and auditing the high volume method
for particulate sampling.
Lesson Objectives:
The student will be able to:
1. Briefly describe the components of a standard high
volume sampler.
2. List the procedure for properly obtaining a high
volume sample of suspended particulate.
3. Outline the procedure for calibrating a high volume
calibration orifice using a rootsmeter.
4. Recall and use the method for recalculating the orifice cali-
bration curve when different temperature and pressures are
involved.
5. Describe and use the procedure for calibrating a high volume unit
containing a visifloat or transducer.
6. Discuss briefly the audit procedure for the high volume
sampler.
7. Calculate the total suspended particulate concentration for a
high volume sample, given filter weights, flow rate, sampling
time.
8. Identify the common interferents (errors) associated with total
suspended particulate measurement using the reference high volume
method.
115
-------
Support Material and Equipment:
1. Objective Handout This is in Blue
Folder
2. Carousel Projector with Slides
3. Handout of Federal Register, Vol. 36, No. 84, Part II, This is in
Friday, April 30, 1971, Appendix B "Reference course manual
Method for the Determination of Suspended Particulates
in the Atmosphere (High Volume Method)
Special Instruction: This is the method students will perform in
Laboratory 1.
Selected Reference:
Federal Register, Vol. 36, No. 84, Part II, Friday,
April 30, 1971. Appendix B. "Reference Method for the
Determination of Suspended Particulates in the Atmosphere
(High Volume Method)".
116
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CONTENT OUTLINE
Course: 435 - Lesson #4
Lecture Title: Hlgh volume Method
UJ
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Page
NOTES
TITLE: HIGH VOLUME METHOD
The PURPOSE of this lecture Is to develop an understanding of the
procedures involved in performing, calibrating and auditing the
high volume method for particulate sampling.
GO OVER OBJECTIVES OF LECTURE
INTRODUCTION - High Volume Air Sampling
Historically,suspended particulates (coal dust, fly ash, smoke,
etc.) have been associated with air pollution, as a readily
identifiable form along with photochemical haze. Sampling for
particulates in the air is a basis of modern ambient air monitor-
ing. The Federal Reference Method is contained in 40CFR50
(Appendix B) which is in the Course Manual.
The High Volume Air Sampler is probably the most used method of
ambient monitoring - over 20,000 are in use.
Particulates are one of the seven criteria pollutants for national
primary and secondary ambient air quality standards
High Volume Sampling data is used fora variety of purposes including
Evaluating compliance with air quality standards
Determination of air quality trends
Public Health studies
Development and Evaluation of control measures
and others (Ask students for others)
THE HIGH VOLUME SAMPLER
Development - Developed by Silverman (1948). Used a vacuum
cleaner motor with a 4 in. filter and filter holder. Refined
later (1950's) to take larger filter. 1957 General Metal Works
redesigned the sampler to USPHS specifications to look as it does
today. .
Sampler - Modified electric motor. Stainless steel or aluminum
filter holder. Filter '8x10 in., (20.3x25.4cm) exposed :
surface 7x9 in. (63 in2 or 406.5cm2). Operated at
40-60 cfm (1.1-1.7m3/min) collects particles up to
100 microns (Stokes equiv. diameter) (usually 0.1-30
microns)
Shelter - Shelter provides protection, allows unrestricted
access of ambient air without direct impingement of particles
(fallout or dustfall). Shelter also eliminates particles
larger than 120ym by inertia. Peaked roof acts as a plenum, above
the filters distributing the particles evenly across the face
of filter. Shelter is integral part of sampler, usually built
of wood, aluminum, stainless steel.
117
L4-1
L4-2
L4-3a
L4-3b
L4-3c
L4-3d
L4-4
L4-5
L4-6
L4-7
L4-8
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CONTENT OUTLINE f$
Course: 435 - Lesson #4
Lecture Title: Hi8h Volume Method
\
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NOTES
Constant Flow Samplers - Constant flow hi-vol samplers are
designed to eliminate the problem of flow decreasing with filter
loading; several types are used.
MSA Fixt - Flo Sampler - uses automatic compensating damper -
as resistance increases the bypass damper is closed causing
increased suction.
Pressure Sensitive Regulators - uses pressure sensitive switch
at exhaust port - when resistance increases, exhaust pressure
decreases causing switch to increase the voltage to the motor
which increases suction.
Series Flow Regulator - a spring loaded piston inserted in the
throat of the filter holder. The piston has an annular opening
which is increased in size as the spring relaxes due to lowering
resistance.
Mass Flow Tranducers - Most widely used method. A mass flow
meter probe is inserted into the throat of the Hi-Vol sampling
head. This probe senses the mass flow of air past it.
Electronic circuitry adjust power (current) going to hi-vol motor
to keep mass flow constant. As discussed in earlier lecture
mass flow meters are insensitive to temperature and pressure
fluctuations. If the mass flow is calibrated at standard
temperature and pressure, then airflow through hi-vol is
measured at STP.
Maintenance
1. Replace brushes periodically, approx. 30-60 runs
Based on records of performance
2. "Buck or Boost" transformer to increase brush life, reduces
voltage " 25% (this reduces flow rate-must maintain at least
40 cfm not greater than 60 cfm)
3. Clean or replace flowmeter and flowmeter tubing.
4. Clean and replace face plate gasket, a major area of flow
leakage (point out signs of wear)
5. Clean inside shelter cover.
Filter Media
Influenced by objectives of the sampling program. Glass fiber
filters are the most commonly used. Not perfect but generally
meet requirements. Must be careful of filter pH and uniformity
...also reactions with and/or on filter. Difficult to remove
particles for microscopic study. Artifact formation (SO and
N0_). Usually not possible to use for silica, calcium, sodium,
potassium due to high blank levels. Should take random blank
level readings to subtract out such constituents. Other media
include cellulose and plastics (e.g. teflon). Mention that EPA
will supply free of charge glass fiber filters from their filter
bank to all federally mandated monitoring efforts. Mention also
used in lead analyses as well. 118
Cover these
briefly, as
most use the mass
flow (thermal)
controllers now
L4-9
L4-10
L4-11
L4-12
L4-13
-------
CONTENT OUTLINE
Course: 435 - Lesson #4
Lecture Title: High Volume Method
\
\
Page 3 0/_8_
NOTES
HIGH VOLUME SAMPLING PROCEDURE
Choose Filter Media
Inspect filter for tears, holes, etc. - this can be done on a
photo light table.
Affix ID number - make sure not to damage filter, usually
stamped on.
Equilibrate filter - must be done in a clean room or constant
temp, and humidity chamber - equilibrate at 70-75° F for at
least 16 hrs. before weighing at less than 50% relative
humidity. Atmosphere should be free of acidic or basic gases,
especially HF.
Weigh Filter - to nearest milligram using a calibrated balance.
Balance should be calibrated with NBS weight before and after
weighing batch of filters. Careful not to bend or fold filter.
standard lab balances have special filter weighing tray attachmenjts.
Record Filter Weight - should keep balance log beside balance to
document weights, calibration, etc. After weighing, filter
should be inserted in protective glassine envelope and put in
folder - unfolded - can load in cartridge.
Install filter on High Volume Sampler - make sure filter is
centered and that faceplate gasket is in good condition. Use
equal pressure in applying faceplate - can be done indoors if sambler is
in a windy environment.
Record pertinent data - can be filled in on filter folder.
Should contain: (a) Filter No. (b) Station No. (c) Sampler No.
(d) Starting Time (e) Initial Flow Rate (f) Date and Operators'
Initials (g) Summary of Conditions (Meteorology, Construction
Activities, etc.) - give example.
Sample for 24 hrs. - typical sample is 12 midnight to 12 mid-
night. Can be shorter for heavier loading.
Record final flow rate after 5 min. of warm-up, (this flow
rate should be the actual flow rate-as read off calibration curve)
Record stop time and elapsed time and summary of conditions.
Remove Filter. Note if edge is sharp between soiled and clean
part of filter. If not, may need to replace gasket. If other
than minimal, note on data sheet and possibly discard filter.
Inspect for holes, tears, foreign matter (such as insects), etc.
Fold Filter (lengthwise) soiled surface to soiled surface and
place in envelope and then in folder.
Re-equilibrate to Weighing Room Atmospheric Conditions- 24 hrs.
119
L4-14a
L4-14b
L4-14c
L4-14d
L4-14e
L4-14f
L4-14g
L4-15
L4-14h
L4-141
L4-14j
L4-14k
L4-141
L4-16
L4-14m
L4-14n
-------
CONTENT OUTLINE
Course: 435 - Lesson #4
Lecture Title: High Volume Method
UJ
C3
NOTES
Reweigh filter; record final weight and net weight plus other
pertinent information.
Mention elapsed time meters for timing sample runs, transducers
for flowrate, to determine if a shut down occurred during run.
SUMMARIZE HI-VOL METHOD
1. Filter
2. Vacuum Cleaner Motor
3. Weighing
Calculation of Total Suspended Particulates
TSP (wg/ni )
mass - mass
X 10
X 1440 min./24 hr. x t
(Can use other averaging method)
massf = Final mass of Hi-Vol Filter (grams)
mass. = Initial mass of Hi-Vol Filter (grams)
Qf = Final Flowrate - Corrected to True Flowrate (m /min)
Q. = Initial Flowrate - Corrected to true flowrate
(m3/min)
10 = Conversion of grams to micrograms
t = Sampling time in hours
o
Results in pg/m
CALIBRATION OF THE HIGH VOLUME CALIBRATION ORIFICE
Will perform this in Laboratory A
Description of Calibration Unit - 7.6 cm I.D. 15.9 cm long.
Pressure Tap 5.1 cm from one end. End plate has hole 2.9 cm
in diameter - for orifice calibration .
Five resistance plates to simulate different particulate load-
ings. 5,7,10,13, & 18 holes; 18-hole plate represents clean
filter.
Rootsmeter - serves as a "primary" standard dry gas meter, even
though an secondary standard. Measures volume of air passed
through calibration orifice.
Calibration Procedure
(1) Hi-vol motor is attached to exhaust outlet of the
rootsmeter
120
L4-14o
L4-17
L4-18
L4-19
L4-20
L4-21a
L4-21b
L4-22
-------
CONTENT OUTLINE
Course: 435 _ Lesson #4
Lecture Title: High Volume Method
Page.
of.
111
o
NOTES
(2) Mercury manometer is placed on rootsmeter pressure tap
(3) Orifice unit is attached (resistance plate in place) to
inlet of rootsmeter
(4); Water manometer is attached, to orifice pressure tap
(5) Given volume of air is pulled through unit - rootsmeter,
by Hi-Vol motor.
(6) Time elapsed (min), mercury pressure drop (mmHg), water
pressure drop (in KLO), volume of air passed are
recorded.
(7) Repeated for each resistance plate
(8) Barometric pressure and room temp, are recorded
Calculation of Calibration Curve
Pressure reduced in Rootsmeter, so true Volume must be obtained.
First correct air volume sampled to true air volume using:
L4-23
L4-24
V, = (Pb ~ V (V )
b - m
V, = True Air Volume at Atmospheric Conditions, (m )
P, = Barometric Pressure, (mm Hg)
P = Pressure drop across inlet 'of primary standard, (mm Hg)
o
V = Volume of air measured by primary standard, (m )
Then determine the air flowrate by:
Q = True Air flowrate (m /min.)
V, = True Air Volume, (m )
L4-25
T = Time of Flow, (min.)
This is calculated for each resistance plate and graphed on
log-log graph paper (2x3 cycle)
L4-26
This is the Orifice Calibration Curve for this particular
orifice. Should not use curves supplied with orifices - you
should produce your own and check theirs with yours.
121
-------
CONTENT OUTLINE
Lesson #4
Lecture Title: High Volume Method
\
\
111
o
nf
NOTES
-Recalculation of Orifice Calibration Curve - (Due to change in
atmospheric conditions) - If calibration orifice is used to
calibrate a hi-vol station where atmospheric conditions are
significantly different. Rule of thumb - 15% change in pressure
with a 100% change in temperature yields 15% error. The cali-
bration curve needs to be adjusted. Formula for recalculation:
= .Q
cal
T P -
new cal
T ,P }
cal new/
Q = New Flowrate at New Atmospheric Conditions
Q , = Flowrate calculated previously
T P
new new = New Temperature and Pressure
T P
cal cal = Previous Temp, and Pressure
SHOW THE STUDENTS A SAMPLE PROBLEM AND WORK THROUGH IT FOR THEM
Sample Problem - Correction of Hi-Vol Orifice Calibration Curve
The Hi-Vol orifice was calibrated at 24°C and 762 mmHg. From the
curve of flow rate vs Ap?: the flow rate is 1.28 m /min when
= 6.0 in H00. What is the new flow rate Q
new
new
= 10°C and P
new
= 770 mmHg?
SOLUTION:
new = cal
T P .
new cal
T , P
cal new
new
Q =1.28 m /min @ Apj^ = 6.0 in.
T = 10°C + 273 = 283°K
new
P = 770 mmHg
new 6
T . = 24°C + 273 = 297°K
cal
P . = 762 mmHg
cal
i OQ 37 . /28-3 x 7-62
= 1 . 28 m /min ( -^= - ^7- J
\297 x 770 /
/2
=1.28 m/min (.971)
=1.24 m3/min
Q =1.24 m3/min @ AP-, = 6.0 in H00
xnew J- i
This represents only 1 point on new calibration scale.
122
L4-27
L4-28
L4-29
L4-30 a
L4-30b
L4-31
-------
CONTENT OUTLINE
Course: 435 - Lesson #4 (,
Lecture Title: High Volume Method
Page2
NOTES
CALIBRATION OF HIGH VOLUME UNIT (with vlslfloat or transducer flow-
rate devices)
Procedure for Calibration
1. The filter holder assembly is removed and replaced with
the calibration orifice unit.
2. A water manometer is placed on the orifice pressure tap.
3. The hi-vol motor is run with each resistance plate in place.
4. For each run a pressure drop (in. H?0) reading is recorded,
and a visifloat or transducer reading is recorded.
5. The relative transducer/visifloat flow reading is graphed
against the actual flowrate derived from the orifice cali-
bration curve, to give a calibration curve for this
particular hi-vol unit.
HIGH VOLUME SAMPLING ACCURACY AND PRECISION
Affected by several factors:
Sampler Operating Characteristics - sampler drop in flowrate
due to filter loading introduces some error, line voltage
fluctuations cause errors, flowrate chosen (i.e., 20 cfm, 60 cfm
etc.) can affect result
Peaked roof causes wind direction dependence
Accuracy of Calibration
Filter Characteristics - reactivity and size range of particulati
Location of the Sampler - both site and height
Nature and Concentration of Particles Sampled - artifact formed from
S02 and N02-
Particulate matter accumulated non-uniformly over sampling
period and adsorption and absorption of water vapor.
Can correct many flow problems with constant flow Hi-Vol.
Idle periods show gain in mass.
Slides for visifloat
calibration
L4-32
L4-33
L4-34
L4-35
lides for transduce
calibration
L4-36
L4-37
L4-38
L4-39
123
-------
CONTENT OUTLINE f§
Course. 435 - Lesson //A
Lecture Title: High Volume Method
i
UJ
e>
Page
of _ !L
NOTES
HIGH VOLUME REFERENCE AUDIT PROGRAM
Developed by EPA and NBS to field check calibration orifices. Uses
a plastic box with a series of holes which act as a subcritical
limiting orifice. Each ReF has a K value which is used to deter-
mine the accuracy of the Q values for the calibration orifice unit.
ReF consist of:
(a) Plastic box which attaches directly to hi-vol filter
holder.
(b) Set of resistance plates which fit inside box in a recessed
area above filter holder inlet.
(c) Windscreen - to prevent pressure fluctuations at inlet
(d) Pressure tap and water manometer
SUMMARIZE WITH A REVIEW OF OBJECTIVES
Show reference
device I
L4-41
Refer to lab 1
experiment 2 for
procedures
L4-42
QUESTIONS?
END OF LECTURE
124
-------
HIGH
VOLUME
SAMPLING
PURPOSES OF Hl-VOL
SAMPLING DATA
Evaluating compliance
PURPOSES OF Hl-VOL
SAMPLING DATA
Determining air quality trend*
PURPOS
SAM
I vatuating compliance
Determining air quality trrnd*
Public hv.tth
ntrol mea*ure«
Hl-VOL SAMPLING
PROCEDURE
HI-VOl. SAMPLING
PROCEDURE
Hl-VOL SAMPLING
PROCEDURE
Hl-VOL SAMPLING
PROCEDURE
HI-VOL SAMPLING
PROCEDURE
I (hum mxlu UMgti Illtrr
HI-VOL SAMPLING
PROCEDURE
HI-VOL SAMPLING
PROCEDURE
Hl-VOL SAMPLING
PROCEDURE (Cent.)
HI VOL SAMPLING
PROCEDURE (Cool.)
Sample
HI-VOL SAMPLING
PROCEDURE (Com.)
Hl-VOL
PROC
HI-VOL ____
PROCEDURE
final flow rate and
wd time
ov« fitter
125
-------
HI-VOLSAMPUNG
PROCEDURE (Coot.)
S.rapte
Not* final flow rat* and
HI-VOLSAMPUNG
PROCEDURE (Cant.)
Simple
Notr final flow rat* and
rlapa«d time
Remove nHcr
Inspect filter
- KtM place in em«-I«i(>*'
HI-VOLSAMPUNG
PROCEDURE (Cart.)
Haaxl Final Wmht and (Mm Data
TOTAL SUSPENDED
PAHTICULATE
CALCULATIONS FOR
TSP USING HI-VOL
**"**** ~ "*"
TRUE AIR FLOW RA
Vb tmeal.volu.il.1)
SAMHLJL PHOBIEM;
tintmlh.ii nl HI-Vol
Ortdc. Calibrate* C
SOLUTION (CoattaiMd):
t_ - IOT -m-m-ic
p_ - ntmmH,
T,., -WC -m- W7-K
P.J KlMHa
Qm I 2« »?«!«£,-<» HtO
rrprnm» only 1 potat on
HI VOt ACCURAt.-V AND Pttl' IMOS
f 1A lit M 20«0
126
-------
127
-------
LESSON PLAN
TOPIC: GENERATION OF TEST
ATMOSPHERES
COURSE: 435 - Lesson #5
LESSON TIME: 1 hr. 15 rain.
PREPARED BY: Northrop DATE:2/13/79
Services, Inc.
LESSON GOAL:
To understand the basic methods for generating and analyzing the
controlled atmospheres of gaseous pollutants that are used to
calibrate or examine certain parameters of gaseous sampling and
analysis methods.
LECTURE OBJECTIVES:
The student will be able to:
(1) identify the stability problems associated with low
level cylinder gases specifically, S0? N0? and
CO.
(2) Given the appropriate data, perform calculations
necessary to determine the concentrations of gases
produced by permeation systems and dilution systems.
(3) Outline at least two methods for actually metering
diluent gas into a static or dynamic systems.
(4) Recognize and identify the adsorbents and apparatus
necessary to produce zero air.
(5) Define NBS traceability in terms of Standard Reference
Materials and non-NBS standards.
(6) Describe the construction and use of permeation systems.
SUPPORT MATERIALS AND EQUIPMENT:
Carousel projector and slides
Overhead projector or blackboard not required but convenient
to have available.
128
-------
SELECTED REFERENCES
1. Student Course Manual
2. "Gases: C. Static Calibration Techniques and D.
Dynamic Calibration Method," in Instrumentation
for Environmental Monitoring- Air, pp. 13-28,
Published by Lawrence Berkeley Laboratories,
Feb., 1976.
3. Nelson, G. 0., Controlled Test Atmospheres, '
Chapter 4 - "Static Systems for Producing Gas
Mixtures," pp. 59-94, and Chapter 5, "Dynamic
Systems for Producing Gas Mixtures," pp. 95-160,
Ann Arbor Science Publishers, 1971.
4. Bennett, Berne I., "Stability Evaluation of Ambient
Concentrations of Sulfur Dioxide, Nitric Oxide, and
Nitrogen Dioxide Contained in Compressed Gas
Cylinders", EPA 600/4-79-006 (Feb..-1979) Quality .
Assurance Branch, Environmental Monitoring Systems
Laboratory, Research Triangle Park, NC.
5. Kebbekus, E., and Scornavacca, F., "Factors in the
Selection of Calibration Gas Standards", Am. Lab.,
July 1977.
6. "Traceability Protocol for Establishing True
Concentration of Gases Used for Calibration and
Audits of Continuous Source Emission Monitors"
(Protocol No. 1), Environmental Monitoring Systems
Laboratory, Office of Research and Development,
U.S. Environmental Protection Agency, Research
Triangle Park, NC.
7. "Traceability Protocol for Establishing True
Concentrations of Gases Used for Calibration and
Audits of Air Pollution Analyzers" (Protocol No. 2,
June 1978), Environmental Monitoring Systems
Laboratory, Office of Research and Development,
U.S. Environmental Protection Agency, Research
Triangle Park, NC.
8. Reckner, L. R., "Development of Technical
Specification for Standard Gas - Diluent Mixtures for
Use in Measurement of Mobile Source Emissions"
U.S. Environmental Protection Agency, EPA-650/4-74-020.
129
-------
9. Saltzman, B. E., et al, "Performance of Permeation
Tubes as Standard Gas Sources", Anal. Chem. 5,
1121-28, (1971).
10. Singh, H. B., et al, "Generation of Accurate
Halocarbon Primary Standards with Permeation Tubes"
Environmental Science and Technology, 11, 511-513 (1977)
11. Hughes, E. E., et al, "Performance of a Nitrogen
Dioxide Permeation Device", Anal. Chem. 49, 1824-29,
(1977).
12. Pellizzari, E.D., "The Measurement of Carcinogenic
Vapors in Ambient Atmospheres", Section 6,
"Permeation System for Synthesizing Air/Organic
Vapor Mixture for Calibrating Instruments."
U.S. Environmental Protection Agency, EPA-600/7-77-055.
13. Mage, D. T., "Urban Diffusion Simulation Model for
Carbon Monoxide and the Need for Accurate Span Gas
Analysis," J. Air Poll. Control Assoc., 23, p. 970,
(1973)
130
-------
CONTENT OUTLINE /S
mmmmHmmmfmmmfmmmmmmmmmmm^fi^ 5 fsM?
Course 435 - Lesson #5
Lecture Title: GENERATION OF TEST ATMOSPHERES
UJ
O
<
Page-}- /_JL
NOTES
Review Lesson Objectives with the students.
INTRODUCTION
Test atmospheres are generated to provide calibration
standards for air monitoring instrumentation. A working
knowledge of preparation methods, stability, and availability
of gas standards is essential since this is probably the
greatest source of error in gas concentration measurement.
The problem with generating test atmospheres for the cali-
bration of ambient instruments is particularly difficult
because low levels (sub ppm range) of pollutant are
required. There are numerous ways to generate these levels,
but the following are in common use:
A. Dynamic Systems - continuous generation of atmospheres
(1) Dilute concentrated cylinder gas (e. g. concen-
trated cylinder gas followed by a series of
dilutions)
(2) Permeation Systems
(3) Ozone generated by exciting 02 with Hg vapor lamp
B. Static Systems - bag samples
Which system is the most accurate for generating the
standard is \dependent on the pollutant.
II. Pressurized Gas Cylindeis and the stability of Ambient
Concentrations of Sulfur Dioxide, Nitric Oxide, and Nitrogen
Dioxide contained in compressed gas cylinders.
A. Three basic types of materials used to contain Compressed gases
(1) Steel cylinders
(2) Aluminum cylinders
(3) Treated cylinders
B. Factors affecting tjhe stability of gas standards in
pressurized cylinders:
(1) contamination
(2) reaction
(3) absorption
(4) adsorption
131
Mention the NAAQS
levels for S02, 03,
N02, etc to
illustrate the low-
levels - measured.
L5-1
Only mentioned.
L5-2
L5-3
-------
CONTENT OUTLINE
Course: 435 - Lesson #5
Lecture Title GENERATION OF TEST ATMOSPHERES
a
Page I.. o/_JL
NOTES
In addition to the criteria gaseous pollutants (N02, S02> CO
and HC), industries and agencies are being required (e. g. by
the Toxic Substances Control Act, FDA, OSHA, etc) to
analyze for such compounds as vinyl chloride, ammonia,
hydrogen sulfide, and a variety of solvent vapors. The
difficulties in preparing trace level concentrations of
these compounds remain contamination, reaction, absorption,
and adsorption in addition to the method of preparation. We
will, at this point, confine our discussion to criteria
air pollutant gases.
C. Stability of Criteria Gases
1. Sulfur Dioxide
Sulfur dioxide is a highly reactive gas which has been found
to be unstable at low concentrations ( e. g. 100 ppm and .
lower). The instability is due to:
1. reactions with moisture
2. reactions with other trace gas impurities
3. reactions with the cylinder wall
2. Nitrogen Dioxide
Like sulfur dioxide, nitrogen dioxide is a highly reactive
and corrosive gas which has been found to be extremely
unstable at low concentrations (e. g. 100 ppm and lower)
for the same reasons.
Because of their instability in cylinders and the
availability of stable permeation devices (S02 and NO-)
and dilution systems Permeation systems are the best
methods for calibrating NO-N02~NOX or S02 ambient analyzers.
L5-4
A description of
the stability of
the gaseous criteri,
pollutants will be
emphasized since
students will be
most concerned with
these calibration
gases
L5-5
L5-6
*A stable gas mix-
ture is defined
as one in which the
concentration of
the trace gas changes
no more than 3%
from its original
concentration over
a 3-month period.
Point out that
permeation devices
and the associated
dilution systems
will be discussed
in detail later in
this lecture.
132
-------
CONTENT OUTLINE /£
----i-- § tsW*
Course: 435 - Lesson #5 ^
Lecture Title: GENERATION OF TEST ATMOSPHERES
01
O
<
Page.
of-A.
NOTES
3. Carbon Monoxide
The most common cylinder material for CO gas standards
has been steel alloys. Stable mixtures of 10-500 ppm
CO in nitrogen are available and may be stored at
temperatures from -10° to 100°F without loss of stability
in manganese steel cylinders. The selection of the
cylinder material is important since CO was found to be
unstable in chrome-moly and other ((treated) cylinders. The
manganese steel cylinders are heavier ( ~ 20 pounds)
which adds higher transportation cost - but provides a
stable calibration gas mixture. It is believed that
unstable CO mixtures are primarily the result of the
formation of iron carbonyls on the cylinder walls.
A. Nitric Oxide
Although NO is not a criteria pollutant, it is used in the
calibration of NO-N02-NO ambient analyzers and is, there-
for e/an important gas standard. 100 ppm cylinders of NO
are stable in steel or aluminum cylinders and are com-
mercially available.
Low level concentrations of both CO and NO can be easily
generated by dilution of cylinder gas (e. g. 100 ppm to
10 ppm by a ten-fold dilution)
5. Hydrocarbons
The stability of hydrocarbons in compressed gas cylinders
is dependent on the particular hydrocarbon for which a
standard is needed. In general, the more reactive
hydrocarbons are the least stable ...
L5-7
L5-8
L5-9
L5-10
relatively less stable:
relatively more stable:
aromatics, oxygenated or halogenated
hydrocarbons, etc.
L5-11
propane, butane, hexane, methane
(methane most commonly used in Air
Pollution monitoring)
6. Ozone and other Photochemical Oxidants
Because Ozone (0-) is unstable in any material for even
short lengths of time, the standard must be generated
and measured in-situ by an absolute technique
(e. g. UV photometry). Methods for preparing standards
for other photochemical oxidants such as the acyl nitrates
-0
L5-12
L5-13
(e.g. PAN
ment stage.
CH3-
-0 - 0 - N02) are still in the develop-
133
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CONTENT OUTLINE
Course: 435 - Lesson #5
Lecture Title: GENERATION OF TEST ATMOSPHERES
\
'/
Page
of _ §_
NOTES
III. Permeation Systems
Permeation tubes were originally described by O'Keeffe and
Ortman in 1966 as convenient calibration sources. They
consist of liquified gases such as sulfur dioxide, nitrogen
dioxide, hydrocarbons, halocarbons, or hydrogen sulfide in
an inert plastic tubing such as FEP Teflon (fluorinated
ethylene propylene copolymer) or TFE Teflon (tetra-fluoro-
ethylene polymer) which permeate through the tubing walls at
constant rates for long periods. The permeation rate is
extremely temperature sensitive; a change of 0.1°C can alter
the permeation rate on the order of 4%. The determination
of permeation rate or calibration of the tube is a straight
forward gravimetric procedure:
rate (yg/min) = ""init" nasfinal
time
Tubes which are purchased from NBS have certified permeation
rates at various temperatures.
They can be calibrated by a set-up in which the weight loss
of the tube is recorded directly. This avoids the possible
weigh errors due to the adsorption or absorption of water
vapor. The slope of the recorder trace is the permeation
rate.
In toto, a permeation system would consist of a permeation
tube which is maintained at a constant temperature (usually
by a water bath or constant temperature oven) and flow of
clean dry air across the tube (ranges from 10-500 cc/min.
depending on the permeation rate). This air stream is
further diluted with zero air in a mixing bulb. The flow
of the dilution air or the flow across the permeation tube
may be varied to give different concentrations of calibration
gas.
The concentration of the calibration gas in ppm
P (PR) (MV)
" «tot«l> (MW>
Where: C = concentration in ppm
PR = permeation rate in yg/min
MV = molar volume in yfc/ymole
Qtotal = total flow rate (flow rate across.the
permeation tube + the diluent gas flowrate)X,/min
MW = molecular weight in yg/ymole
As can be seen from the equation , the accuracy of the flow-
rate measurement is as important as the permeation rate,
_ 134
L5-14a
L5-14b
(Note: 2 major types
of permeation device i
exist*most common is
as in L5-14a. Other
is primarily for N02
as in slide L5-14b)
L5-15
Explain NBS cali-
bration set-up.
L5-16
L5-17
L5-18
L5-19
L5-20
Explain these
components on a
portable system
This equation is
derived by taking
the PR and dividing
by the flow rate
and then converting
the yg to ymoles
and from ymoles to
M&. Make sure
students understand
this is a variation
of the calculation
they performed in
Lecture #2 and home-
work exercises
-------
CONTENT OUTLINE
Course: 435 - Lesson #5
Lecture Title: GENERATION OF TEST ATMOSPHERES
o
T
Page.
of.
NOTES
PERMEATION SYSTEM CALCULATIONS
Problem 1.
L5-21
Given: Permeation rate = 1.75 pg S02/min @ 25°C
Permeation Temp = 25°C
dilution flow:
dilution air = 6350 SCCM (ml/min)
carrier across permeation tube = 50 SCCM (ml/min)
What is the concentration of the S02 atmosphere generated?
Solution: The molar volume @ 25°C, 1ATM = 24.46 y£/ymole
Molecular weight of S02 = 64 yg/ymole
cn
'total
SO,
= 50 SCCM (ml/min) + 6350 SCCM (ml/min)
= 6400 SCCM (ml/min) =6.4 A/min.
= (1.75 pg/min.) (24.46 p£/pmole)
(6.4 Jl/min.) (64pg/pmole)
= 0.105 \iKH = .105 ppm S02
Problem 2.
An S0? continuous analyzer has been calibrated with an NBS
permeation tube and a permeation system. A SO tube was
purchased commercially and it is desired to determine the
permeation rate using the calibrated S0« analyzer. The flow
across the permeation tube is 100 cc/min or ml/min and the
dilution flow is 1 £/min. The analyzer reads .250 ppm, what is
the permeation rate?
Solution: PR =
(Cppm) (MW) (Q
totalJ
MV
@ 25 C and 760 mmHg
PR = (.250)(64)(1.1)
(24.46)
= . 720yg/min
This is one of the steps for NBS traceability of commercial
permeation tubes: Traceability to Standard Reference Materials
is important in monitoring for a variety of reasons. The trace-
ability process is basically a sequence of prescribed analytical
procedures that relate a SRM (Standard Reference Material) to
Non-NBS standards.
135
L5-22
Jse blackboard to
un through this
jroblem
L5-23
-------
CONTENT OUTLINE /g
Course: 435 - Lesson #5
Lecture Title: GENERATION OF TEST ATMOSPHERES
\
\
UJ
O
Page.
of-JL
NOTES
IV. Preparation of (Zero) Diluent Air
In order to dilute gas standards from cylinders or gas
streams coming from permeation systems, clean, (e.g.'
free of the pollutant being measured and/or any possible
interfering species) dry "zero" air must be readily avail
able. Zero air can be purchased or prepared in-situ. In
general, this consists of passing the air to be cleaned
through:
1. filter to remove heavy oils and particulates
2.
3.
Molecular sieves and/or other drying agents
such as silica, perma-pure dryer, etc.
Having discussed
method of intro-
ducing the diluent
gas, a; method of
preparation of the
"zero gas" or
diluent air will be
discussed.
L5-24
UV lamp used to convert
adsorbed by carbon.
NO
to NO which is readily
4. Carbon bed to remove
and organics
filter
drying
agents
I I
Carbon
bed
UV lamp
air in
clean, dry
"zero" air
V. Methods for Dilution of Concentrated Gas Streams
Once a stable.relatively high concentration gas stream has
been generated by a permeation tube or cylinder gas, it is
necessary to accurately introduce a known volume of diluent
air (usually zero air) into a mixing chamber in order to
generate a specified concentration of pollutant. Generally,
this can be done by a single dilution or a series of
dilutions. Dilution systems consist of a flow control
mechanism and method to measure the flow - for example:
Flow control valves or flow metering valves and
a primary standard such as a soap bubble meter
(and timer) or secondary standards (rotameter or
mass flow meter) to measure the flow rate.
L5-25
iPictuEe of actual
\
drying set-up.
Explain components
in actual set-up.
L5-26
136
L5-27
Explain the operatio
of a fine metering
valve
-------
CONTENT OUTLINE ,
-*--*-- §
Course:435 - Lesson #5
Lecture Title: GENERATION OF TEST ATMOSPHERES
ul
O
PageJofJL
NOTES
\. adjusting the stem of the valve controls the opening of
the orifice and thus the flow.
Uses
It is used frequently for carrier gas control on gas
chromatographs and air flow control in many atmospheric
analyzers and sampling systems.
Vary pressure drop across an orifice and relate the pressure
drop to the flow rate
L5-28
e.g.
flow
rate
Pressure drop
Calculations: Basic Equation for dilution problems
C1V1 ' C2V2
or
C1Q1
Dilution Problem:
Given:
tank cone: 94.8
flow rate from tank: 4.6 ml/min.
flow rate of dilution gas: 2250 ml/min.
What is the concentration of diluted gas?
137
Slide L5-29
Students will be
using this method
in the laboratory.
Actual instrument
using % pressure
drop gauge as flow
rate control.
L5-29a
actraal instrument
L5-30
L5-31
-------
CONTENT OUTLINE
Course: 435 - Lesson #5
Lecture Titte: GENERATION OF TEST ATMOSPHERES
NOTES
c2 =
L5-32
tank concentration = 94.8
= tank flow rate = 4.6 mJl/min
= tank flow rate + dilution flow rate
= 4.6 m£/min + 2250 raJl/min = 2254.6 mA/min
(94.8 yfc/&) (4.6 ml/min).
2254.6 ml/min
L5-33
0.193 y)l/A
0.193 ppm
138
-------
S'nf NO 3S 7«
iNSfHt EMULSION SlOi DOWN
UST ATMOSPHERE GENERATION
FACTORS
AFFECTING
STABILITY
SULFUR DIOXIDE
SUIFUR DIOXIDE WSTAM.ITY
V
SO, AlUHMUM CYLHDCR
NITROGEN DIOXIDE CARBON MONOXIDE
NITRIC OXIDE
HYDROCARBONS
HYDROCARBON GENERAL STARILIt <
OZONE
OZONE GENERATION
50. PtRKCAION TUM
ff r(
PERMEATION SVSTEM
(PR) (MV)
(Q J («*)
PRODUCTION OF ZERO Aw
M« mvtacwlv w«|M m (t
F» - UK
NBS TRACEABILITY
Ken A SEQUENCE OF PRESCRIBED
ANAlVTICAl PROCEDURES THAT
'"V.,.. "ELATr ANDARDS
' -
DILUTION SYSTEK
FLOW CONTROL VALVE
*»« l A I ir t
139
-------
140
-------
LESSON PLAN
TOPIC: Air Movers
COUf?SE:435 - Lesson #6
LESSON TIME: 30 Min.
PREPARED BY: Northrop
DATE: 2/13/79
Services, Inc.
5
5SS
111
E
LESSON GOAL:
To introduce the types and principles of operation for various
pumps used in atmospheric sampling.
LESSON OBJECTIVES:
The student will be able to:
1. List six considerations in selecting an air mover
for a given sampling situation.
2. Differentiate between positive displacement and centri-
fugal pumps.
3. Describe the operation of the following air movers
a. Piston pump
b. Diaphragm pump
c. Vane pumps
d. Ejectors
e. Liquid displacement
SUPPORT MATERIALS AND EQUIPMENT:
1. Objective Handout
2. Carousel Projector and Slides
3. Overhead or blackboard
SPECIAL INSTRUCTIONS:
It will aid the instructional process to have examples of
the various pumps in the classroom for demonstration.
141
-------
SELECTED REFERENCES:
1. Furtado, V. C. and Harris, W. B., "Air Movers,"
Air Sampling Instruments. American Conference
of Governmental Industrial Hygienists.
Fourth Edition, 1972.
2. Kristal, F. A., and Annett, F.A., Pumps.
McGraw-Hill Book Company, Inc., New York,
1953, Ch. 1.
3. Mitchell, C. B., "Which Pump and Why?" Chapter 4
of Fluid Flow in Practice. Reinhold Publishing
Corporation, New York, 1956.
142
-------
CONTENT OUTLINE
Course: 435 - Lesson #6
Lecture Title: AIR MOVERS
O
NOTES
I. INTRODUCTION
An air mover is what the term indicates - a pump, mechanism,
or device for moving air.
It creates an air flow through the sampling system in order
to collect contaminants for analysis.
The air mover is an integral part of the atmospheric sampling
system.
II. CRITERIA FOR SELECTION OF AN AIR MOVER
1. Pollutant concentration and sampling time
2. Sampling rate required. Must sample at a sufficient
rate and time to collect the minimum quantity of
contaminant required for proper analysis.
Example: lOyg of contaminant required for analysis. Air
Mover samples at 1 nrVhr. Air contains an
average 1 yg/m^ contaminant. 10 hour sample
time would therefore be necessary.
Important in impingement systems where chemical reactions
times are involved, particulate sampling involving
inertia.
3. Physical and Chemical Nature of air to be sampled.
Air Mover must be resistant to abrasives, explosive gas
mixtures, corrosive gases, heat, cold, etc. common to
sampling site.
4. Portability of Air Movers
If Air Mover isn't in a permanent facility it must be
capable of easy relocation i.e., light, compact. External
power requirements - electricity.
5. Air Mover Noise
Important in closed work environment due to OSHA
standards, residential area uses.
6. Air Mover Maintenance
Should be serviceable in the field, parts should be
easily accessible, shouldn't be time consuming, parts
must be relatively inexpensive and easily purchased.
7. Resistance - Air Mover must overcome the resistance to
air flow caused by sampling device.
143
L6-1
Slide showing Air
Mover position in
a sample train
L6-2a
L6-2b
Show this example
on overhead or
blackboard
L6-2c
L6-2d
Slide
L6-2e
L6-2f
L6-2g
-------
CONTENT OUTLINE
Course: 435 _ Lesson #6
Lecture Title: AIR MOVERS
\
\
o
Page.
of.
NOTES
8. Constant Flow Rate - Important in knowing the true amount
of air sampled so as to calculate concentration of
contaminant per unit volume of air.
III. TYPES OF AIR MOVERS
L6-2h
A.
L6-3
1. Major device employed as an Air Mover
2. Two Types - Postive displacement pump, and centri-
fugal pump
a. Positive Displacement Pump
Characterized by a linear relationship between
suction pressure and pump capacity (as pump flow
rate increases, pressure drop across the pump
increases)
Operates by principle of air being displaced (move
by the, movement of movable, tight fitting parts
pistons, gears, lobes, etc. Two sub categories
of positive displacement pumps - Reciprocating
(Piston, Plunger, Diaphragm) and Rotary (gear,
lobe, vane)
b. Centrifugal Pumps
Ap to AQ relationship is not linear. Operate by
air being forced outward by centrifugal force
from an impeller. Movement of impeller creates
a low pressure at its center which draws air in.
The air is moved around by the impeller in a
volute casing (snail shell) which decreases
velocity but increases pressure. A common hair
dryer and Hi-Vol blower are good examples.
c. Description of Selected Pumps
1. Piston pump: air is drawn in through the
suction valve and displaced through the
discharge valve.
2. Diaphragm pump: A pulsating rubber diaphragm
moves relatively large volumes of air
3. Carbon vane: Of the rotary type. Are positive
displacement pumps in which the vanes or im-
pellers move rotationally requiring no suction
or discharge valving.
144
L6-4
L6-5
L6-6
-------
CONTENT OUTLINE
oT
Course: 435 - Lesson #6
Lecture Title: AIR MOVERS
UBV
of.
NOTES
B. Ejectors (aspirators)
Operate by jet principle - high velocity driving
force passed through a suction chamber. High
velocity stream result in lower pressure thereby drawing
in ambient air for sampling...uses Bernoulli's principle.
High velocity stream supplied by water, steam, compressed
air, C02, etc.
Advantages - No electrical power source required
Disadvantages -Time limit on driving force, low sampling
rates
C. Liquid Displacement
Operate by simple displacement of liquid in a closed
container by air upon release of the liquid; only used
in grab sampling.
D. Evacuated Flask
The flask is evacuated by means of a vacuum pump and is
then sealed. In the field, a valve is opened and air
being sampled is taken into the flask.
END OF CLASS FOR THE DAY
145
L6- 7
L6-8
L6-9
L6-10
-------
SITU n 3b 71
INSM1 tMUUION SIDE DON*
ASSIGNMENT _
Dcvtcct for
Moving Air
E<*U (OK ULf CTKM 01 *N *W «OVth
i tm siu cnon o* AH ut WVFK
^L T
POSITIVE DISPLACEMENT PUMPS
CENTRIFUGAL PUMP
EJECTORS ASPIRATORS
LIQUID DISPLACEMENT
CfT
146
-------
LESSON PLAN
TOPIC: PROBLEM SET I
COURSE: 435 - Lesson //7
LESSON TIME: 45 min.
PREPARED BY: Northrop DATE 2/1/79
Services, Inc.
LESSON GOAL: To review problem Set I with the students.
LESSON OBJECTIVES:
At the conclusion of this session, the student should be able to:
Work the exercises in problem Set I.
SUPPORT MATERIALS:
Overhead Projector or blackboard
Exercise Manual (Lab Manual)
SPECIAL INSTRUCTIONS:
Students are assigned this problem set as homework at the end of the
first day of the course. In the morning of the second day, the problems
are reviewed in class.
Students have difficulty with these calculations. They should,
therefore, be explained thoroughly. Students occasionally have
problems with dimensional analysis, therefore, include the units
in each problem.
147
-------
435 - Atmospheric Sampling
Problem Set I
EXAMPLE PROBLEM
Problem:
An atmosphere was analyzed for N02 using the TGS-ANSA
equivalent method. In this method the sample air is
drawn through a known volume of absorbing reagent where
the N0_ is quantitatively collected over a known time
period. The concentration of NO^ in the absorbing
reagent is determined by a colorimetric analytical
procedure. The following data was collected:
Solution:
Sampling Conditions: 25 C, 760 mmllg
Sampling Flowrate: 200 m£/min
Sampling Time: 24 hrs
N0? concentration
found in the Absorb-
ing Reagent: 3.0 yg/m£
Volume of Absorbing
Reagent: 50 m£
MW of NO.: 46 g/mole
Collection Efficiency: 93%
What is the NO- concentration in the atmosphere in
Mg/m and ppm.
(1) Determine the mass of N0« collected
Mass of NO,,
collected
/ concentration N02 in
Absorbing Reagent
Volume of
I Absorbing j
V Reagent /
= 3.0
MgNO,
50 m£ I = 150 ygN02
-------
(2) Only 93% of the N02 was collected; therefore, a
correction must be made to obtain the total amount
of NO (100%) that should have been collected:
(l50 UgN02) (
= 161
(3) Determine the volume of air sampled
Volume of air sampled = (flowrate) (time)
=(-I (24 hrs) [ J = 2
\ min / \ / \ hr /
(4) Calculate concentration
ygNO /161 ygN02\/10 A 3
^ - ^ITof = -T^""^^1 = 559yg/m
m , \
air x
3
(5) To obtain ppm convert yg/m to ppm
ppm
Ppm
air
46ygN00 /l ymole
2
0.297 vSL/H or
0.297 ppm
149
-------
ATMOSPHERIC SAMPLING
COURSE A35
PROBLEM SET 1 (1) Standard conditions for temperature and pressure
are 0 C and 760 mm Hg for most chemistry applications.
The molar volume (V) of an ideal gas at 0 C and 760 mm
Hg is 22.4 liters/mole. Standard conditions for report-
ing air pollution data is 25 C and 760 mm Hg. What is the
molar volume (V) of an ideal gas at 25 C and 760 mmHg?
3
(2) Convert 3200 yg S02/m to ppm S02 (y£SO /«.) if the
sampling conditions were EPA standard conditions, 25 C
and 760 mm Hg, (MW of S02=64g/mole).
(3) Thirty (30.0) liters of air were passed through 10
ml of absorbing solution. Chemical analysis of the solu-
tion gave a result of 0.3 micrograms of S0« per ml of
absorbing reagent. Assuming reference conditions of 760
mm Hg & 25°C and 100% collection efficiency, what was the
concentration of S02 in the atmosphere, expressed in y£/£
(ppm)? (MW of S02 = 64g/mole).
(4) Calibration of an NDIR Carbon Monoxide (CO) instru-
ment is sometimes done with static test atmospheres. In-
struments are usually calibrated at 90% of full scale.
A chemist wishing to calibrate the 50 ppm range of a
CO monitor must add how many m£ of 500 ppm CO to a
10 liter Tedlar bag to obtain a concentration of 45 ppm
(90% of 50 ppm).
(5) Using the following data on a N0_ permeation system,
calculate the concentration of N0_ expressed in ppm in
the test gas stream.
150
-------
Permeation rate: 1.65 yg/min @ 25.0 C
Permeation temperature: 25.0 C
Total flow rate: 3000 mil/min
Molecular weight NO-: 46 g/mole
(6) The single dilution system shown is used to calibrate
an NO-NO-NO instrument. If the flow from the 109ppm NO
2. x
109 ppm NO
Figure 1.
(NO) OUT
Single Dilution System
ZERO AIR
cylinder is 8.9 m£/min and the flow from the zero air cylinder
is 1500 m£/min, what is the concentration of NO exiting the
mixing chamber? :
(7) A high volume sampler was run for one day from midnight to
midnight. The initial flowrate was 55 cfm. The final flow was
53 cfm. The clean filter weighed 2.9845g. The filter weighed
2.9969g after sampling. What is the total suspended particulate
3
(TSP) concentration in yg/m ?
(8) A moving bubble meter is used to calibrate a lowflow
rotameter. The rotameter is placed before the bubble meter
in the calibration train. The bubble meter volume is 100 m&.
If the calibration conditions are 27.6 C and 756 mm Hg what
percentage error will be made if the bubble meter volume is
not corrected to dry conditions (tank air is used so the
rotameter is measuring dry air)? The vapor pressure of water
at 27.6°C is 27.696 mm Hg. HINT: Percent error is calculated
by the following formula:
% ERROR
True Value - Measured ValueUlOO)
True Value /
151
-------
CONTENT OUTLINE /£
Page.
of.
Course: 435 - Lesson 7
Lecture Title: PROBLEM SET i
\
Ul
O
PRO^
NOTES
SOLUTIONS TO PROBLEM SET I.
V
/298 °K
22.4£/mole V 273 °K
V = 24.46£/mole
nRT
This problem can be worked using the ideal gas law: V = ,
However, since the only parameter being changed is P
temperature and the volume at 0°C and 760 mmHg is given (22.4£)
it is more convenient to use Charles' Law. Review this if
necessary. This problem was also worked in class.
2.
(
3200 pg SO/*
)
1.22 y«,/£ or 1.22 ppm
Step 1: Determine total amount of SO- collected
j (lO ml J =
.3 pg/ml lO ml
3 yg
Step 2: Determine concentration in
3 yg/30 £ = .1 yg
Step 3: Convert yg/£ to
f.l yg/^N /
\ / \
Or .038 ppm
1 ymole\ / 24.46y)l\
64 yg / \ ymole /
.038
(500 ppm) V1
V, =
(45 ppm) (10£)
(45)
V, =
V, =
(500)
0.900 a
900 ml
152
-------
CONTENT OUTLINE /£
Course: 435 - Lesson 7
Lecture Title: PROBLEM SET i
Page.
of.
u)
O
NOTES
5.
(PR)(MV)
(QT)(MW)
(1.65 yg/min) (24.46 yl./ymole)
(3£/min) (46 yg/ymole)
.29 y£/Jl or .29 ppm
6.
C1Q1
C2Q2
(109 ppm) (8.9 ml/min) = C2 (1508.9 ml/min)
Q = Q + dilution air flow
(109 ppm) (8.9 ml/min)
2 = (1508.9 ml/min)
C0 = .64 ppm
Point out that all units cancel out except ppm.
7.
TSP in _yg = (W.. - W.) (10 )
3 . i i
m (flow) (Time)
3
Where flow is in m
min '
weight is in grams,
and time is in min.
TSP = (2.996% - 2.
/
\
_
53 + 55 cfm V.. 02832mj > (24 hrs) (60 min )
2 A"^3 / hour
= .0124 x 10'
2202.16
5.63 yg
m-
153
-------
CONTENT OUTLINE
Course: 435- Lesson 7
Lecture Title: PROBLEM SET I
\
UJ
O
Page _J of 1
NOTES
8.
V V /Patm ~ PH20
correct = original ( £
atm
V =100 [756.00-
/756.00- 27.696\
^ 756 7
V = 96.34 ml
% Error = /True Value - Measured Value\ (100)
\ True Value /
True value = 96.34 ml
Measured value = 100 ml
Error
9.6.34 ml - 100 ml
96.34 ml
= -3.8%
(100)
154
-------
LESSON PLAN
TOPIC: PRINCIPLES OF GASEOUS
SAMPLING
COURSE: 435 - Lesson //8
LESSON TIME: 45 Min. 0/1/in
PREPARED BY: Northrop DATE: 2/1/79
Services, Inc.
LESSON GOAL:
To recognize and understand the principles and equipment that are used
in sampling for gaseous pollutants.
LESSON OBJECTIVES: The student will be able to:
(1) Distinguish between the principles of grab and integrated
gas sampling.
(2) Identify the characteristics of adsorption, absorption, and
freezeout sampling.
(3) List at least two common materials used as adsorbents.
(4) List the type of samples most commonly collected by
adsorption and freezeout sampling.
(5) Describe at least one type of analytical procedure for
quantifying gaseous pollutants collected by adsorption.
(6) List at least two potential problems common to adsorbent
collection and analysis of gases.
(7) List at least two factors affecting collection efficiency
of an absorber.
(8) Distinguish the difference between physical and chemical absorption.
SUPPORT MATERIAL AND EQUIPMENT:
1. Objective Handout
2. Carousel Projector and Slides
155
-------
SPECIAL INSTRUCTION:
Although the content of this lecture deals with numerous gaseous
sampling methods, the specific details of methods for the
criteria pollutants should be avoided since they are discussed
in detail in the Reference Method Lecture (Lesson #12) on day
4. The lecture concerns principles and basic methods for
collecting and analyzing gaseous pollutants. Each principle or
technique should be illustrated with current examples as well
as the limitations and problems associated with each technique.
Avoid generalities, yet do not over emphasize one subject or
technique. For example, some of the techniques currently
being used in conjunction with adsorbent cartridges
(e.g. GC/MS) or in gas phase analysis ( e.g. a continuous pulsed
fluoresence I^S monitor, monitors for vinyl chloride using
chemiluminescence, etc.) are somewhat esoteric and beyond the
scope of a 45 min. introductory lecture.
SELECTED REFERENCES:
U.S. Department of Health, Education and Welfare,
"NIOSH Manual of Analytical Methods" NIOSH 75-121.
U.S. Department of Health, Education and Welfare,
"NIOSH Manual of Analytical Methods" Vol. 3, NIOSH/
77-157-C.
Dunlap, K.L., Sandridge, R.L., Keller, J.,
"Determination of Isocyanates in Working Atmospheres by
High Speed Liquid Chromatography", Anal. Chem. 47,
497-499 (1976).
"Polynuclear Aromatic Hydrocarbons: Trace Level
Determination in Workplace Air" Waters Associates,
Application Note # H71, Waters Associates, Inc.,
Maple Street, Milford, MA (1976)
Pellizzari, E.D., "The Measurement of Carcinogenic
Vapors in Ambient Atmospheres" EPA-600/7-77-055,
June 1977.
Black, M.S., Herbst, R.P., Hichcock, D.R., "Solid
Adsorbent Preconcentration and Gas Chromatographic
Analysis of Sulfur Gases" Anal. Chem., 50, 848 (1978)
Cheremisinoff, P.N., Morresi, A.C., Air Pollution
Sampling and Analysis Deskbook, Chapter 6,
"Ambient Sampling", Ann Arbor Sciences Publishers, Inc.,
Ann Arbor, Michigan, 1978.
156
-------
Madjar-Vidal, C., Gonnord, M.F., Benchah, P., Guiochon,G.
".Performances of Various Adsorbents for the Trapping and
Analysis of Organohalogenated Air Pollutants by Gas
Chromatography" J. Chromatogr. Sci., 16, 190 (1978).
Lewis, R.G., Brown, A.R., Jackson, M.D., "Evaluation
of Polyurethane Foam for Sampling of Pesticides,
Polychlorinated Biphenyls and Polychlorinated Napthalenes
in Ambient Air", Anal. Chem., 49, 1668 (1977)
Fine,'D. H., Et al, "Nitrosodimethylamine in Air",
Bulletin of Environmental Contamination and Toxicology,
15, 6, 739 (1976).
* These references are very specific for different airborne
pollutants - however, they illustrate most of the topics
discussed in this lecture.
157
-------
CONTENT OUTLINE ,
' |
Course: 435 _ Lesson #8
Lecture Title: PRINCIPLES OF GASEOUS SAMPLING
ul
O
NOTES
I. REVIEW LESSON OBJECTIVES WITH THE STUDENTS.
II. In sampling for gaseous pollutants, there are four
principles or methods that are most often used:
1. Absorption
2. Adsorption
3. Condensation or freezeout techniques
4. Grab sampling
These are the general methods that will be covered in
this lecture.
A. Absorption
The removal from a gas stream of a gaseous constituent by
a solid or liquid matrix in which the molecules of the
gas actually penetrate into the matrix.
1. Types of Absorption
a. Physical Absorption - (Dissolution) Material
penetrate the matrix with no chemical reaction involvet
ex. bubbling 0» into water.
Less stable than chemical absorption, temperature
dependent, high templower efficiency
b. Chemical Absorption - The gas reacts with the absorbing
medium to form another compound. This resulting
compound is somehow retained in the absorbing medium.
(gas) (liquid)
L8-1
L8-2
ex. L NH_ + n2b°4 *
Also temp dependent, reaction dependent
2. Absorbing Medium
a. Properties of Ideal Absorbing Medium
(1) Relatively non-volatile
(2) Inexpensive
(3) Stable
(4) Low - viscosity
(5) Moderate foaming
(6) Non-flammable
(7) Non-corrosive
(8) Non-toxic
Slides L8-3a-h
stress individual
properties. Slide
L8-3i can be used
alone if individual
stress is not desire 1
L8-3a
L8-3b
L8-3c
L8-3d
L8-3e
L8-3f
L8-3g
L8-3h
L8-3i
Good choice which fits all of these is distilled H20
158
-------
CONTENT OUTLINE /£
- Lesson #8
Lecture Title: PRINCIPLES OF GASEOUS SAMPLING
2 of 8
NOTES
b. Factors Influencing Absorbing Medium Selection
(1) Solubility
(2) Reactive properties of solvent and pollutant
(important in both physical and chemical
absorption)
(3) Subsequent analysis
3. Absorber
Device for containing the absorbent, allowing efficient
collection by the absorbent.
a. Factors Affecting Absorber Collection Efficiency
(1) Gas phase diffusion - should have some means of
of diffusing the gas passing into the absorbent.
This causes good mixing resulting in more
efficient capture (better distribution of
molecules)
(2) Liquid phase diffusion - should have some means of
allowing "fresh" absorbent to come in contact
with gas. Increases efficiency
(3) Residence time - the longer the time that the gas is
in the absorbent the better the collection efficiency
Especially true of chemical absorption. Depends
on flowrate.
(4) Bubble size - smaller the bubble the larger the
surface area of gas exposed to absorbent. More
surface area exposed, better the efficiency.
L8-4a
L8-4b
L8-5
(5) Solubility - mentioned earlier.
factors.
Refers to other
(6) Reaction time - related to residence time. In
chemical absorption, the reaction requires .a
certain amount of time. Shorter the time of
reaction, better the efficiency.
(7) Flow rate - related to bubble size, residence
time, reaction time.
Optimize these parameters to get high collection efficiency.
159
-------
CONTENT OUTLINE
I*
a
Course: 435 - Lesson #8 ^
Lecture Title: PRINCIPLES OF GASEOUS SAMPLING
Page-JL
NOTES
b.
Types of Absorbers
(1) Fritted Glass
(2) Impingers
efficient but susceptible to
clogging. Frit size (porosity)
is variable. Not used much now.
- bubble is broken up by an impinge
ment device thereby increasing
surface area and increasing
efficiency. Used a lot now.
L8-6
L8-7
(a) Smith Greenburg -
(b) Midget
large, has a plate fitted
below the bubbler opening
to act as impinger.
small, with bottom of the
tube acting as the impinger.
4. Limitations
a. Although an ideal absorbing medium would possess the
properties mentioned previously, no absorbing solution
possesses all these characteristics.
For example, the Sodium Arsenite method for collecting
N02 is ideal (1% sodium arsenite and O.lMNaOH) in most
respects. The arsenite, however, is toxic and requires
a strict disposal procedure.
Discuss the limitations of the wet S0_ method in
the same fashion (i.e. toxicity of TCM which contains
mercury-waste disposal problem).
b. Another limitation of collecting gaseous pollutants
via absorption in a bubbler is that the collection
efficiencies and interferents are sometimes unknown
or poorly defined. Systematic studies (e.g. inter-
laboratory and intra-laboratory collaborative test-
ing) have been carried out for the wet S02 and N02
methods establishing not only the collection
efficiencies but also that these methods can be used
with confidence by different groups. However, for
some of the more esoteric pollutants, this is not the
case.
160
Having discussed
the process of ab-
sorption in conjunc-
tion with bubbler
sampling trains in
general terms and th
factors affecting
collection efficienc
mention some practi-*
cal considerations.
Students are probab.'i
most familiar with
the wet methods for
the collection of
N02 and S02-
-------
CONTENT OUTLINE
Course: 435 _ Lesson #8
Lecture Title: PRINCIPLES OF GASEOUS SAMPLING
W,
o
PageJL-ofJL
NOTES
5. Applications
This technique can be used for the collection
of N02 or S02 as discussed previously. Other applications
can be found in the NIOSH Manual of Analytical Methods.
These include:
(1) Collection of cyanide and total fluoride via
impinger filled with 10 ml 0.1M NaOH
Individual applica-
tions are stressed
in slides L8-8a-8f.
Slide L8-8f can be
used as summary or
in lieu of series
a-e.
L8-8a
L8-8b
analysis
via
ion specific
electrode
(2) Collection of Acrolein via complexation
with 4-hexylresorcinol, in ethyl alcohol -
trichloroacetic acid in the presence of
mercuric chloride
L8-8c
forms a blue colored complex that is measured
spectrophotometrically.
(Abs = Ebc; c
Abs
Eb
)
(3) Collection of formaldehyde via reaction of
formaldehyde with an acid-sulfuric
V
acid reaction forms a purple complex that is
measured spectrophotometrically.
These are three typical procedures for collection of gaseous
pollutants by absorption.
There are many more described in the literature and the
NIOSH Manual of Analytical Methods.
B. Adsorption
The removal from a gas stream of a gaseous constituent by a
solid matrix in which the gas molecules are deposited on the
surface of the adsorbent.
Adsorption - outside
Absorption - inside
161
L8-8d
L8-8e
L8-8f
(Summary)
L8-9
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CONTENT OUTLINE
Course :435 - Lesson #8
Lecture Title: PRINCIPLES OF GASEOUS SAMPLING
\
\
<3
Page.
of-JL
NOTES
1. Types of Adsorption
a. Physical Adsorption - primarily due to electrostatic
forces.
e.g.
(1) Van der Waals Forces (define and explain)
(2) dipole-dipole interactions, especially
the strong dipole-dipole interaction of
hydrogen bonding which is dominant between
polar adsorbents and pollutants.
b. Chemical Adsorption - chemical reaction takes place
at the surface of the adsorbent.
2. Factors Affecting Adsorption Efficiency
a. Nature of the Adsorbent
(1) Surface area - larger, better
(2) Size and shape - rough, porous, best
(3) Polarity
(4) Reactivity
b. Temperature*
c. Velocity of air stream
d. Concentration of gases in stream
e. Degree of adsorption
3. Ideal Adsorbent
Granular, size, shape
High adsorptive capacity
Inert
Non-corrosive
Readily activated
Easy release of adsorbate
4. Typical Adsorbents
Carbon
Tenax GC
Porapack Q (and other polymeric GC solid adsorbents)
Polyurethane foam
Molecular sieves
XAD series
162
L8-10
L8-11
L8-12
L8-13
Instructor at this
point should pro-
vide some insight
into the properties
of at least two of
these adsorbents.
-------
CONTENT OUTLINE £g
Course: 435 - Lesson #8
Lecture Tif/e: PRINCIPLES OF GASEOUS SAMPLING
i
Ul
NOTES
Chemical structure of two typical sorbent resins
(point out the differences in chemical structures)
Gives rise to different uses - e.g. differences in polarity
5. Applications and Limitations
a. Illustrate the trade-offs involved in selecting
or using a particular adsorbent.
(1) For example, carbon is ideal in many respects:
(a) high adsorptive capacity
(b) granular etc.
(2) On the other hand, carbon cartridges have the
following disadvantages:
(a) variable collection efficiency (varies with
the carbon lot)
(b) pollutant desorption efficiency varies
(c) of all adsorbents, probably the most
susceptible to artifact formation
(e.g. in-situ reactions on the adsorbent
surface)
b. Adsorbent capacities are reported in the literature
for different pollutants (explain what is meant by
capacity - in GC this is termed breakthrough volume)
This could be a serious sampling error if this
information is not taken into account. You will
saturate the adsorbent.
L8-13a
Visuals for chemical
structures of
Tenax-GC and XAD
supplied.
The instructor may
opt to use other
typical adsorbents
with which they
have experience.
163
-------
CONTENT OUTLINE
Course: 435 - Lesson #8
Lecture Title: PRINCIPLES OF GASEOUS SAMPLING
UK1
Page.
of-L
NOTES
6. The following illustrate how some of the various adsorbent
can be placed in a sampling train and the related
analytical procedure.
(a) Typical high speed organic vapor collector.
(b) Collection of pesticides and PCBs in a polyurethane
foam by placing the adsorbent (e.g. polyurethane
foam)in the throat of a Hi-Vol.
(c) The adsorption process provides pollutant concen-
trations that can be detected and quantified by
analytical procedure.
Once the pollutant has been collected, the
analysis requires the pollutant to be removed from .th<
adsorbent by a process such as thermal desorption.
This thermal desorption involves heating the
adsorbent until the pollutants have been desorbed.
(d) The total sampling - collection - analysis process
as a system
C. Other sampling methods
1. Freeze-out or Condensation
An excellent application of this technique is described
by Fine, et al for the collection of ambient N-Nitroso-
dimethylamine.
a. Condensing gas constituent out of a gas stream by
removing enough heat from the system so that the
gas will change to a liquid when the boiling temp-
erature is reached.
L8-14
L8-15
L8-16
L8-17
Another type of
enrichment technique
b. Freeze-out Mechanisms
(1) Ice + H20
(2) Ice + Salt
(3) Dry Ice
(4) Liquid Oxygen*
(5) Liquid Nitrogen
L8-18
0°C
-16°c
-79°C
-183°C
-196°C
Select the bath for the temperature required to remove the
pollutant(s) of interest. Can be used for mixture separa-
tion. Used in stack sampling for moisture analysis.
*Avoid open flames when using liquid oxygen.
164
-------
CONTENT OUTLINE
Course: 435 - Lesson #8
Lecture Title: PRINCIPLES OF GASEOUS SAMPLING
I*
+t,
-------
'NSfN! (MULSION SIDE OOWM
PRMCIPU METHODS
FOR GASEOUS SAMPLING
ABSORPTION
PROPERTIES OF AN IDEAL
ABSORBING MEDIUM
PROPERTIES OF AN IDEAL
ABSORBING MEDIUM
PROPERTIES OF AN IDEAL
ABSORBING MEDIUM
D «? Ml f
PROPERTIES OF AN IDEAL
ABSORBING MEDIUM
PROPERTIES OF AN IDEAL
ABSORBING MEDIUM
PROPERTIES OF AN IDEAL
ABSORBING MEDIUM
PROPERTIES OF AN IDEAL PROPERTIES OF AN IDEAL
ABSORBING MEDIUM ABSORBING MEDIUM
PROPERTIES OF AN IDEAL
ABSORBING MEDIUM
i SUM* Non-comMfv*
FRITTED GLASS ABSORBER
FACTORS AFFECTING ABSORBER
COLLECTION EFFICIENCY
> Hm« Ftow rate
APPLICATION*
APPLICATIONS
APPLICATIONS
APPLICATIONS
Coi«r.rjj**tr IA t .1 M rfoeo
IDEAL ADSORBENT
TYPICAL ADSORBENTS CHCMICAI
-------
167
-------
LESSON PLAN
TOPIC: PRINCIPLES OF PARTICULATE
SAMPLING
435 - Lesson #9
COURSE:
LESSON TIMEa hr. 15 min.
PREPARED BY: Northrop DATE:2/l5/79
Services, Inc.
LESSON GOAL:
To develop an understanding of the principles and instrumentation
that are used in particulate sampling.
LESSON OBJECTIVES:
1. Describe three principle types of particulate collection
devices: gravity, filtration, impaction and recall
examples of each.
2. Identify at least two common errors in inertial
collection of particulates.
3. Describe the mechanism for size fractionation by
inertial sampling.
4. Define collection efficiency of an impaction device.
5. List four properties of aerosols and four properties
of collecting devices which affect the collection
efficiency of impactors.
6. Discuss how the following particulate samplers
operate and what each is used for:
a. Cascade Impactor
(1) Andersen Impactor
b. Cyclone Samplers
8.
Describe the rationale for size fractionation of ambient
particulate matter.
Define the differences between respirable and non-
respirable particulate matter.
168
-------
9. Describe how the dichotomous sampler
fractionates respirable and non-respirable
particulate matter.
10. Discuss -some of the advantages and dis-
advantages of the three types of filter
materials.
SUPPORT MATERIAL AND EQUIPMENT:
Objective Handout
Carousel Projector with slide tray
SPECIAL INSTRUCTION: None
SELECTED REFERENCES:
Corn, M., Esmen, N. A., "Field Sampling of Airborne
Particulates", American Laboratory, July, 1978, p.13.
Dzubay, T. G., Hines, L. E., and Stevens, R. K.,
"Particle Bounce Errors in Cascade Impactors", Atmospheric
Environment, 10:229 (1976)
Stevens, R. K. and Dzubay, T. G., Dichotomous Sampler -
A Practical Approach to Aerosol Fractionation and
Collection" US Environmental Protection Agency, EPA-
600/2-78-112, 1978.
Wedding, T. E., McFarland, A. R., and Certnak, T. E.,
"Large Particle Collection Characteristics of Ambient
Aerosol Samplers", Environ. Sci. and Tech., 11, No. 4:387
(1977).
Gelman,' C., and Meltzer, T.H. , "Membrane Filters" Anal.
Chem., 51 (6) 22A-31A (1979).
Smith, W. B., Gushing, K. M., and Lacey, G. E.,
"Andersen Filter Substrate Weight Loss" US Environmental
Protection Agency, EPA-650/2-75-022, 1975.
Stevens, R. K., and Dzubay, T. G., "Recent Developments
in Air Particulate Monitoring" IEEE Transactions on
Nuclear Science, Vol. NS-22, No. 2, p. 849-855 (1975).
169
-------
CONTENT OUTLINE
Course: 435 - Lesson #9
Lecture Title: PRINCIPLES OF PARTICULATE SAMPLIN&
S*.
NOTES
Review lesson objectives with the students
I. INTRODUCTION
In particulate sampling, as in gaseous sampling, there are
many methods and combination of methods for sampling.
The methods to be discussed in this lecture are:
1. Gravity
2. Filtration
3. Impaction
The general requirements of any particulate collection
device are:
1. Low pressure drop
2. High and known collection efficiency
3. Resistant to chemical and physical attack
4. Resistant to moisture
5. Withstand high temperature and/or extreme low
temperatures ..._.
6. Collected material easily removed
7. Low noise, low cost and maintenance require-
ments.
II. GRAVITY
Dustfall jar best example, usually made of resistant material
Jar is often contained in stand which serves to protect the
jar from spilling. Wire rim to protect it from collecting
bird droppings. Sampling period is usually 30 days, but can
be variable. Results are calculated by filtering liquid,
then weighing solids.
III. FILTRATION
Hi-Vol and tape samplers are examples.
The tape sampler was also used for episode monitoring at
one time and also used for fluoride sampling to some extent.
Modified Hi-Vol reference method now used in episode
monitoring.
Properties of Filter Media in Common Use
1. Cellulose Filters - originally designed for liquid
solid separation
Advantages:
Low ash content
Generally inexpensive
170
Good collection efficienci
Low metals background
L9-1
L9-2
L9-3
L9-4
L9-5a
L9-5b
L9-5c
L9-5d
L9-5e
L9-5f
L9-5g
L9-6 \ ,
(I
y
I
L9-8
iigh Volume sampling!
was discussed in >
detail in a '
previous lecture
L9-9
L9-10
L9-11
ss
-------
CONTENT OUTLINE /g
Course: 435- Lesson #9 \^
Lecture Title: PRINCIPLES OF PARTICULATE SAMPLiff&i
Use in a variety of applications
Disadvantages;
Pressure drop is often high
Non-uniform flow and variable collection efficiencies
Hygroscopic
Artifact formation (SO? and NO-)
Glass Fiber Filters
Finely spun glass fibers pressed with an organic binder;
binder is usually flashfired off for air sampling.
Advantages
High collection efficiency
Non-Hygroscopic
Moderate Pressure drop
Used routinely in high volume sampling
Disadvantages
Fragile - breaks apart easily
Not especially suited for microscopy.
Difficult to remove particulate matter
Variable composition
Contamination, commonly Fe, Al, Mg, Na, and K.
Difficult to ash - high silica content
Filters are not neutral pH - aids in artifact formation,
especially for sulfates and nitrates.
Membrane Filters
Generally dry gels of cellulose esters.
They are commonly cellulose acetate or cellulose nitrate.
Manufacturing process can control both pore size and
internal membrane structure.
These filters can be made of Teflon.
Note: Filtration
samplers do not
operate solely as a
"strainer"but also
uses diffusion,
inertia, and
electrical forces.
See Course Manual
for a more detailed
explanation.
L9-12
L9-13
Refer to table in
Course Manual for
specific filter
names and specifi-
cations.
171
Page.
of-2. _
NOTES
L9-14
-------
CONTENT OUTLINE
i
Course: 435 - Lesson #9
Lecture Title: PRINCIPLES OF PARTICULATE SAMPLIN&.
Page.
of.
NOTES
Advantages
Selective pore size
Adaptabilityfor example can be manufactured
for a variety of applications, e.g. low ash
easily dissolved, etc.
Relatively inexpensive
Moderately non-corrosive
Suited for microscopic . studies
Disadvantages
High pressure drop
Tend to be brittle and need a backing
Short sampling times tend to plug quickly
in areas of high particulate concentration
Static charge build-up
Variations in pore diameter. ' .
L9-15
IV.
IMPACTION
Inertia:
A particle with a constant velocity is resistant
to changes in speed and direction
See course manual
for more details
on this
L9-16
L9-17
This property of particles moving in an air stream is used
in air sampling to collect particles in groups of varying size.
Larger particles which do not have the momentum to remain in thje
air stream when the air makes a quick change in direction
and then collide with and remain on the impaction or
collection surface.
The momentum and inertia pf_ particles are properties of
aerosols that are utilized to give size fractionation in
impaction devices. These properties also affect the
collection efficiency of a particular impaction device. The
efficiency is that fraction of particles in an incident
aerosol stream that are retained on the collection surface of
the sampling device. The properties of collection devices tha
affect collection efficiency are:
L9-18
172
-------
CONTENT OUTLINE /g
^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^ i W^J^ffr
Course: 435- Lesson //9 \^
50 m/s
2. Jet shape - though not that significant.
3. Distance between the jet and collection surface.
Usually decreases with each successive stage...
controls degree of deflection of particle stream...
large deflection angle required for small particles.
4. Collection Surface - Shape, texture, degree of
attraction (e.g. sticky or hard)
^Factors affecting the inertia of particles and the collection
efficiency of an impactor.
Velocity of the air stream (the velocity of the air
stream imparts a certain velocity to the particle)
Particle mass and density
Electrical forces: attractions or repulsions that
build up on the collection surface
Mobility - a function of particle size, mass and
density.
Examples of Impaction Devices
Impaction collection devices are used to separate
particulate matter into size fractions. One type
is generally referred to as a "Cascade Impactor". The
cone shape of the entrance nozzle increases the air .
velocity and particles are separated according to mass
because particles with the higher mass fall out first...
intermediate particles fall out in later stages.
1. A type of Cascade Impactor is the Andersen Sampler.
This sampler uses various numbered and sized holes
to produce different jet velocities which gives
rise to a size fractionation among the various
stages. There are two types: viable (for biological
sampling) which uses petri plates with selective
media and non-viable which uses sticky plates or
filter paper for collection.
173
Page.
NOTES
L9-19
L9-20
L9-21
L9-22
L9-23a
L9-23b
L9-23C
L9-23d
L9-23e
Several of these
properties combined
are referred to
as stickiness of
particles.
L9-24
L9-25
L9-26
L9-27
L9-28
-------
CONTENT OUTLINE
Course: 435 - Lesson #9
Lecture Title: PRINCIPLES OF PARTICULATE SAMPLING
^^^^
NOTES
2.
A modification of the High Volume Sampler
is the High Volume Andersen Sampler. With slight
variations, it operates similar to the Cascade
impactor. It is adapted to fit on standard High
Volume Samplers. It has a higher (20 (ifm) sampling
rate and better collection efficiency. The impaction
occurs as the stream turns from one hole to the next.
Sierra cascade Impactor operates with slits instead of
holes and can operate at a flowrate of 40 cfm or greate
Another type of impaction device is the Cyclone
Sampler. This is an inertial separator without moving
parts. It separates particulate matter from a carrier
gas by transforming the velocity of an inlet stream intD
a double vortex confined within the cyclone. The enter
ing gas spirals downward at the outside and spirals
upward at the inside of the cyclone outlet. The parti-
culates, because of their inertia, tend to move toward
the outside wall, from which they are led to a receiver
t Not efficient collectors of particles with a
diameter <5ym.
Often used as a preseparator with filters.
Disadvantage of collecting large particle fraction
on their inner walls which must be cleaned off.
L9-29
L9-30
L9-31
L9-32
L9-33
3.
Another type of impaction device is the Rotorod
Sampler. This is really impaction in reverse; instead
of particles being moved onto the collection surface,
the collection surface is moved into the particles.
Rotating arms contain removable bars which are coated
with a sticky substance. The bars are removed after
sampling and analyzed microscopically. This sampler
has been used mainly in pollen sampling.
Limitations and Sources of Error for Cascade Samplers
L9-34
Mention only briefly
L9- 35 a
1. Particle shattering; this gives rise to inaccurate
size fractionation. This is especially important in
particle size determinations and respirable dust
studies. Specifically, particles > 200 ym are often
shattered; > 50 ym , some particles are lost by impaction
on walls;<5 um,difficult to collect because momentum of
particulates is not appreciably different from air strejam momentum.
2. Re-entrainment of particles and wall losses - again
causes inaccurate sizing results.
L9-35b
Limited sample quantity - true for many of the low
flow rate, high pressure drop samplers, that use
membrane filters.
174
L9-35c
-------
CONTENT OUTLINE
Course: 435 - Lesson #9
Lecture Title: PRINCIPLES OF PARTICULATE SAMPLiifo
Page.
of.
NOTES
L9-36
V. Rationale for size fractionation and the potential new
particulate standard.
The 1977 Clean Air Act Admendments required that existing
ambient pollutant standards be reviewed by 1980. One that
they will consider changing is TSP. Since the total sus-
pended particulates measurement includes particles which are
both inhalable (less than 15 ym) and not inhalable (greater
than 15 pm), non-attainment of the TSP standard at present
may be the result of particulate which does not constitute
a health hazard, even though they do cause adverse public
welfare effects.
Present (TSP) Standard has problems.
Larger particles > 15 ym are not very harmful
Hi-vol inaccuracies (see Lesson 4)
Wind blown dust and sand causes high levels of TSP
in Western states.
Particles smaller than 15 ym are inhaled to at least the
upper respiratory tract.
Secondary data may be required on "fine" size fraction
(smaller than 2.5 ym) in order to develop control strategies
but will not be part of the standard. At one time it was
thought that the "fine" fraction <2.5 ym vs. the course
fraction > 2.5 < 15 ym was the more important health hazard,
but since then it was found that inhalables posed an equal
threat. - (One reason for the design of the Dichotomous
Sampler - evaluate the need for a "respirable" "fine" standard).
If an additional or revised standard is found necessary it
would likely be proposed in the 1980's. Of the several approaches
for a standard Reference Method for collecting Inhalable Par-
ticulates the Dichotomous Sampler has been given much attention L9"-37
in EPA evaluation and testing.
Dichotomous Sampler
Originally designed to meet the need of separating
"respirables" from "non-respirable" the dichotomous sampler
has the added advantage 'of collecting both the fine and
course modes to give the total < 15 ym particles or Inhalables.
*It is also believed that large particles can enter into
the digestive system where they too may pose a threat to
human health, e.g., cancer of the stomach.
175
-------
CONTENT OUTLINE
Course: 435 - Lesson #9
Lecture Title: PRINCIPLES OF PARTICIPATE SAMPLIN^
(»
Page.
of 8
NOTES
L9-38
Consists of two modules, the sampling module and the control
module. The two separate modules allow locating the samp-
ling module on the roof of an air-quality monitoring
station with the control module inside. The inlet is designec
to have an upper particle size cut-off to prevent entry of veiy
large particles, (greater than 15 pm). The sampled particles
smaller than 15 pm pass through the flow-straightening inlet
tube and enter the virtual impactor head. The particles are
then accelerated through the impactor nozzle. By virtue
of their greater inertia, particles >3.5 pm impact into the
"void" of the receiver tube. To prevent back flow, the
receiver tube has a flow rate of 0.1 m-^/hr. The coarse
particles greater than 3.5 pm, and 1/10 of the fine particles
are collected on a 37mm Teflon filter. The fine-particles
flow at a flowrate of 0.9 nr/hr. (15.0 £pm) around the
receiver tube and are collected on a second 37 mm filter.
Advantages of the Dichotomous Sampler
1. Separates particles into respirable and non-
respirable fractions.
2. "Bounce" and particle shattering found in Cascade
impactors is eliminated
3. The sampler is omnidirectional (e.e., does not
suffer from the wind directional sensitivity like
that of the Hi-Vol sampler)
4. Particulate is collected on membrane filters
which facilitates chemical analysis by x-ray
fluorescence - (gives elemental composition).
(Teflon filters may be used).
Other more cost effective approaches to collecting the
Inhalable fraction have been suggested: (1) Tape Samplers
(2) Size select inlet - Adapts to a standard Hi-Volume
Sampler (SSI).
Omni-directional inlet. Uses inertial impaction
to procure a clear particle size cut-point of
15 pm. Flow must be held constant (e.g. 40 cfm) to
achieve this distinct cut-point. (See lesson on
Inertial Samplers). Collects particles on a standard
8 x 10 glass fiber filter.
L9-39
L9-40
L9-41
L9-42
176
-------
CONTENT OUTLINE /£
Course: 435 - Lesson #9
\
v, x
Lecture Title: PRINCIPLES OF PARTICULATE SAMPLING^ "RO^
Page
of
NOTES
Review with class questions
1. What are three common filter materials used
in atmospheric sampling?
2. What are two sources of error in inertial or
impaction collectors?
3. Explain the rationale for size fractionation
of particulate matter?
4. What are the properties of impaction collectors that
affect collection efficiency?
(see objectives)
177
-------
STYLE NO 35 71
INSERT EMULSION SIDE DOWN
PARTICULATt SAMPLING
REQUIREMENTS Of
A COLLECTOR
GRAVITY
REQUIREMENTS Of
A COLLECTOR
Low pr«uur« drop
Htgh and known ffld^Ky
ftMtetom to ctwmfcel attack
REQUIREMENTS Of
A COLLECTOR
Low pf uur* drop
tafetant to moHtuf*
REQUIREMENTS OF
A COLLECTOR
Low pttHur* drop
IMPACT1ON
REQUIREMENTS OF
A COLLECTOR
tow ptttiur* drop
Vhtvtand tcmpwotur* »xtr
REQUIREMENTS OF
A COLLECTOR
Low pr*Mur« drop
* Knlitont to dwmkol ouacK
R»*!jlom to moiltur*
DUSTFALLJARS
Hi Vol Tap* Sompin
FILTRATION
CEUULOSE FILTERS
GLASS FIDER FILTERS
MEMBRANE FILTER
A poitkt* wlih a axwam v*kxHy
li rttHiam to dxmgM In ip*«) ond
dlncilon. Oty** of robtonc* l>
propoftkxxjl to mou.
INEM1AL COtLECTO*
FAQORS AFFECTING INERTIA FACTORS AFFECTING WERTIA FACTORS AFFECTWG INERTIA
Ponkk vrtodty
Porlld* v«4odty
AkKwamwIodTy
P
-------
s *«
FACTORS AFFECTING INERTIA FACTORS AFFECTING INERTIA
PortiCl* v*(ocliv
Parnc'# ("now and density
Pafpct* velocity
* Atr ur*om velocity
1 PQTIKI* mau and d*mif y
j Eitctncol totcej
* Pofttc(«moWlrty
CASCADE IMPACTOR
CASCADE SAMPLER
Limitations and Error Sources
Particle shattering
CYCLONE i»»PUR
CASCADE SAMPLER
Llmltotions and Error Sources
* Particle shattering
Re-emralnment and wall
losses
CASCADE SAMPLER
limitations and Error Sources
Potticie shattering
Re-«ntfOlnment and wall
- Limited sample quantity
-Virtual Impose- H»od
ADV AMI AGES OF
DICHOTOMOUS SAMPLERS
frtKtio«iOf« f»x>f'Qb(* Qrvd
'Kx»-f»iplrobl» po" kulotff
179
-------
LESSON PLAN
TOPIC: LABORATORY SAFETY BRIEFING
COURSE: 435 - Lesson #10
LESSON TIME: 30 Minutes
PREPARED BY: Northrop DATE: 2/21/79
Services, Inc.
SB.
ui
CD
LESSON GOAL: Familiarize students with general safety considerations.
Each lab instructor will review safety in his or her laboratory.
Generally,
1. Safety glasses will be worn at all times while in the
laboratory.
2. Lab coats should also be worn. Never worn to
cafeteria, etc.
3. No canvas, sandals, or open-toe-shoes.
4. Point out fire extinguishers in each lab.
5. Clearly show emergency exits.
6. Absolutely no smoking, eating, or drinking in the lab.
7. No horseplay.
8. Fire safety equipment, what and how is alarm sounded,
exit routes, etc.
9. Safety facilities, (e.g. eye flush, showers, hoods)
A. location
B. operation
In addition to the above general safety precautions, specific safety
considerations for the High Volume Sampler and Standard Test Atmospheres
labs follow:
1. High Volume Sampler Lab
A. Check all electrical cords for cracked insulation and
loose plugs.
B. If it is necessary to run extension cords on floor, the
cords must be securely taped to floor.
180
-------
C. Rootsmeter stands must be sturdy and stable.
Test Atmospheres Lab
A. Compressed gas cylinder safety.
1. All cylinders must be clamped to lab benches or
placed in cylinder stands.
2. Cylinder valve protection caps must be left on cylinders
until the cylinders have been properly secured and are
ready for use.
3. Cylinders should be moved by using a suitable hand truck
(one that has a retaining chain or belt).
4- No part of a cylinder should be subjected to a temperature
above 125°F.
5. Eye washes and safety showers should be located near cylinder
use areas, but out of the immediate area which is likely to
become contaminated in the event of a large gas release.
6. When cylinders are considered empty, the following procedure
should be followed:
a. cylinder valves should be closed
b. valve protection caps should be attached to the cylinders
c. cylinders should be labeled "Empty"
d. cylinders should be placed in a proper storage area
(segregated from full cylinders)
B. Compressed gas cylinder regulator operation
1. Attach the regulator to the cylinder without forcing threads.
2. Check for leaks using a soap solution.
3. Turn the delivery pressure adjusting screw until it turns
freely.
4. Open the cylinder valve slowly until the cylinder pressure
gage on the regulator registers the cylinder pressure.
5. With the flow control valve at the regulator outlet closed,
turn the delivery pressure adjusting screw clockwise until
the required delivery pressure is reached.
6. Open the flow control valve until the required flow rate
is obtained.
181
-------
LESSON PLAN
TOPIC: PROBLEM SESSION II
COURSE:435 Lesson #11
LESSON TIME: 45 Min.
PREPARED BY: Northrop DATE:2/l/79
Services, Inc.
LESSON GOAL:
To review Problem Set II with the students
LESSON OBJECTIVES:
At the conclusion of this session, the student should be able to:
Understand and work the exercises in Problem Set II
SUPPORT MATERIALS:
Overhead Projector or Blackboard
Laboratory and Exercise Manual
SPECIAL INSTRUCTIONS:
Review as completely as possible
Answer all student questions.
182
-------
435 - ATMOSPHERIC SAMPLING
PROBLEM SET II
EXAMPLE PROBLEM
2. A High-volume sampler at site 137 ran for 24:00 hours with an Initial
visifloat reading of 55 and a final visifloat reading of 53. The initial
(tare) weight of the filter was 4.5288 grams, under equilibrium conditions.
After sampling and re-equilibration the filter and sample weighed 4.6437
grams.
Determine the concentration in yg/m using the following information:
(a) An orifice device numbered 173457 was calibrated in the lab with the
following results. The temperature and pressure in the lab was 24°C
and 762 mm Hg respectively.
Resistance Volume Time APm
Plate No. Passed ft3 fain) mm He in. of H?0
5 200 5.553 93 2.95
7 200 4.463 80 4.7
10 300 5.515 66 7.2
13 300 4.925 55 9.5
18 300 4.488 46 11.7
(b) The high volume sampler at site 137 was calibrated using device
numbered #73457 in the field with the following results. NOTE;
The temperature was 10°C and pressure 770 mm Hg at the time of
calibration.
Plate No. AP2 in. of water Visifloat Reading
5 2.85 34 '
7 4.40 42
10 6.25 51
13 7.70 57
18 9.40 62
SOLUTION;
1. Appropriate calibration curves for orifice unit should be drawn up as
follows :
183
-------
3
(a) Volumes must first be converted form ft (as read off rootsmeter) to
m using a conversion factor of .02832 m /ft . This yields (V ) 5.6m3
for 200 ft and 8.4m for 300 ft3. m
(b) Since the orifice device lowers the pressure within the rootsmeter
below atmospheric by AP we must correct each volume by that amount
using:
P - AP .
atm m '
-- _ -
P
atm
-, .. c ,r
Plate no. 5 - V _ -
actual
c £ 3 /762 mmHg - 93 mmHg\
= 5.6m I -- =^75 - ^ - &
\ 762 mmHg /
3
V _ - = 4.92m V = Actual Volume
actual a
Do this for plates nos. 7-18 with the following results: True air Volume:
(V m3) = 5.01, 7.67, 7.79, 7.89m.
d.
(c) Using these true air volumes you can now divide by the appropriate times
it took these volumes to pass through the rootsmeter to give you true
flowrate Q m /min.
Q.
3 3
Volume ,., t ,. v n _ - 4.92m .886m /min
-- = flowrate (Qa> plate no. 5
Do this for plate nos. 7-18 with the following results: 1.123, 1.39,
1.76m3 /min. (Q )
a
3
(d) Plot Q m /min vs. AP, in inches of H?0 (pressure drop from orifice
device; on log-log paper. This curve is for lab conditions of 24°C and
762 mm Hg. (See Fig. I)
(e) In this case, field conditions were different from lab conditions
(temp and press.), therefore a new calibration curve should be drawn
up. (In Fig. I this is plotted alongside of the lab orifice curve)
The Equation for temperature and pressure corrections for flows is as
follows:
Q (corrected) = Q (lab)I / 2 . 1 (Note square root sign)
3 [to field a V Ti P2
condition
T°K = 273 + T°C
field condition
plate no. 5: Q _ 8661/283. 762
corrected to = ' * 77°
QQ - .860 m3/min
a "~ ' ~ *
corrected to
field condition
Do this for plates nos. 7-18 with the following results: 1.09, 1.34, 1.53,
1.70 m /min. Plot new Q 's against A?1 for curve reflecting field
conditions. (See Fig. IJ
184
-------
lOEAIITHBIC 2 I 3 C«Ui
I. Orifice calibration curve
Lab conditions
T « 24°C, P 762 mmHg
ttf
Corrected for field conditions
T=10°C, P« 770 mmHg
1 4 S 6 1 8 9
incbes of H2O
17191
-------
Figure II. Viufloat calibration curve
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2. Using field condition curve just plotted find a Q (true flowrate) that
corresponds to the AP» as read in the field (use AP, axis on curve). Plot
these Q (now designated Q,) against your visifloat reading on linear paper.
These extrapolated Q 's for plates 5-18 are as follows: .82, 1.03, 1.24,
1.37 and 1.5 m /min (check these yourself). (See Fig. II)
2
3. To determine concentration of particulates in yg/m use the formula.
TSP yg/m = (Wfg - W.g) x 10 (conversion of g to yg)
/Ff+Fi\
\~~2~)
(m3/min)
t = our sample ran for 24 hours x 60 min = 1440 min
hr
convert flow indication readings to Q. readings from curve II
Ff 55 = 1.33 m3/min
F 53 = 1.28 m3/min
QF I _1.33 + 1.28 . , 3, .
= I . J m /min
Wfg - W±g = 4.5288g - 4.6437g = .1149 grams x 106 jog_ = 1.149 x 105 yg
g
TSP = 1.149:.x 105 yg
1.3 m3/min x 1440 min
6.13 x 101 yg/m3
187
-------
ROBLEM SET 2 (1) An orifice calibration unit was calibrated in the
laboratory with the following results (24°C, 762 mm Hg)
Vm
cubic feet
200
200
300
300
300
T
minutes
5.7
4.49
5.53
4.86
4.45
APm
mm Hg
95
82
60
56
48
APX
inches of water
3.0
5.0
7.9
10.2
12.7
A high-volume sampler and visifloat were calibrated in
the field at 24°C and 762 mm Hg with the above orifice
calibration unit with the following results:
AP2 Visifloat
inches of water reading
3.1 31
4.9 38
7.4 47
9.2 52
10.9 57
Plot the appropriate curves and use these to solve the
following problem:
A high-volume sampler was run for 24:00 hours with
an initial visifloat reading of 57 and a final visi-
float reading of 55. The initial (tare) weight of
the filter paper was 4.5314 g., after sampling and
re-equiibration to less than 50% relative humidity,
the filter paper and sample weighed 4.6524 g.
Determine the concentration of particulate expressed
in micrograms per cubic meter, under the following
conditions.
188
-------
Temp Barometric Pressure
Lab conditions 24°C 762 am Hg
Field conditions 24°C 762 mm Hg
(2) Determine the concentration of participates if the
above experiment was run under the following conditions.
Temp Barometric Pressure
Lab conditions 24°C 762 BO Hg
Field conditions 36°C 711 mm Hg
(3) A high-volume sampler was run for 24:00 hours. The
weight gain on the filter was 0.2550 grams. The sampler
has a recorder for recording the actual air flow over the
entire sampling period and the attached chart was obtained
during this sampling run.
Using the calibration curves from problem II, calculate
the micrograms per cubic meter using the following methods:
( assume Transducer curve is identical to visifloat curve)
A. Use recorded air flows at start and end of sampling
period.
B. Use recorded air flow for every two (2) hours.
C. Assume that the result in B is correct and calculate
the Z error in A.
189
-------
wcte
Froblen 2, Tigure 2-1 Pressure transducer recording for Froblea 2.3
190
-------
OR CONTENT OUTLINE ^
^1 ^^n Course: 435 - Problem Session II \^^mlim^ g
ULjBBl Lecture Title: Atmospheric Sampling ^ PRO^
1. V = Volume measured by rootsmeter at reduced pressure
m
P = Barometric pressure
a.
Ap = Read off mercury manometer
m 3 1
Vm in ft can be converted to nr at this step. However, flows
can be calculated in ft /min and placed on graphs. We are
converting at this step, and graphs reflect this.
200 ft3 = 5.66 m3, 300 ft3 = 8.49 m3 from f. 02832 m3 1
I *'j
correct each volume (Vm) by this formula:
V = (Vm) /Pa - Apm} V = actual volume corrected for
\ Pa / pressure drop caused by orifi
(1) V =5.66 m3 /762mmHg - 95 mmHg\ = 4.954m3
(formerly 200 ft3)\ 762 mmHg /
(2) V = 5.66 m3 /762mmHg - 82 mmHg^ = 5.05m3
a \ 762 mmHg /
(3) V0 = 8.49m3 /762 - 60 \ - 7.821m3
\ 762 >
(4) Va = 7.865m3
(5) Va = 7.955m3
V.,(m3) Time (min)
4.954 5.70
5.050 4.49
7.821 5.53
7.865 4.86
7.955 . 4.45
/ 0 \
Q /m \ _ Va Qa APi (inches of
a \minl Time / 3 , . N water)
\ / 1 m /mini
0.869 3.0
1.125 5.0
1.414 7.9
1.618 10.2
1.787 12.7
A curve for your calibrated orifice consists of plotting Qa vs. Ap
(Fig I) (on Log-Log paper)
191
Page-1 ofJL
NOTES
:e
-------
LOGARITHMIC
46 7320
2X3 CYCLES »«D£ IN u. 5. «.
KEUFFEL a ESSER CO.
7891
Ap, (inches of water)
-------
CONTENT OUTLINE /£
Course: 482 ~ Lesson
Lecture Title: Atmospheric Sampling
UJ
O
PRO
°
Page1_ of'.
NOTES
The next step consists of calibrating a visifloat against the
calibrated orifice. Because you are at the same conditions
in the field as you were in the lab... No corrections are
needed.
The Ap9 (inches of water) can be related to a volume flow by
using the log-log plot from your calibrated orifice.
Aj?2 (inches of water)
(AP1 on plot)
3.1
4.9
7.4
9.2
10.9
Q1 m /min
c -i i
from log-log
plot (Q on plot)
3.
.88
1.12
1.38
1.52
1.68
Visifloat
Reading
31
38
47
52
57
Plot visifloat reading vs. flow (0^). (Fig. II) on linear paper.
This is a curve for thi calibrated visifloat.
Use this curve to convert flow indication readings (visifloat)
to actual flow readings Q, m /min.
F.57 = 1.68 m /min
F^SS =1.62 m3/min
r
Average /I.68 + 1.62\ . ,_ 3, ,
Flow =( 2 ) 1>65 m /min
mass,.-mass.= .1210g
TSP in p£ = /liass (g) - Mass (g)\ [106 y^j
3 V / V g/
m
in
/AVE f low Q' (m-Vminfi /(t (min)\
V rate ' /\ /
(.12lOg\ flO6 M)
« A LV s_/
m
fl^nr. \
\ min/
50.9 yg
3
24 hrs.l [60_min
hr
m
193
-------
10 X !0 TO Y, INCH 7 X 10 INCHES
KEUFFEL & ESSER CO. M»Dt IN U.S.*.
46 1323
-------
CONTENT OUTLINE /g
Course: 435 - Lesson 11
Lecture Title: Atmospheric Sampling
\
o
Page.
NOTES
2. Now, field conditions have changed and are different from the
conditions at which the orifice was calibrated. Therefore,
the flow must be corrected to the new temperature and pressur
Average flow reading = 1.65 m /min
correct by:
corr
Q = 1.65
Tneasured
& found from
curve
3 f
mn
297 711
Q = 1.74 m. /min
TSP in
3
.mogHio
)
. 74
m3\(24 hrsJ/'
Mn" A y V
min\
hr
= -48.3 vg/ 3 at new conditions
m
when correcting
flow remember v-
Note
273
K
Ideal Gas Law
equation dictates
that T must be in
3. a. Use visifloat curve as a transducer curve here:
initial
corresponds to 1.76 m /min from curve
Q
^final = 42-cfm corresponds to 1.24 m /min from curve
1.5m/min
Average flow reading using just initial and final readings,
Volume of air = (24 hrs)(60 min) (1.5jn ) - 2160 m"
hr min
TSP in ug/m3 = (.255g)(106 ug/g) = 118.0 yg/m
2160 m3
195
-------
HH CONTENT OUTLINE
^^jn^J Course: 482 - Lesson #11
LM_jflV Lecture Title: Atmospheric Sampling
^eosr,,^ 6 af 6
{^! NOTES
TT A Converted to actual flows
Using 2 Hour Averages from Transducer Curve/Visiflojit curve
3b. Q - 2: 59~ft3/min = 1.74
2-4: 57=ft3/roin = 1.68
4-6: 54 = 1.59
6-8: 49 = 1.44
8 -10: 46 = 1.36
10 -12: 45 = 1.32
12 - 2: 44 = 1.30
2-4: 43.5 = 1.27
4-6: 43.5 = i.27
6 - 8: 43.5 = 1.27
8 -10: 42.8 = 1.40
10 -12: 42.4 - 1.38
|| = Q = 1.42 m3
mm
V = (1440 min) (1.42 m3 ) = 2044.8 m3
min
TSP in yg/m3 = (.2550 g) (106 yg/g)
2044.8
= 124.7 yg/m3
3c. % Error = (True Value - Measured Value\ , nn
\ True Value / X 10°
_ /124.7 yg/m3 - 118.0 yg/m3)
V 124.7 yg/m3 '
- 5.37% error
196
m /min
m /min
m /min
m /min
m /min
m /min
m /min
m /min
m /min
m /min
m /min
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LESSON PLAN
TOPIC: AMBIENT REFERENCE METHODS
FOR GASES
COURSE: 435 Lesson #12
LESSON TIME: 2 hours
PREPARED BY: Northrop DATE: 2/21/79
Services, Inc.
LESSON GOAL:
To develop an understanding of the principles and operation
of the Reference Methods for monitoring gaseous pollutants.
LESSON OBJECTIVES:
The student will be able to:
1. Distinguish between a Reference Method or Measurement Principle
and Calibration Procedure and an Equivalent Method for ambient
; air pollutants.
2. List the gaseous ambient pollutants now specified as criteria
pollutants.
3. List the Reference Method or Measurement Principle and
Calibration Procedure currently specified for each criteria
pollutant.
4. Describe the operating principles of each Reference Method.
SUPPORT MATERIALS AND EQUIPMENT:
Objective Handout
Slide Projector and slides
List of Designated Reference and Equivalent Methods
SPECIAL INSTRUCTION:
None
SELECTED REFERENCES:
Ellis, E.G., "Technical Assistance Document for the Chemiluminescence
Measurement of Nitrogen Dioxide" US Environmental Protection Agency,
EPA-600/4-75-003
Others given in the lesson plan.
197
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CONTENT OUTLINE /g
Course: 435
Lecture Title: AMBIENT REFERENCE METHODS FOR
\
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13
NOTES
REFERENCE AND EQUIVALENT METHODS
A. Reference Method - One specific method of analysis for a
particular pollutant which is set as the standard by EPA.
B. Equivalent Method - A method which has been found experimentally
accurate enough by EPA to matchanalysis specifications given
for the reference methods (range, precision, sensitivity). This
provides a freedom of choice for establishing monitoring networks
according to Federal guidelines.
These methods (Reference and Equivalent) were chosen by the EPA
after a comprehensive review of available methodologies for measur-
ing the criteria* pollutants. Although, perhaps, not representative
of "state of the art" techniques, these methods have been carefully
evaluated and errors and/or interferences quantified where possible.
They also represent the legal methods required by EPA for use in most
federally mandated ambient monitoring. There is no difference
legally in a Reference and Equivalent Method,. Either may be used
for monitoring, so the choice of Reference versus Equivalent should
be based on other factors such as cost, availability, etc.
A Reference Method may be either manual or automated. If
manual, it is a detailed chemical procedure specifying all important
parameters. If automated, it consists of a measurement principle
(MP) and a calibration procedure (CP). Thus for an automated
method, any instrument using the measurement principle
(and designated by the EPA) is a separate reference method. Among
the gases, SO,, is the only manual Reference Method...N0», 0.,, CO,
and hydrocarbons (HC) use automated methods and thus follow
particular measurement principle ; there are several reference
methods for each.
For a current list of the designated Reference and Equivalent
Methods, contact address at top of list handed out in class. For
additional information, see first page of the list.
The Federal Reference Methods (i.e., the complete description
of the procedure for manual methods and the detailing of the
measurement principle (MP) and calibration procedure (CP) for auto-
mated Methods) are contained in the Appendixes to 40 CPR 50
*NOTE: Criteria pollutants refer to those pollutants for which
there is a national ambient air quality standard (NAAQS). The name
is derived from the document which provides the criteria for select-
ing a particular pollutant level as the standard. These include
SO,,, 0_, N0?, CO, Hydrocarbons, TSP, and Lead.
L12-1
L12-2
L12-3
L12-4
198
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CONTENT OUTLINE £g
Course: 435 - Lesson #12 '
Lecture Title.-AMBIENT REFERENCE METHODS FOR GA
\
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2 nf 13
NOTES
Currrently these are:
Pollutant
Total Suspended Particulates (TSP)
Lead
Sulfur Dioxide (SO,,)
Ozone (0 )
Hydrocarbons
corrected for Methane
Method
Hi-Volume Sampler
Manual
Hi-Volume sampler with
subsequent Atomic
absorption analysis
Manual
Pararosaniline Method
Manual
chemiluminescence with
ethylene (MP)
Ultraviolet photometry
(CP) Automated
gas chromatography with
a flame ionization
detector GC /FID (MP)
span gases (CP)
Automated
Chemiluminescence with
Ozone (MP) gas phase
titration (GPT) of an
NO standard with Ozone
or N0? permeation
device (CP)
Automated
Non-dispersive infra-
red spectrometry
(NDIR) (MP)
span gases (CP)
Automated
This lecture deals only with the gaseous pollutants or the last 5
on the list so ...
L12-5
L12-6
Nitrogen Dioxide (N02)
L12-7
Carbon Monoxide (CO)
Note: It will
probably prove
useful to quickly
review the
Appendixes of
AOCFR50 con-
taining these
methods before
lecturing.
199
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CONTENT OUTLINE
Course: 435 - Lesson #12
Lecture Title: AMBIENT REFERENCE METHODS FOR
tW?i
*ttZJ
NOTES
Sulfur Dioxide (S00)
Current Standard
Primary _
80 pg/m (0.03 ppm) -
365 Mg/ta (0.14 ppm) -
Annual
Arithmetic
Mean
Maximum 24 hr
concentration
not to be
exceeded more
than once
per year
Mention that std is
given for infor-
mation only
Not required to be
memorized.
L12-8
Secondary
1300 jag/m (0.50 ppm)
Maximum 3 hr.
concentration
not to be
exceeded more
than once per
year
The Federal Reference Method for SO is a Manual, wet chemical
Method involving bubbling air at a controlled rate through an
absorbing reagent. The exposed reagent is then chemically altered
to a colored solution and the intensity of color is related to the
S0~ concentration .
Now, to examine the reaction in more detail . . .
S02 is drawn through a solution of potassium tetrachloromercurate
(K-HgCl.) also known as TCM. A reasonably stable dichlorosulfito-
mercurate complex (K HgCl-SO ) is formed. This solution of TCM + the
complex is reacted with pararosaniline(tris 4-amino-phenylmethanol,
C H gN.,0) and formaldehyde (CH_0) to form an acid (pararosaniline
mechyl sulfonic acid) which is intensely colored (a purplish-pink).
Then a spectrophotometer is used to measure the absorbance at 548 nm.
L12-9a
b
c
d
L12-10
S0
TCM
complex
L12-11
Complex + pararosaniline
w/formaldehyde » Acid dye
dye absorbance at 548nm is proportional to SO-
concentration
By Beer-Lambert
Relationship
A = abc
where
A » Absorbance
a » constant
b = path length
c « concentration
200
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CONTENT OUTLINE £g
Course: 435 - Lesson n2 ?
Lecture Title: AMBIENT REFERENCE METHODS FOR a
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Page.
of.
13
NOTES
***NOTE:
***
This material is somewhat technical and the level of in-
struction should be determined from the individual class
population.
The following chemistry is included as information not
absolutely necessary to discuss with entire class only
interested individuals
(H2S03) pK=1.8
[H20 S021 3=*: IH+]
PK=6.9
2[H+] + [SOj ].
K2H8CI4
it
[0]
I
2IH+]
SC>2 in TCM equilibrium equations.
/ Improved temperature stability of sulfur dioxide samples J\
\collected by the Federal Reference Method from EPA-600/4-78-018, p.7'/
In field operation, a flow controller is required capable of
measuring flow within ±2%. Can use hypodermic needles or critical
orifices size of needles recommended is in Method different
size (i.e., diameter and length) for different flows. Whichever is
used, a membrane filter is required to prevent blockage.
The flow rate and bubble size are very important in this method
and affect collection efficiency.
Flow controlled as mentioned, bubble size by using a glass
impinger, 6" long with a 0.6 mm i.d. tip. Calibrate with
jeweler's drills #79 fits, #78 shouldn't. Calibration procedure
is time consuming and clumsy drills bits stick and break.
Assembled units in sample box . Point out various parts
including pump, absorbers, impingers, filters, flow controller.
L12-12
L12-13
201
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CONTENT OUTLINE /£
Course: 435 - Lesson #12
Lecture Title A^1^1 REFERENCE METHODS FOR
5_^__i!
NOTES
Calibration of the sampling train involves checking the
calibration of the impinger(s), orifice(s), and total system.
To obtain a calibration curve for the spectrophotometer
wet chemical solutions of sodium sulfite ormetabisulfite can be used
or alternately an SO- permeation tube can be used to generate
required SO- concentrations.
For complete calibration information, see Appendix A 40CFR50.
PROBLEMS AND ADDITIONAL CONSIDERATIONS
Most pressing problem is temperature instability
Three pertinent publications :
"Effect of Temperature on Stability of S02 Samples Collected
by the Federal Reference Method" EPA 600/5-76-024.
"Sulfur Dioxide Bubbler Temperature Study", EPA-600/4-76-040.
"Improved Temperature Stability of S0? Samples Collected by
the Federal Reference Method" EPA-600/4-78-108.
3
Over the range of 35 to 278 yg S02/m , absorbed S02 is lost. Rate of
decay increases five-fold for every 10 C increase in temperature
over range 20°C to 40 C.
First publication gives a mathematical model that allows sample decay
to be calculated if temperature history of sample is known.
Second publication evaluates 2 commercially available temperature
controlled sampling boxes and gives guidance on constructing a
suitable unit from a small refrigerator.
Third publication deals with chemistry of reaction and an attempt
to improve absorbing solution.
All three are useful.
MINOR PROBLEMS INCLUDE:
Toxicity of TCM (Readily absorbable through skin potential
source of Mercury poisoning if mishandled). Also problem with
waste disposal
Pararosaniline dye often does not meet specifications and must
be purified.
Sizing of impingers bubble size and flow rate do affect
collection efficiency.
202
L12-14
spectrophotometer
calibration should
be checked periodi-
cally using neutral
density filters
L12-15
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CONTENT OUTLINE /S
mmmm*mmmmimmmmmtmmHmmmmm*mm 5 Vsff^1
Course: 435 - Lesson #12
Lecture Title- AMBIENT REFERENCE METHODS FOR
\
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NOTES
KNOWN INTERFERENTS AND CORRECTIVE ACTION
N02 - Removed from TCM by treating with sulfamic acid before
formaldehyde and pararosaniline are added.
Ozone (0~) 20 minute time delay between sampling and
analysis will allow ozone to decompose.
Heavy Metals Removed by addition of a chelating agent
(ethylenediamine tetra acetic acid - EDTA)
Oxidants in distilled water Need to use high purity, freshly
boiled, cooled distilled - water in preparing reagents
OZONE (03)
L12-16
helating agents
merely complex or
"tie up" the netals
to prevent an
interference
L12-17
Current Standard - Primary
0.12 ppm - hourly average with the expected
number of daily exceedances not greater than
one per year as averaged over the previous
three year period
Secondary
Same as primary
Ozone is an automated method, therefore^'it consists of a
stated measurement principle and a calibration procedure.
Measurement principle is Chemiluminescence with Ethylene (C«H.)
Chemilutninescence is merely a term describing a chemical reaction
which emits light energy as a by-product. This type of principle
is also used for the determination of NO-.
L12-18
very .
reactive
reaction
uncertain
C2H4
-^Ozonide
0
-^Aldehyde
Light
L12-19
H/ o-o \H
The sample stream enters the analyzer and is mixed with ethylene in
a reaction chamber. The light energy emitted from this reaction is
then measured by a photomultiplier tube ( a device converting the
light energy to an electrical signal) and is related to the ozone
concentration.
L12-20
203
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CONTENT OUTLINE
Course: 435 - Lesson #12
Lecture Title: AMBIENT REFERENCE METHODS FOR
Page-I nf 13
NOTES
The light intensity is measured by the photomultiplier tube at
420 nm. The basic reaction and principle is reasonably simple and
usually operates trouble free.
A Bendix 8002 chemiluminescent Ozone monitor
The calibration of ozone monitors currently follows two choices
1. Boric acid potassium iodide (BAKI)
2. Ultraviolet photometry (UV)
UV photometry is the preferred method, but BAKI will be allowed for
an *18-month phase-in period to allow labs to obtain and become
familiar with the equipment required for UV photometry. The phase-
in period ends on August 8, 1980** and after this date any
calibration method used will have to be referenced to the UV method.
An ozone generator, consisting of a low pressure, Mercury vapor lamp
is used to produce ozone for both calibration methods. The amount
of 0, produced is a function of the oxygen content of the air stream,
the irradiating energy (i.e. the intensity of the bulb) and of
course the flow rate.
The specifications for a generator are given in
40CFR50.
U.V. PHOTOMETRY CALIBRATIONS
Appendix D of
The air stream containing ozone is introduced into a manifold
which is then sampled concurrently by the analyzer being calibrated
and a UV photometer.
To calibrate with a UV photometer, several things must be done:
1. The source of zero air should be the same
as the air supply being used to produce
ozone.
2. An attempt should be made to determine
if ozone loss is occurring in the absorption cell
of the UV photometer.
3. Temperature and pressure of absorption cell
should be known.
Some other points of interest, especially in using a Dasibi 0_
monitor as a calibrator are noted in two Technical Assistance
Documents (TAD's) from the Environmental Monitoring Systems Lab
(EMSL) (Address is on list of designated methods). These documents
deal with:
1. Technical Assistance Document for the
Calibration of Ambient Ozone Monitors
2. Transfer Standards for Calibration of
Ambient Air Monitoring Analyzers for Ozone
L12-21
L12-22
*proposed time peril
subject to change
*18 months from date
of publication
L12-23
'L12-24
L12-25
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CONTENT OUTLINE
Course: 435 - Lesson #12
Lecture r///£».AMBIENT REFERENCE METHODS FOR GAS^
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NOTES
BAKI CALIBRATIONS
The Boric Acid KI technique is a modification of the neutral
buffered KI (NBKI) technique that was formerly the calibration
procedure. Due to inherent chemical errors, (Often resulting
in errors of 15-30%) NBKI was replaced.
The stoichiometry of the reaction is:
03 + 2I~ + 2H = I2 + 02 + H20
The sampling arrangement is the same as with UV photometry, with
the exception that you sample concurrently with an analyzer under
calibration and a BAKI sample train. This train is composed of
2 midget impingers in series filled with the BAKI absorbing reagent.
This technique is not dissimilar from the NBKI
1. Sample stream is bubbled through impingers (2 all glass
midget impingers in series at a flow of 0.4 to 0.6 £/min.).
2. Absorbance of the 2 impingers is determined with a
spectrophotometer at 352 nm. This absorbance relates
directly to 0« concentration by Beer-Lambert relationship.
(i.e., A calibration curve is prepared using a standard
iodine solution and this plot - concentration versus
absorbance - is used during the subsequent calibration).
PRECAUTIONS AND ERRORS
a. 0., is very reactive, therefore the sampling train must be
kept compact and composed of glass and teflon.
b. The absorbing reagent must be checked for the presence of
reducing compounds. Procedure is contained in the Method.
If the procedure is followed carefully, errors should be reduced to
jf2%. (Error value is from "Further developments in ozone cali-
bration using Boric Acid Buffered KI", presented at 71st Annual
APCA Meeting, June 25-30, 1978, by Daniel L. Flamm,
Richard J. Paur, and Kenneth A. Rehme)
To return to the measurement principle (chemiluminescence with
ethylene), the only identified interferent is H»0 which can cause
a small positive bias. The actual reason for this bias has not
been established.
L12-26
For students who
desire it - stress
that it is not
required to be
memorized.
L12-27
205
L12-28
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CONTENT OUTLINE /g
Course..'435 - Lesson #12
Lecture Title: AMBIENT REFERENCE METHODS FOR
PageJi nf 13
NOTES
To summarize, the 0,, reference methods are based on:
Automated Method
LI2-29
Measurement Principle
Chemiluminescence with
Ethylene
Calibration procedure
Ultraviolet (UV) photometry
or (during phase-in)
Boric Acid
Potassium Iodide (BAKI)
HYDROCARBONS CORRECTED FOR METHANE OR NON-METHANE HYDROCARBONS
(NMHC)
Current Standards
Primary
160 fig/mj (0.24 ppm)
Maximum 3 hr concentration (6-9 a.m.)
not to be exceeded more than once per
year.
Secondary
same as primary
L12-30
NOTE: The standard for NMHC is designed for use as a guide in
devising State Implementation Plans (SIPs) to achieve the
ozone standard. It does not mean that hydrocarbons as a
class are a health or welfare hazard (although obviously
some - benzene, etc., are problems)
AUTOMATED METHOD
Measurement principle is gas chromatography using a Flame
lonization Detector (FID)
Calibration procedure involves using a series of calibration
gases.
Gas chromatography is a technique which allows for separation
of compounds. The hydrocarbons are thus separated and then
burned or ionized in a hydrogen flame. The flame is the
heart of the FID. Most commonly, the procedure is as follows:
1. 1st Cycle - Determination of total Hydrocarbons.
All hydrocarbons in the sampled air including
methane are burned in the flame and detected.
This signal is stored as total hydrocarbons.
L12-31
L12-32
206
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CONTENT OUTLINE
Course..-435 - Lesson #12
Lecture Title: AMBIENT REFERENCE METHODS FOR GA
tu
O
2.
3.
4.
5.
6.
7.
2nd Cycle - Sample Is passed over a stripper
column which removes CO-, H~0, HC heavier than
CH,. Air leaving column contains only CO + CH,.
CO, CH^ mixtureProceeds to an analytical column
where they are separated.
CH, then goes through a methanator column which
causes no change in the methane. It then goes
to the FID where the methane is measured and the
signal is stored.
The CO follows the methane through the methanator
and is reduced to methane. It then leaves as
methane to the FID where it is measured and the
signal is stored as CO.
The stripper column is back flushed to clean
the column to prevent FID contamination.
The non methane total Hydrocarbon Concentration
is determined manually or electronically by
subtracting Methane Concentration (signal) from
the total Hydrocarbon Concentration (signal).
The CO measurements are not sensitive enough to allow their
use for ambient monitoring. They can be used for relative values
however.
The Beckman 6800 Air Quality Chromatograph is an example of
this technique. As can be seen, this method involves valving and
switching of flows . There are problems (leaks, sticking valves,
etc.) that need to be carefully checked.
CALIBRATION
The Federal Register Calibration procedure requires
that various concentrations of Methane be used.
PROBLEMS AND ERRORS
The sampling for ambient levels of NMHC by the Federal
Reference Method has many difficulties. We will discuss some of
the more significant.
207
P/7/7P 10 nf 13
NOTES
L12-33
L12-34
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CONTENT OUTLINE /g
Course:435 - Lesson #12
Lecture Title: AMBIENT REFERENCE METHODS FOR
0
11
13
NOTES
1. The FID has a non-linear response to
increasing number of carbons In hydrocarbons.
In general, the response decreases with increas-
ing number of carbon atoms. Also, response can
vary depending on the chemical structure (type
bonds and bond placement)
2. GC columns and FID have individual response
characteristics. They are not interchangeable.
3. The detector cell is temperature sensitive.
Must be insulated.
4. Span drift may exceed EPA specifications
(+5% for 24 hours)
5. Atmospheric moisture content appears to affect
measurements.
6. Poor accuracy at concentrations near NAAQS.
For further discussion of errors with this method see:
"Evaluation of the EPA Reference Method for
the Measurement of Non-Methane Hydrocarbons -
Final Report" EPA-600/4-77-033.
Further developmental work is being done to revise this
method, and caution is advised in its application.
L12-35
L12-36
L12-37
, L12-38
L12-39
L12-40
NITROGEN DIOXIDE
L12-41
Primary Standard:
.05 ppm or 100 ug/m
Annual arithmetic mean.
Secondary Standard: Same as primary standard
Ambient air contains both nitric oxide (NO) and nitrogen dioxide
(NO ). The measurement principle for nitrogen dioxide requires
thai nitrogen dioxide first be converted to nitric oxide and then
using the measurement principle of the chemiluminescence resulting
from the reaction of nitric oxide with ozone to indirectly measure
the concentration of nitrogen dioxide.
L12-42
NO + 0,
N0
N0
0
hv
The light, thus produced, passes through an optical filter that
isolates a given spectral region and strikes a photomultiplier (-PM)
tube. The intensity of the emission is directly related to the
concentration of NO.
208
L12-43
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CONTENT OUTLINE fg
Course:435 - Lesson #12 '
Lecture Title: AMBIENT REFERENCE METHODS FOR G;
\
Page
of _ il
NOTES
Nitric Oxide is measured directly. Total oxides of nitrogen
measurements are made by catalytic conversion of nitrogen dioxide
to nitric oxide by a carbon base and/or other metal converter
resulting in a total oxide of nitrogen concentration
(NO = NO + N02). The difference between total oxides of nitrogen
(N0~ + NO) and nitric oxide is a measure of nitrogen dioxide con-
centration.
CALIBRATION:
There are two methods designated for the calibration of a
NO-NO - NO- analyzer. The first method involves the rapid Gas
Phase Txtration of an NO standard with 0,,. This produces a known
channel of the
3',
amount of N0~ which is used to calibrate the NO
instrument.
NO + 00
To obtain stoichiometric quantities of N0?, the residence time, the
time allowed for the reaction to occur, is critical and specifi-
cations for the reaction chamber, flow rates, etc., are given in
Appendix F of 40CFR50.
L12-44
L12-45
L12-46
L12-47
The other method for the calibration of the NO
use of a NO
2 channel is by the
permeation tube with a dilution system. The
N02 produced from the permeation system is diluted with zero air
to produce known concentrations of NO-. This is used to calibrate
the NO- channel of the instrument.
An NO standard in combination with a dilution system is used to
calibrate the NO and NO channels of an NO-NO - N09 instrument.
X X &
An excellent document for use in the calibration of these instrument
is "Technical Assistant Document for the Chemiluminescence
Measurement of Nitrogen Dioxide", US Environmental Protection Agency,
EPA-600/4-75-003.
L12-48
This was discussed
thoroughly in a
previous lecture.
L12-49
CARBON MONOXIDE
Primary Standard J
1 hour standard = 35 ppm (40 mg/m,)
hour standard - 9 ppm (10 mg/m )
to exceed more than once a year
Secondary Standard: Same as primary standards
The Measurement Principle for determining carbon monoxide is non-
dispersive infrared spectrometry.
Infrared light passes through the sample and reference cells and the:i
passes through a bandpass filter which limits the wavelengths of
light entering the detector cell. The reference cell is filled with
a non-absorbing inert gas such as argon or nitrogen. If no
pollutant gas is present in the sample cell, the amount of radiation
reaching the reference half and the sample half of the detector cell
__ 209 _
L12-50
L12-51
L12-52a
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CONTENT OUTLINE
Course: 435 - Lesson #12
Lecture Title: AMBIENT REFERENCE METHODS FOR
Ul
O
T
13 nf 13
NOTES
will be equal; therefore, the temperature (and resulting pressure)
of both halves of the detector will be equal. As pollutant gas
enters the sample cell, the energy reaching the sample half of the
detector will be less, due to the absorption of some of the infrared
light by CO. The temperature (and resulting pressure) is lowered
on the sample side of the detector cell facilitating a distention
in the diaphragm (the pressure is directly related to the
temperature of a gas at a constant volume.) The distention of the
diaphragm produces a capacitance change that is converted to a
voltage output by the instrument. The optical chopper serves to
create an alternating current (ac) signal which can easily be
amplified.
This technique as described thus far suffers from interferences due
to broad band absorption of carbon dioxide, water vapor, and
hydrocarbons. When these interferents are present, the NDIR would
yield a higher concentration of CO than was actually present. If
the detector cells are arranged in series rather than in parallel,
the distention of the diaphragm is the result of the differential
absorption of CO in the front and rear chambers and these inter-
ferences are minimized. Calibration of NDIR instruments is
accomplished by simple dilution of concentrated cylinder gases.
Review:
Reference Methods vs Equivalent Methods
Criteria gaseous pollutants and Reference Methods for each.
L12-52b
L12-53
L12-54
L12-55
L12-56
L12-57
210
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sim no as n
INSERT EMULSION SIDE DOWN
REFERENCE
METHODS
one
specific
method
of analysis for a pollutant
MANUAL AUTOMATED AUTOMATED METHOD
Measurement Principle
MP
Calibration Procedure
POLLUTANTS AND
THBR MFBIBKX METHOD
fOUUIANl AKTHOO
SULFUR DIOXIDE (SO2) SULFUR DIOXIDE
Standards
Collection
HOOVV ^Vkll* t tr M jfro
Reaction
Spectrophotometry
f (i «oo»« ?vtrf/>im
SMCTHOPHOtOMITKY
REAaiON PHASE
-
|J *
^
SO3 TCM -COMPLEX
Ho»Contrd
P* »*« ^^^
tit i JUi "
IF* WO 4 7* «4
, MMK rf so, !«-»* Potauium
MOT*. M.^>J WrQ Q,!,,,,, M^cural.
Impingw(s)
Orifice(s)
K,HgCI4
WTERFERENTS
R«mov«d by treating
OZONE (03)
Current Standards
Oj Tim. dolay
MtAVY MtTAlS AddMKXi of ctaMng PKIMAKY SECONDARY
OKSCHVIO .
OXIOAN1S
Meosurement Principle
MOOVV ^*vtf i»]wrn ?o«o
^wkfV* l» irw* ?r**o
02ONC OENHATO*
uv nK>tOM£ny CAIIMAIION
*T«chnkd AMMonn DocunwO
OMMMenHw"
7rancf*rSKxtdard>torColitiralkin
of Amb*«nf Air Monitoring
Anolyl«rs for Ozone
< o^r^c w i f i A
211
-------
is'Rl «0 35 78
INSERT tMuiSlUN SIDE. DOWN
INTERFERENTS
O, REFERENCE METHOD
(Automated)
IKMUBMENT
( ntOCEDUM
NON-METHANE
HYDROCARBONS (NMHQ
M*atur*m*nt Principl*
PRIMARY SECONDARY f GASOOQMAtO
CALIBRATION
PROCEDURE
i Span or calibrof ion
gases
NOW UNtAK FID WSTONH
nb«r o* Cafbon Atomi
NITROGEN DIOXIDE NO,
PRIMAKY SBXINOAflY
r m *«4
MTERNATlVfA,
NO+Q,
G?T CALIWATION Sf IljP
P£RM£ATION SYSTtK
EPA-600/4-75-003
'Technical Assistance
Document for the
Chemiiuroinoscwtce
Meosurement of
Nitrogen Dioxide"
DETEOOR CEUS IN SERIES
212
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213
-------
LESSON PLAN
TOPIC: SURVEILLANCE NETWORKS
COURSE: 435 - Lesson #13
LESSON TIME: 45 min.
PREPARED BY: DATE: 2/15/79
Northrop Services, Inc.
LESSON GOAL:
LESSON OBJECTIVES:
SUPPORT MATERIAL
AND EQUIPMENT:
SPECIAL INSTRUCTIONS:
Familiarize the students with the status of ambient air
monitoring regulations pertaining to surveillance networks and
the requirements of such a network, including its major sub-
systems. This lecture overlaps the lecture that follows on
Site Selection.
The student will be able to:
Describe the need to specify the objectives of sampling tied
to intended use of the data as the first step in designing
the network.
Cite the major sources of EPA guidance on monitor siting.
Discuss the composition of SAMWG and the status of its
recommendations.
Defend the need for a quality assurance program.
Describe an ambient monitoring network including its major
subsystems.
Objective handout
Slide projector with tray
Students have been away from lecture for a day now, and
need to be returned to note taking. Keep lecture moving and
light, while watching feedback to insure attention. This
lecture also ties in with the next lecture on site selection.
Read that lesson plan before giving this lecture. Remember,
a week has been spent dealing with specific points. This
lecture summarizes rapidly and gives a loose framework capable
of being used with any size network.
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SELECTED REFERENCES: "Air Monitoring Strategy for State Implementation Plans"
EPA-450/2-77-010, June, 1977.
"Quality Assurance Handbook for Air Pollution Measurement
Systems", Vol. I - Principles, EPA-600/9-76-005, March 1976.
"Quality Assurance Handbook for Air Pollution Measurement
Systems", Vol. II - Ambient Air Specific Methods, EPA-600/
4-77-027a, May 1977.
Title 40 Code of Federal Regulations Part 58 (May 10, 1979).
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Course: 435 -; Lesson #13
Lecture Title:
55
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SURVEILLANCE NETWORKS
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INTRODUCTION
Before starting into network design, first some background
information about EPA efforts.
To critically review and evaluate current air monitoring
activities, the Standing Air Monitoring Work Group was formed
in October 1975. This group was composed of state and
local air pollution control agencies in conjunction with
regional and program offices of the EPA.
MAJOR FINDINGS
(1) Too few monitors in some locations, too many in others
(2) Data produced of unknown quality poor quality
assurance programs
(3) Lack of coordination of monitoring activities
(4) SIP network regulations too inflexible (for others see
pp. 2-3 of Air Monitoring Strategy for State
Implementation Plans, EPA 450/2-77-010)
To correct these, several steps were taken, most important of
which are:
(1)
A complete revision of nearly all of the ambient air
monitoring regulations with the intent to
(a) Improve data quality,
quality assurance ,
siting, and,
methodology
Improve the timely submittal of data
Improve the cost effectiveness of monitoring
(b)
(c)
(d)
Improve monitoring program's responsiveness to
data needs
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(2) This reorganization was promulgated in the Federal Registei
on May 10, 1979 and detailed the requirements for:
(a) A minimum quality assurance plan
(b) Network design and periodic reevaluation of
monitoring network
(c) Methodology
(d) Siting - instrument and probe
(e) Data reporting
The majority of these regulations, among others, are part of
40 CFR 58 with seven (7) appendixes.
216
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Formerly in
40 CFR 50
40 CFR 51
40 CFR 53
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CONTENT OUTLINE
Course: 435 - Lesson #13
Lecture Title: SURVEILLANCE NETWORKS
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I. Regulations
(Explain briefly Federal System of publishing regulations)
A. Code of Federal Regulationsyearly summary (July 1 -
June 30) of all Federal Regs, then supplemented with daily
Federal Register publications.
B. 3 types of monitoring stations are defined.
SLAMS - State and Local Air Monitoring Stations
(required for SIP networks)
NAMS - National Air Monitoring Stations (required
for SIP networks)
SPMS - Special Purpose Monitoring Stations (optional)
This regulatory reorganization now makes it easier to under-
stand and find EPA ambient monitoring regulations.
II. Network Design
A. Network can be divided (arbitrarily) into 2 major systems
Sensor System
Data System
B. PRELIMINARY PLANNING must be done first
1. First step should always be to define the purpose of the
program and the uses for the data.
a. Most important - emphasize need to carefully
accomplish this step.
b. Hopefully, if this design process is done care-
fully, we'll minimize expense while meeting program
needs. This step also is used in siting monitors
as will be discussed in the next lecture.
2. After identifying the purpose of the network, we can
assemble background materials on:
a. Meteorology
b. Topography
c. Source characteristics affecting area of interest
d. Legal and administrative concerns
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Throughout design
process, illus-
trate steps with
examples from
your own experience
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Ask students to
name some typical
ones (see siting
lecture for 12 S02
uses)
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Appendixes of SO-
siting manual
(EPA-450/3-77-013)
have some sources
of background
materials
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Course: 435 - Lesson #13
Lecture Title: SURVEILLANCE NETWORKS
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C. This background material will provide the basis for decisions
that must be made during the DESIGN PROCESS
1. SENSOR SYSTEM
Need to answer several questions
What to monitor
How to monitor.
Where to monitor
Maintenance and calibration needs
a. What to Monitor
(1) Determined from needs of program, could be:
legal standards
expected problems
PSD or background
(2) Need to specify what will be monitored and if
more than one specie involved
b. How to Monitor
(1) May be specified by regulations
(2) Often reference or equivalent methods - EPA
TSP - Hi-volume method
CO - Non-dispersive infrared
NMHC - GC with flame ionization detector
0- - Chemiluminescence with ethylene
N0? - Chemiluminescence with ozone
S02 - Pararosaniline
Lead - Hi-vol w/atomic absorption
(3) Other standard methods
ASTM, NIOSH, or others + literature Searches
c. Where to Monitor
(1) Will come in detail in the next lecture
(2) EPA has issued a reasonable amount of guidance
in this area, includes probe locations
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good time to re-
view reference
methods
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Lecture Title: SURVEILLANCE NETWORKS
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d.
Maintenance and calibration needs are difficult to
estimate include here manpower, equipment, parts,
etc.
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sources of information
Manufacturer's recommendations tend to be
optimistic
Other users
can obtain names from equipment
manufacturers or state agencies
In-house records or former experience
(a)
(b)
2.
(c)
This completes the sensor design and the first half of
the Network. Next deal with design of the Data System.
DATA SYSTEM
Composed of 2 subsystems:
recording and transmission
data handling
a. Recording and Transmission
(1) Recording
(a) handle' an electrical signal from an instrument
or record a reading from a manual analysis.
Must decide if need requires a machine readable
format for computer handling.
(b) Difficult to decide - process is dependent on
individual system - each unique.
(c) Roughly, if more than 1 man week/month is
required in data handling, may be more cost
effective to use some automated processing.
(d) Can s'eek help from computer system engineers
(2) Transmission
(a) How fast do you need data don't overemphasize
and use telemetry if data is for a quarterly
report.
(b) Automated data loggers coupled with telemetered
lines take time to debug -- include this in
network cost.
(c) Make as simple, cheap and uncomplicated as
possible.
(d) Eventually move data to a central processing
or handling facility.
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"rule of thumb"
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Lecture Title: SURVEILLANCE NETWORKS
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b. Data Handling
Having recorded data and transmitted it to a central
unit, can now design data handling subsystem involves
formating, validating, analyzing, storing and retrieving
data.
(1) Format - basically just a systematic listing
(a) should be:
clean and understandable
well documented
suitable for interchange
available
(b) Might consider SAROAD Format - developed by EPA
for use with the National Air Data Bank. A
convenient format suitable for use to EPA and
states has already been de-bugged.
(c) Need to consider if different data users (i.e.
EPA, internal, etc.) can use same format
(2) Validation - should be performed by an Air Pollution
professional with intimate knowledge of the sensor
and data systems, as well as any peculiarities of the
air pollution problem in the area. The validator
should be:
officially designated
check abnormal values and rapid changes
make corrections where possible
(This function is extremely important and reflects
the major deficiency noted by SAMWG.)
For guidance on this and other areas of quality
assurance see:
"Quality Assurance Handbook for Air
Pollution Measurement Systems" Volumes I and II.
Vol. I. EPA-600/9-76-005
Vol. II. EPA-600/4-77-027a
Both are valuable aids in designing an effective
quality assurance program.
(3) Analysis - possibly consult a professional
statistician familiar with Air Pollution data; use
of data will probably dictate appropriate statistics
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SAROAD - storage
and retrieval of
aerometric data
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Log - normal distributions'for long-term trends,
various types of means, not complete consensus
among "experts", can consult EPA.
Monitoring and Data Analysis Division (MDAD)
US EPA/MD-14
Research Triangle Park, N.C. 27711
(4) Storage
(a) secure - possible legal requirement
(b) systematic - easily comparable year to year
(c) protective - prevent physical deterioration
thermally sensitive
magnetic or electric interference
(d) accessible - to proper personnel
(5) Retrieval
(a) easily located
(b) secure
(6) Reporting '
(a) State Implementation Plan (SIP) monitoring
networks are required to report data collected
before January 1, 1981 from all stations on
a quarterly basis to EPA.
(b) For data collected after January 1, 1981:
(1) NAMS data must be submitted quarterly
(2) A SLAMS data summary report must be
submitted annually
Have covered design of Data System
Combine Sensor and Data System for total Network
Summarize material
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Time spent on sum-
mary is dependent
on class attention.
Use instructor
discretion.
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LESSON PLAN
TOPIC: SITE SELECTION
COURSE: 435 - Lesson #14
LESSON TIMERS Min.
PREPARED BY: Northrop DATE:2/22/79
Services, Inc.
LESSON GOAL:
Familiarize students with location of EPA siting regulations
and guidance. Briefly outline procedure used in EPA siting
documents and discuss its utility, and to give a basic
understanding of some of the important factors involved in
correctly siting ambient air quality monitors.
LESSON OBJECTIVES:
The student will be able to:
Discuss the need to properly site pollutant monitors
Locate the documents for guidance on siting pollutant
monitors
Outline the procedure used to site monitors as described in
the guidance documents.
Locate regulations associated with monitor siting
Recognize factors involved in selecting proper siting of
monitors.
SUPPORT MATERIAL AND EQUIPMENT:
1. Handout of p.31 of SO siting manual
2. Objective handout
3. Slide projector w/tray
4. EPA-450/3-77-013 "Optimum Site Exposure Criteria
For S0~ Monitoring"
SPECIAL INSTRUCTIONS:
This lecture is presented near the end of the course - students'
attention span and motivation are typically reduced (concerned
about Final, returning to work, etc.) Attempt to be light and
watch feedback from students to maintain attention. Material
is important!!
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SELECTED REFERENCES:
"Selecting Sites for Carbon Monoxide Monitoring", EPA-450/3-75-077,
Sept. 1975.
"Optimum Site Exposure Criteria for SO- Monitoring", EPA-450/3-77-013,
April, 1977.
"Selecting Sites for Monitoring Total Suspended Particulates",
EPA-450/3-77-018, June 1977.
"Site Selection for the Monitoring of Photochemical Air Pollutants"
EPA-450/3-78-013, April 1978.
"Guidance for Air Quality Monitoring Network Design and Instrument Siting
(revised)", OAQPS 1.2-012, Sept 1975.
' ' -, 3
40CFR58 Appendixes D and E
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CONTENT OUTLINE
I1
55
Course 435 Lesson #14
Lecture Title: SITE SELECTION
1
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Page 1 / 6_
NOTES
INTRODUCTION: Review of available siting guidance
OAQPS 1.2-012 "Guidance for Air Quality Monitoring
Network Design and Instrument Siting" (Revised
Sept. 1975.)
OAQPS (Office of Air Quality Planning and Standards) is responsible
for setting standards and methods among other thingsthey have pub-
lished a series of guideline documents in these areas... The above
is most current.
Material is somewhat outdated, superseded by the individual siting
documents, 1.2-012 has 2 appendixes, CO Siting and Monitoring around
Large Point Sources. Both are also of limited utility. 1.2-012 is
mentioned mainly to avoid future confusion if someone should locate
it later. It does contain some useful information, yet you must
be careful in using it.
Next, the 4 Siting Documents. . .
"Selecting Sites for Carbon Monoxide Monitoring"
EPA-450/3-75-077, Sept. 1975.
"Optimum Site Exposure Criteria for S02 Monitoring"
EPA-450/3-77-013, April 1977.
"Selecting Sites for Monitoring Total Suspended Particulates"
EPA-450/3-77-018, June 1977.
"Site Selection for the Monitoring of Photochemical Air
Pollutants", EPA-450/3-78-013, April 1978.
These were done under contract to EPA and all 4 utilize the same
approach.
This approach basically is as follows:
1. Define purpose of site or need for data
2. Assemble background information and site selection aids
3. Define the general siting area accounting for chemical
and meteorological individualities
4. Establish the final site characteristics including probe
height and location
The guidance contained in these documents is consistent with the
regulations for ambient air monitoring contained in 40CFR58 plus
its appendixes.
TITLE SLIDE
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Course: 435 - Lesson #14
Lecture Title: SITE SELECTION
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Course: 435 - Lesson #14
Lecture Title: SITE SELECTION
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9. Supporting enforcement actions.
10. Documenting episodes and initiating episode controls.
11. Documenting population exposure and health research.
12. Providing information to:
(a) public - air pollution indices; and
(b) city/regional planners, air quality policy/decision
makers - for activities related to programs such as
air quality maintenance planning (AQMP), prevention
of significant deterioration (PSD) and the prepara-
tion of environmental impact statements.
These are rather broad but should start the process, now on to
"Locating general - level Regional Scale Stations" for SO
measurements.
S02 monitoring sites may be either:
groximate - oriented toward measuring concentrations resulting
from specific source or group of sources.
General - Measurement of total concentrations where contri-
butions from individual sources are either not required to be
known or do not predominate.
Other concept in title is of spatial scale. Concept is- applicable
to all pollutants. Is useful in describing and defining sites.
Spatial Distances are approximate (4\LO%). Scales are as follows:
Microscale. Ambient air volumes with dimensions ranging from
meters up to about 100 meters are associated with this scale.
Middle Scale. This scale represents dimensions of the order
from about 100 meters to 0.5 kilometers and characterizes areas
up to several city blocks in size.
Neighborhood Scale. Neighborhood-scale measurements would
characterize conditions over areas with dimensions in the 0.5
to 4.0 kilometer range.
Urban Scale. Urban-scale measurements would be made to repre-
sent condi tions over areas with dimensions on the order of 4
to 50 kilometers.
Regional Scale. Conditions over areas with dimensions of as
much as hundreds of kilometers would be represented by regional-
scale measurements. These measurements would be applicable
mainly to large homogeneous areas, particularly those which are
sparsely populated.
228
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Lecture Title: SITE SELECTION
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National and Global Scales. These measurement scales represent
concentrations characterizing the nation and the globe as a
whole.
For this example, we are using regional scale.
So 1st, determine purpose of site
either A. Assess S0? transport
or B. Determine Regional Mean concentration
II. Assemble Site Selection Aids - (Addresses for providers of aids
in back of SCL siting manual-Appendix
A & D)
1. Climatological Data
(a) Assess representativeness for site or area
(b) Choose season for stability and wind rose data if possible
(1) Winter versus summer
Peak energy demand tied to maximum
S02 production
(2) Different Meteorological Features
prevailing winds
frequency of inversions
heights of inversions
2. Maps
(a) U.S. Geological Survey
(b) Sanborn
(c) Aerial
(d) Satellite
3. Population Data
(a) Census Bureau
(b) Local planners
4. Diffusion Model Output
Optional, yet desirable (See Appendix E of S02 Manual)
STEP 3 OF PROCESS
III. Defining general siting area
Work with left side of flow chart first.
Assess S02 transport
Interstate - Urban area
Interstate - General
Intercity
Interstate-Urban Area - defines state line and two areas of
interest
229
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CONTENT OUTLINE r e%
Course.-435 - Lesson #14
Lecture Title: SITE SELECTION
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NOTES
Since looking at transport into state, don't want emission from own
city interfering - so eliminate sites within interference distance
either by removing source (attempt at humor) or modeling.
Interference distances are determined by modeling worst case
conditions using a Gaussian model. They differ depending on the
scale. For regional scale, they are:
Eliminate Prospective Specific Sites Within:
30 km of large point sources, e.g., 400 MW power plant.
15 km of medium-sized town, population 25,000
10 km of large industrial source, emissions 500 T/yr.
0.6 km of individual home (103 gal/yr of #2 oil).
Now add appropriate interference distance and wind rose. Wind rose
is a statistical representation of wind data. Most commonly, the
longer the bar off of the circle, the more frequently winds blow
from that direction
1. Primary Site
Site is as close as possible to state line if looking for
maximum impact-not most frequent impact.
2. Secondary Site
Downwind, just across state line
3. Additional Sites
If blessed with many monitors, ideally would cover all of
state line (as with S02 bubblers perhaps)
Interstate-General
Similar reasoning, along state line. Note interference
distance and winter wind rose- (Winter, if applicable)
Intercity
1. Define area
2. Interference distance + wind rose
3. Primary site - located in area from prevailing wind
direction
4. Secondary site - 2nd prevailing wind direction
Before discussing individual site characteristics or probe location,
finish right side of flowchart.
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Slide indicates
aumorous approach
to removing source
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Ask students to
locate
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Course: 435 - Lesson #14
Lecture Title: SITE SELECTION
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Regional Mean Concentration
1. Define area - mixture of sources
2. Add appropriate interference distances
3. Appropriate wind rose
4. Diffusion Model Output
ensure your concentration gradient is
not too steep
5. Locate site - upper left of figure (see figure 4-3,
p. 34 of S02 siting manual)
STEP 4 OF SITING PROCESS
IV. Establish final site(s)
Having located areas of possible siting, a few final considerations
1. stationary or mobile
2. availability
3. security
4. cost
5. topography
avoid low lying areas
uniform topography - all flat or all hills, etc.
6. probe location - different for each pollutant
but generally between 3-15m. above ground. Probe
constructed of non-reactive material.
7. Others
Summarize and emphasize that these are the simplest examples from
the S02 Manual, and that the siting documents are useful. This
example was covered to illustrate the approach to give an idea of
what to expect, Manual covers many other more complex siting
problems.
This siting approach is not necessarily "the" siting approach, yet
has several good points:
1. It is the EPA approach
2. It is a logical, systematic approach that
allows a logical selection of a monitoring
site and provides for suitably documenting your
choice.
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/ t ^Hlk- Of St«l
ESTABUSI fWAL SITE CHARACTaUSTKS
MMKISAKI OK *I)UU: '
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LESSON PLAN
TOPIC: ASSURING HIGH QUALITY DATA
COURSE; 435 - Lesson #15
LESSON TIME: 30 Min.
PREPARED BY: Northrop DATE: 2/15/79
Services, Inc.
LESSON GOAL:
Identify general characteristics of Quality Assurance as they
apply to atmospheric sampling and analysis and develop an
appreciation for Quality Assurance.
LESSON OBJECTIVES:
The student should be able to :
1. Define Quality Assurance.
2. State three major reasons why a quality assurance program
is important in sampling and analyzing atmospheric
pollutants.
3. Recognize that many different quality assurance elements
are involved in the process of producing valid data, list
several of those which are directly applicable
to the individual who samples and analyzes atmospheric
pollutants.
4. Recognize that QA principles and specified QA methodologies
are located in Vols. I & II of the Quality Assurance
Handbook and 40CFR58 Appendixes A and B.
5. Recall that EPA conducts an Interlaboratory Performance
Audit Survey arid that participation (voluntary at present)
will be required by 1983 in accordance with SLAMS provisions.
SUPPORT MATERIALS AND EQUIPMENT:
35 mm slide projector - required
Overhead projector or blackboard not required, but convenient
to have available.
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SPECIAL INSTRUCTIONS: This lecture should be covered quickly with
emphasis on the sources of information for
quality assurance. Try to get students to
see the need for quality assurance.
SELECTED REFERENCES:
Quality Assurance Handbook, Vol. I, EPA-600/9-76-005
Vol II, EPA-600/4-77-072a
Published by EPA, Quality Assurance Branch, MD-77, Research
Triangle Park, N.C. 27711
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Course: 435 _ Lesson #15
Lecture Title: ASSURING HIGH QUALITY DATA
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NOTES
I. INTRODUCTION
A. Objectives
B. Quality Control vs. Quality Assurance
Quality Control - system of activities to provide you
with a quality product.
Quality Assurance - system of activities that assures that
the quality control system is performing
adequately.
Quality Assurance can be called "quality control on
quality control."
II. QUALITY ASSURANCE
Class Question: What is the principal product of an air
pollution measurement system? DATA
Class Question: What is the principal product of a QA
program? valid data.
No data is better than incorrect data
Class Question: Why is a quality assurance program important?
It is cost effective; in the long run, the cost per bit
of valid data is less expensive.
Minimize bad data
It adds credibility to data
It supports legal cases: Data supported by quality
assurance is virtually unassailable in a court of law.
Environmental lawyers have learned how to attack data
validity, and validation of data thru a QA program is
very difficult to discredit.
III. QUALITY ASSURANCE WHEEL
Organization
Responsibility of several people (approximate percent
responsibility)
Refer students to
objectives handout
read objectives to
students
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Lecture Title: ASSURING HIGH QUALITY DATA
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23 elements involved in QA Program
Consider only certain elements in this course
data validation
audit procedures
preventive maintenance
sample collection
sample analysis
data reporting
calibration
IV. REFERENCES
Quality Assurance Handbook
Vol. I: Principles
Vol. II: Ambient Air Specific Methods
Vol. III. Source Emissions Specific Methods
Available free-of-charge from
Environmental Monitoring Systems Laboratory
MD-77
Environmental Protection Agency
Research Triangle Park, N.C. 27711
(Also should mention 40CFR58 Appendixes A and B (May 9, 1979)
V. The Measurement Process
3 basic components
(1) Separation of pollutant from the air matrix in which it
is mixed.
Physical or chemical separation
ex. SO - collect in TCM
ex. CO - instrumental method only "sees" CO, so it
is "separated" from the rest of the air matrix
(2) Determine pollutant quantity and air matri-x volume
(3) Calculate concentration by dividing pollutant quantity by
air volume.
Calibration is the process of establishing the relationship
between the output of a measurement process, or portion
thereof, and a known input.
THE SINGLE, MOST IMPORTANT STEP IN THE MEASUREMENT PROCESS IS
CALIBRATION.
237
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Course:435 - Lesson #15
Lecture Title: ASSURING HIGH QUALITY DATA
NOTES
Six Elements of a Calibration Program
(1) Statements of allowable time between calibrations
usually maximum time allowable
(2) Statements of minimum quality of calibration standards
ex. Chemicals - ACS reagent grade (minimum)
(3) Statements of proper environmental conditions
ex. Hi Vol filters - equilibrated at 50% RH
SC- samples stored prior to analysis at
less than 5°C.Electrical power: controlled?
regulators needed?
(4) Provisions for written procedures
Make calibrations, analyses, etc. less operator
dependent
(5) Provisions for standards traceability
all calibration standards should be traceable
to standards of higher accuracy NBS-SRM's
preferred.
(6) Provisions for proper record-keeping
station log books
laboratory note-books
"chain of custody"
VI. THE AUDIT PROCESS
Intralaboratory audits
"within your own laboratory"
Interlaboratory audits
"between laboratories"
collaborative testing
EPA Performance Audit Program
Semi-annual audit program
Free to participants
Schedules published in:
JAPCA
Quality Assurance Newsletter
Stack Sampling News
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_ Lesson #15
Lecture Title: ASSURING HIGH QUALITY DATA
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NOTES
To find out more about program, contact:
Your Regional Quality Assurance Coordinator
OR
Write: Director, EMSL
US EPA, MD-77
Quality Assurance Division
Research Triangle Park, NC 27711
Students who are interested in a more in-depth coverage of
Quality Assurance as it deals with air monitoring are
recommended to take APTI course. . .
#470 Quality Assurance for Air
Pollution Measurement Systems
L15-16
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COURSE 435 - ATMOSPHERIC SAMPLING
LABORATORY INSTRUCTIONS
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LABORATORY INSTRUCTIONS
I. Lab Facilities should ideally have 3 separate rooms (can go with 2 rooms
or one large room)
total of 10 people in each lab at one time
Lab 1: Hi Vol Lab 25 feet of standard lab bench top space
2 to 4 electrical outlets
extremely noisy lab ideally should have its
own room.
Lab 2: Flow Lab 30 feet of standard lab bench top space 4 to 6
electrical outlets
tap water supply is nice.
Lab 3: Test Atm. 25 feet of standard lab bench top space
6 to 8 electrical outlets
Lab exhaust hood is best (can possibly do without)
Total of 80 feet of standard lab bench top space.
II. Laboratory Materials and Equipment
The following list indicates the equipment and materials required for
successful presentations of the lab sessions using the procedures contained
in the Course 435 Laboratory Manual.
Equipment List - Lab #435 Atmospheric Sampling
(A) LAB 1 - CALIBRATION OF A HIGH VOLUME SAMPLER
1. Portable "in the field" calibration kit (optional)
2. 2 - Pressure transducers (Dixon meters) and Hi-vol blowers.
3. 2 - Visifloat and Hi-vol blowers (used with rootsmeters)
4. 2 - Rootsmeters with stands
5. 4 - Water manometers - capable of measuring 16 inches or more.
6. 2 - Mercury manometers - capable of measuring 160 mm xjr more.
7. 4 - Ring stands and 10-3 prong holder clamps
8. 2 - Sierra or other make constant flow controller units
9. (and calibrator to correspond _to constant flow unit)
10. One cartridge "type" filter holder (optional)
11. 2 - Orifice units (calibrator with load plates)
12. 4 - Electrical outlet - multiplugs - (extension cords okay)
13. 2 - Reference flow devices (Ref) (Dexco, Inc.)
14. Tubing - thin walled - Tygon
15. Miscellaneous - (A) rubber gaskets
(B) one box of clean filters (glass fiber)
(C) oil - (rootsmeter grade oil)
(D) Mercury
(E) Distilled water with added coloring - ten drops/liter HJD
e.g. fluorescein green dye
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(B) LAB 2 - FLOW MEASURING INSTRUMENTATION
1. 2 - Mass flowmeters (0-3 liter range)
2. 2 - Displacement bottles (10 liter capacity)
3. 2 - Two liter class "A" volumetric flasks
4. 2 - Wet test meters (1 liter/rev)
5. 2 - Stopwatches
6. 2 - vacuum pumps (capable of pulling 25" Hg vacuum)
7. 4 - Smog bubblers
8. 8 - Gas metering valves
9. 6 - Vacuum gauges (0-30 "Hg vacuum range)
10. 4 - 500 ml Erlenmeyer flasks (plastic)
11. 2 - Particulate filters and holders (Teflon filters)
12. 2 - Moving soap bubble meters (graduated 0-500 ml)
13. 500 ml soapbubble solution
14. 2 - 250 ml beakers
15. 10- Metal squeeze clamps for glass sockets
16. 4 - One-holed stoppers (rubber)
17. 2 - 2-holed stoppers (rubber)
18. 2 - 500 ml washbottles
19. 10 - ring stands
20. 4 - Mounting rods (horizontal)
21. 28 - 3-prong clamps
22. 2 - rotameters (glass) (0«^3£ range)
23. 2-23 gauge hypodermic needles
24. 36 - clamp holders with 45° angle thumbscrews
25. 40' - 50' of vacuum tubing (rubber)
26. 6' - thin walled tubing (rubber)
(C) . LAB 3 - STANDARD TEST ATMOSPHERES EQUIPMENT REQUIRED*
1. Continuous S0« Analyzer - (e.g. Teco Model 43)
2. Continuous NO - N02 - NO Analyzer (e.g. Bendix 8102)
3. Portable Dilution system (e.g. Bendix Model 8861D)
4. Portable permeation system (e.g. Bendix Model)
5. Misc. (a) hardware Swagelok fittings - clamps
(b) tubing (e.g. Teflon and/or glass )
(c) mixing bulbs - (glass) and/or glass manifold
(d) support gases needed
(1) zero air
(2) NO bottled gas (50 ppm)
(e) permeation tube 1 yg/min SO,, @ calibrator/permeation
oven temperature
*May substitute other equipment so long as the principles put forth in the
lab write-up are demonstrated i.e., permeation/dilution system utilized to
calibrate monitor and gases and their dilution as an alternate calibration
method.
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III. SPECIAL INSTRUCTIONS
Lab 1: Hi Vol Lab
a. Divide groups in half during their first lab session. They will remain
in these groups throughout the 3 labs.
b. Each group of about four will first calibrate an orifice vs. a rootsmeter.
Go over with them first the proper principle/operation of a rootmeter.
Show them oil level indications - 3 of them.
Explain why the mercury manometer is used and give a demonstration
of the pressure drop.
Show the volume indicator and explain why we use the non-compensated
dial because gas companies usually utilize the meter and they use
60?F as their standard temperature.
Explain how to read a mercury vs. a water manometer.
<* Mercury the top of the meniscus vs. the bottom for a water manometer.
- due to the properties of these two liquids.
If there is a mercury barometer available explain how to read it.
Take a temperature reading as well, ideally the temperature should be
the temperature in the room.
Rootsmeters should be warmed up prior to calibration procedures.
See Lab Manual.
c. After the orifice unit is calibrated vs. a rootsmeter have the groups now
calibrate a visifloat and/or a transducer (ideally both) vs. the orifice.
Explain how to read a rotameter - center of ball and and how to set up
and read a pressure transducer. (Should zero them first - and remember to
tap them before you take a reading). See instruction manual.
d. Next exercise consists of checking the orifice curve with a ReF flow audit
device. Follow instructions and explain to students why this unit
is more accurate. (1) more highly precisioned (i.e. plates) (2) placed on
top of the sampler head vs. screwed on top of blower motor. Remember to
perform a leak check with the plate without any hole. (This might be
a plate with one hole and should be closed with enclosed screw and wing
nut). K values are given with each unit. (received from EPA).
e. Last exercise consists of checking the constant flow control unit.
Follow directions and explain to students how flow is critical in the
method as well as going over the principle of operation, i.e., flow
sensing anemometer.
2A3
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f. Explain all calculations that are to be used in this lab.
Lab 2: Flow Lab
(a) Groups should be in their respective subgroups.
(b) Set-up as diagramed in lab exercise manual.
(c) Best to use two complete set-ups of each exercise on
adjoining benches. This allows one group to start from
one end of one bench and the other group the opposite end of
the adjoining bench, (facilitates space allocation).
(d) Be sure the students have read over the instructions.
(e) Describe the procedural steps utilizing the set-ups themselves.
(f) Go over the lab data reporting requirements with each group.
(i.e., which data sheets should be turned in for grading)
(g) Demonstrate proper reading of lab barometer (mercury barometer)
(h) While the lab is proceeding, go over with them the principles
of operation/theory of a mass flow meter , wet-test meter,
rotameter, moving bubble meters, and a limiting orifice.
(i) After data is collected, the students may re-enter the classroom
to perform calculations and construct appropriate curves.
(j) Instructor should be present to assist with the calculations.
Lab 3: Test Atmospheres
(a) Instructor should thoroughly review operating manuals for the
ambient air monitors and permeation systems used.
(b) Instruments should be check-out and running 48 hours before lab
commences.
(c) Plumbing considerations include use of only Teflon/and or glass
for pollutant gases. This should include both lines and fittings.
(d) Be sure students have read over instructions prior to lab. After
this, instructor can demonstrate with the instruments the procedures
themselves.
(e) See Lab 2 (f)(i)(j)
(f) While the lab is proceeding the students could benefit by added
instruction concerning these items: principle/operation of instruments,
handling of specialty gases and cylinders, permeation device
operation and calculations involved.
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Assemble Site Selection Aids:
CUmatological Wind Data
Maps (various scales) showing
- topography
- developed areas
Population Data by Town
Diffusion Model Ouput (Optional)
Is Purpose of Site to Ass'ess $03
Transport or Measure Regional Mean
Concentrations?
Interstate, general
Tentative primary site located
as near as possible to state
line on out-of-state urban
area side, as close to urban
area as possible, but no closer
to an in-state urban area than
30 km. Additional sites lo-
cated directly downwind of ur-
ban area in prevailing winter
or annual wind direction, or '
symmetrically about the pri-
mary/secondary siting areas
(see text).
Tentative Siting
area located as
near as possible
to state line.
If only one site
Is considered,
then locate on
winter windward
side; I.e., state
line toward maxi-
mum winter wind
frequency
Eliminate Prospective Specific Sites Within:
30 km of large point sources, e.g., 400 MW power plant.
15 km of medium-sized town, population 25,000.
10 km of large industrial source, emissions 500 T/yr.
0.6 km of Individual home (103 gal/yr of 12 oil).
Avoid low lying areas. (see Table 4-2)
Intercity
Single Site: Tentative
siting area located not
less than 30 km from
large urban area upwind
1n most frequent winter
wind direction (also,
see Table 4-2). Addi-
tional sites ray be lo-
cated same distances
upwind in the next most
frequent winter wind
direction
Tentative siting area located not
less than 30 km from nearest urban
area. Urban area should be toward
direction of the lowest winter
wind direction frequency and in an
area characterized by flat concen-
tration gradient, as revealed by
diffusion model output, and in an
area of uniform topography
SUe Characteristics: Trailer or
existing permanent structure.
Inlet Height: 3-10 m above ground.
Flow chart showing procedures for locating
general-level regional-scale stations.
Siting Handout
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
'. REPORT NO.
EPA 45Q/2-8Q-OQ6
2.
3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
APTI Course 435
Atmospheric Sampling
Instructor's Guide
5. REPORT DATE
February. 1980
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
M. L. Wilson, D. F. Elias, R. C. Jordan
K. C. Joerger, B. M. Ray, J. C. Henry
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Northrop Services, Inc.
P. 0. Box 12313
Research Triangle Park, NC 27709
10. PROGRAM ELEMENT NO.
BA8A2C
11. CONTRACT/GRANT NO.
68-02-2374
12. SPONSORING AGENCY NAME AND ADDRESS
U. S. Environmental Protection Agency
Manpower and Technical Information Branch
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
TriRfriirtTir ' a
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The Instructor's Guide for Air Pollution Training Institute Course 435
"Atmospheric Sampling" contains guidelines for conducting a four and one-half
day course in ambient sampling. The Guide contains lesson plans, laboratory
instructions, exams, and solutions to problem sets. The lesson plans include
keys to APTI audio visual materials and suggested instructional techniques.
These materials are intended for use in conjunction with Student Manual
EPA 450/2-80-004 and Student Laboratory and Exercise Manual EPA 450/2-80-005.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Sampling
Measurement
Air Pollution
Gas sampling
Air Pollution Monitoring
Samplers
Collecting
methods
Instruments
Ambient Air
Air Pollution
Calibration
Instruction
Teaching
13 B
SRIM 44 P
3. DISTRIBUTION STATEMENT
19. SECURITY CLASS (ThisReport)
Unclassified
21. NO. OF PAGES
Unlimited
20. SECURITY CLASS (Thispage)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
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