Task Analysis of State and
Local Air Pollution Control Agencies and
Development of Staffing Guidelines
VOLUME
Detailed Task Data,and
Staff Guidance
LABORATORY
SUPPORT
UN I TED STATES
ENVIRONMENTAL PROTECTION AGENCY
Manpower Development Staff Office of Air Programs
Research Triangle Park, North Carolina 27711
-------
United States
Environmental Protection Agency
Contract No. 68-02-0306
Applied Science
Associates, Inc.
Task Analysis of State and
Local Air Pollution Control Agencies and
Development of Staffing Guidelines
VOLUME
Detailed Task Data,
Staffing Guidance
LABORATORY SUPPORT
K. I. Rifkin, Senior Staff Scientist, ASA
R. L. Dueker, Staff Scientist, ASA
W. F. Diggins, Staff Scientist, ASA
F. C. Foss, Staff Scientist, ASA
and
Michael Senew, Project Officer, USEPA
Prepared for the
United States Environmental Protection Agency
Manpower Development Staff
Office of Air Programs
Research Triangle Park, North Carolina 27711
November 1972
-------
This ts not an official policy and standards
document. The opinions, findings, and conclusions
are those of the authors and not necessarily those
of the United States 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.
-------
INTRODUCTION
One of the pressing problems in the air pollution control effort at
Federal, state, and local levels is planning manpower requirements and
developing manpower resources. Questions are being asked such as, how
many people are needed, what kind of past experience and education should
they have, how should their jobs be structured, what do they need to know
to do their jobs, what special abilities do they need, and what kind of
training should they receive to do their jobs? These questions are
becoming increasingly meaningful as the control effort broadens with the
creation of more and more local agencies and as existing agencies in-
crease the scope and depth of their programs. Adequate answers are
required if progress is to continue toward the goal of clean air.
In order to begin to answer questions relevant to manpower planning
and development, a data base describing the tasks to be performed by
control agency personnel and the skills and knowledge they must have to
perform those tasks effectively must be available. Guidance concerning
the use of the data base in making staffing decisions must be prepared.
It is the purpose of this study to provide such a data base and the
appropriate guidance.
A. Obj ectives
The objectives of this project were the following:
1. To identify as great a proportion as possible of the
population of tasks currently being performed by air
pollution dontrol agency personnel at the state and
local level throughout the country.
2. To describe the identified tasks in terms of component
behaviors and the skills and knowledge required to perform
those behaviors.
3. To identify and describe categories of air pollution con-
trol agency personnel who would perform the tasks mentioned
above.
continued
-------
4. To structure and communicate the data which resulted
from achieving the above objectives in a form which could
be used by agency management in planning and developing
manpower resources.
B. General Project Overview
The project was performed in two phases. Phase I dealt with achieving
the first two project objectives, and resulted in the development of a
detailed data base describing the major tasks performed by agency personnel
in terms of the procedural components of the tasks and the skills and
knowledge required to perform them. Phase II dealt with achieving the
last two major objectives, and resulted in production of a guidance docu-
ment which integrates and structures data developed in Phase I and presents
it in a form designed to assist agency manpower developers.
-------
THIS IS VOLUME D
Additional books available are:
VOLUME A: Guidance and Supporting Information for Staffing and Training
Decisions in an Air Pollution Control Agency - Introduction
and Directions for Using These Guidelines
VOLUME B: Guidance and Supporting Information for Staffing and Training
Decisions in an Air Pollution Control Agency - Engineering
VOLUME C: Guidance and Supporting Information for Staffing and Training
Decisions in an Air Pollution Control Agency - Field Enforcement
VOLUME E: Guidance and Supporting Information for Staffing and Training
Decisions in an Air Pollution Control Agency - Air Monitoring
and Meteorological Support
VOLUME F: Guidance and Supporting Information for Staffing and Training
Decisions in an Air Pollution Control Agency - Source Testing
VOLUME G: Guidance and Supporting Information for Staffing and Training
Decisions in an Air Pollution Control Agency - Agency Management,
Program Development, and Public Information Support
AND
TECHNICAL REPORT:
Task Analysis of State and Local
Air Pollution Control Agencies, and
Development
of Staffing Guidelines
For complete sets, or individual titles, or the Technical
Report please address your request to:
United States Environmental Protection Agency
Manpower Development Staff
Research Triangle Park, N. C. 27711
-------
LABORATORY SUPPORT
The task data and staffing guidance presented in this volume
cover a group of tasks which are generally performed by a chemical
analysis laboratory in support of the agency's air monitoring and
source testing efforts. The tasks include standard chemical analyses,
equipment maintenance, supervision, and development of new methods.
The operations are performed by Chemists, Chemical Laboratory Technicians,
and Equipment Technicians.
The following tasks are included and are located within the
t
volume as indicated below:
1. Determination of Nitrogen Dioxide and
Nitric Oxide Concentrations in the Atmo-
sphere Using the Saltzman Method Page D-4
2. Determination of Sulfur Dioxide Concen-
tration in the Atmosphere Using the
West-Gaeke Method page D-9
3. Determination of Sulfur Dioxide and
Sulfur Trioxide Concentrations in
Stack Gases Page D-14
4. Determination of Suspended Particulate
Concentration in the Atmosphere by
Means of High Volume Sampling Page D-18
5. Determination o,f Hydrogen Sulfide
Concentration in the Atmosphere
Using the Methylene Blue Method Page D-21
6. Determination of Nitrate Concentration
J -i Suspended Atmospheric Particulates
Using the 2, 4 Xylenol Method Page D-27
D-2
-------
7. Determination of Sulfate Concentration
in Suspended Atmospheric Farticulates
Using the Turbidlmetric Barium Sulfate
Method Page D-32
8. Determination of Metal Concentration
in Suspended Atmospheric Farticulates
by Means of High Volume Sampling Page D-37
9. Determination of Particulate Concen-
tration in Stack Emissions Page D-42
10. Identification of the Constituents
of Dust Particles Page D-47
11. Maintenance of Laboratory Devices Page D-52
12. Supervision of Laboratory Support
Tasks Page D-56
13. Development of New Methods for the
Analysis of Air Pollutants Page D-65
D-3
-------
Determination of Nitrogen Dioxide and
Nitric Oxide Concentrations in the Atmosphere
Using the Saltzman Method
Task- Overview
The Saltzman Method for determining concentrations of nitrogen dioxide
and .nitric oxide is routinely performed in several agencies. It varies
somewhat from the reference method contained in the Federal Register
(Reference 1). However, the difference lies in the particular reagents
used. The underlying principle is tne same.
The Saltzman Method is a colorimetric method. As a result, the procedure
is very similar to that of the West-Gaeke'Method for determining the
concentration of sulfur dioxide and consists of the following outline of
steps:
1. Preparation of the chemical reagents required for performance
of the task (including putting the absorbing reagent in the
fritted bubbler in preparation for sampling).
2. Analysis of the sample.
3. Calculation of the sulfur dioxide concentration.
The assembly and operation of the apparatus used for collecting the
sample will be considered within Air Monitoring (see Volume E).
Occupational Category; Chemical Laboratory Technician
Task Description
The procedure for this method of determining nitrogen dioxide and
nitric oxide concentrations is presented in usable form in Reference
3. An abbreviated procedure also appears in Reference 2. Where
grab sample bottles are to be employed in sampling the preparation
of the bottles is considered part of this task.
D-4
-------
Skill Requirements
1. The ability to prepare reagents and handle caustic or otherwise
dangerous chemicals without splattering acid, precipitating an
explosion, or otherwise injuring personnel or damaging equipment,
2. Ability to accurately obtain definite volumes of solutions
using apparatus such as a pipette, syringe, volumetric flask,
or burette.
3. Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability to:
a. Zero the balance.
b. Adjust sensitivity range without extreme changes which
might damage the balance.
c. Read and interpret the indicated mass.
4. Ability to assemble sampling apparatus with each component in
proper sequence using butt-to-butt connections, tygon tubing,
and silicone or florocarbon grease as appropriate to create
a leak-proof assembly.
5. Ability to operate a colorimeter or spectrophotometer in
order to obtain absorbance readings of sample and standard
solutions. This includes the ability to correctly input sample
to the instrument and recognize signs of instrument malfunction.
6. Ability to quickly and correctly solve an .algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given the
sample absorbance reading and the calibration curve.
b. Converting the volume of gas sampled to the volume at
standard temperature and pressure using the perfect gas
equation.
D-5
-------
7. Ability to prepare a calibration curve and compute the slope
of the best fitting straignt line, following a detailed step-
by-step procedure. This may require the use of regression
analysis by the least squares method.
8. Ability to read and interpret data from a table, psychometric
chart, or a nomograph.
9. Ability to distill water so that it is deionized and nitrate-
free.
10. Ability to measure the porosity of the fritted bubbler.
11. Ability to evacuate grab-sample bottles using a vacuum pump,
t
manometer, and a three-way stopcock connection.
Knowledge Requirements
1. Knowledge of general chemical nomenclature in the following areas:
a. The metric system of measurement
b. Standard analytical laboratory apparatus (e.g., flasks,
burettes, absorbers, pumps, etc.)
c. Standard analytical laboratory instrumentation (e.g.,
colorimeter, spectrophotometer, rotameter, etc.)
d. Standard chemical processes (e.g., filtration, titration,
precipitation, etc.)
e. Commonly used reagents
f. Commonly measured pollutants
g. Computations (e.g., standard temperature and pressure,
calibration plot, line of best fit, etc.)
2. Knowledge of tfie composition of required reagents, the procedures
for their preparation, the cautions attending preparation and use,
method of their storage, and their shelf life.
3. Knowledge of the apparatus required for the task and how it
is configured.
D-6
-------
4. Knowledge of the task procedure with all steps in their proper
sequence.
5. Knowledge of the procedure for operating a spectrophotometer
or colorimeter.
6. Knowledge of the procedure for distilling deionized and
nitrate-free water.
7. Knowledge of the procedure for operating and adjusting a
laboratory balance.
8. Knowledge of the procedure for calculating the pollutant
concentration including the correction to standard temperature
and pressure as required.
9. Knowledge of the procedure for quantitatively diluting
exposed absorbing reagent when the color is too dark to be
read. This includes making appropriate adjustments to the
pollutant concentration calculation.
References
1. Environmental Protection Agency. Reference method for the
determination of nitrogen dioxide in the atmosphere (24 hour
sampling method). Federal Register, Vol. 36, No. 84, Friday,
April 30, 1971, pp. 8200-8201.
2. Jacobs,. Morris B. The chemical analysis of air pollutants.
New York: Interscience Publishers, Inc., 1970, pp. 209-215.
3. U. S. Department of Health, Education, and Welfare. Selected
methods for the measurement of air pollutants. PHSP #999-
AP-11, 1965, pp. Cl-7.
Special Staffing Guidance
The following t$sks also involve the use of the colorimeter (or
spectrophotometer) and require similar skills and knowledge and so
D-7
-------
may be efficiently performed by the sama person who performs the
task considered here:
1. The West Gaeke Analysis (see Page D-9).
2. The Hydrogen Sulfide Analysis (see Page D-21).
3. Sulfates Analysis (see Page D-32).
4. Nitrates Analysis (see Page D-27).
D-8
-------
Determination of Sulfur Dioxide Concentration
in the Atmosphere Using the West-Gaeke Method
Task Overview
There are various methods for measuring the concentration of sulfur
dioxide in the atmosphere. These include:
1. West-Gaeke Method
2. Hydrogen Peroxide Method
3. lodine-Thiosulfate Method
4. Iodine Method
t
These methods are described in References 1 through 4.
The West-Gaeke Method (sometimes called the Pararosaniline or Disulfito-
mercurate Method) has been put forth as a reference method in the Federal
Register (Reference 1), and it is a method often used by air pollu-
tion control agencies. Briefly, the procedure consists of the following
outline of steps:
1. Preparation of the chemical reagents required for performance of
the task (including placing the absorbing reagent in the absorber
in preparation for sampling).
2. Analysis of the sample.
3. Calculation of the sulfur dioxide concentration.
This task is concerned only with preparing for and conducting analysis
of a sample. The assembly and operation of the apparatus used for
collecting the sample will be considered within Air Monitoring (see Volume E)
Occupational Category: Chemical Laboratory Technician
Task Description
The procedure for this method of determining sulfur dioxide
concentration is presented in usable form in Reference 3.
D-9
-------
Skill Requirements
1. The ability to prepare reagents and handle caustic or otherwise
dangerous chemicals without splattering acid, precipitating
an explosion, or otherwise injuring personnel or damaging
equipment.
2. Ability to accurately obtain definite volumes of solutions
using apparatus such as a pipette, syringe, volumetric flask,
or burette.
3. Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability
to
a. Zero the balance .
b. Adjust sensitivity range without extreme changes which
might damage the balance.
c. Read and interpret the indicated mass.
4. Ability to clean glassware and other apparatus without
breakage or injury to oneself.
5. Ability to filter precipitate out of sample solution and
wash the filter and apparatus so as to recover all of the
filtrate.
6. Ability to operate a colorimeter or spectrophotometer in
order to obtain absorbance readings of sample and standard
solutions. This includes the ability to correctly input
sample to the instrument and recognize signs of instrument
malfunction.
7. Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given the
sample absorbance reading and the calibration curve.
D-10
-------
b. Converting the volume of gas samples to the volume at
standard temperature and pressure using the perfect gas
equation.
8. Ability to prepare a calibration curve and compute the slope
of the best fitting straight line, following a detailed step-by-
step procedure. This may require the use of regression
analysis by the least squares method.
Knowledge Requirements
1. Knowledge of general chemical nomenclature in the following areas;
a. The metric system of measurement
b. Standard analytical laboratory apparatus (e.g., flasks,
burettes, absorbers, pumps, etc.)
c. Standard analytical laboratory instrumentation (e.g.,
colorimeter, spectrophotometer, rotameter, etc.)
d. Standard chemical processes (e.g., filtration, titration,
precipitation, etc.)
e. Commonly used reagents
f. Commonly measured pollutants
g. Computations (e.g., standard temperature and pressure,
calibration plot, line of best fit, etc.)
2. Knowledge of the composition of required reagents, the procedures
for their preparation, the cautions attending preparation and
use, method of their storage, and their shelf life.
3. Knowledge of the apparatus required for the task and how it
is configured.
4. Knowledge of the highly poisonous nature of sodium tetrachloro-
mercurate and the corrosive effects of acids.
D-ll
-------
5. Knowledge of the procedure for operating a spectrophotometer
or colorimeter.
6. Knowledge of the procedure for estimating the purity of
pararosaniline hydrochloride.
7. Knowledge of the procedure for operating and adjusting a
laboratory balance.
8. Knowledge of the procedure for calculating the pollutant
concentration including the correction to standard temperature
and pressure as required.
References
1. Environmental Protection Agency. Reference method for the
determination of sulfur dioxide in the atmosphere (pararosaniline
method). Federal Register. Vol.36* No. 8A, Friday, April 30,
1971, pp. 8187-8190.
2. Jacobs, Morris B. The chemical analysis of air pollutants.
New York: Interscience Publishers, Inc., 1970, pp. 170-178.
3. U. S. Department of Health, Education, and Welfare. Selected
methods for the measurement of air pollutants. PHSP //999-AP-ll,
1965, pp. Al-5.
4. West, P. W., and Gaeke, G. C. Fixation of sulfur dioxide and
disulfitomercurate (II) and subsequent colorimetric estimation.
Journal of Analytical Chemistry, Vol. 28» No. 12, December
1956, pp. 1816-1819.
Special Staffing Guidance
The following tasks also involve the use of the colorimeter (or
spectrophotometer), require similar skills and knowledge and so may
be efficiently performed by the same person who performs the task
D-12
-------
considered here;
1. The Saltzman Analysis (see Page D-4).
2. The Hydrogen Sulfide Analysis (see Page D-21).
3. Sulfates Analysis (see Page D-32).
4. Nitrates Analysis (see Page D-27).
D-13
-------
Determination of Sulfur Dioxide and Sulfur Trioxide
Concentrations in Stack Gases
Task Overview
This is a method which was developed by the Shell Development Company
(Reference 1), and it is suitable for measuring concentrations of
sulfur dioxide and sulfur trioxide in stack gases. The following is
an outline of the task procedure:
1. Preparation of the chemical reagents required for performance
of the task (including putting the absorbing reagents in the
absorbers).
e
2. Preparation of the sample for analysis.
3. Analysis of the sample using a titration technique.
4. Calculation of the concentrations.
The assembly and operations of the apparatus used to collect the
stack gas sample will be covered under Source Testing (see Volume F).
Occupational Category; Chemical Laboratory Technician
Task Description
The procedure for determining sulfur dioxide and sulfur trioxide
concentrations is presented in usable form in Reference 1.
Skill Requirements
1. The ability to prepare reagents and handle caustic or otherwise
dangerous chemicals without splattering acid, precipitating
an explosion, or otherwise injuring personnel or damaging
equipment.
2. Ability to accurately obtain definite volumes of solutions
usin^ apparatus such as a pipette, syringe, volumetric flask,
or burette.
D-14
-------
3. Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability to:
a. Zero the balance.
b. Adjust sensitivity range without extreme changes which
might damage the balance.
c. Read and interpret the indicated mass.
4. Ability to clean glassware and other apparatus without breakage
or injury to oneself.
5. Ability to assemble sampling apparatus with each component in
proper sequence using butt-to-butt connections, tygon tubing,
and silicone or florocarbon grease as appropriate to create
a leak-proof assembly.
6. Ability to filter precipitate out of sample solution and
wash the filter and apparatus so as to recover all of the
filtrate.
7. Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given the
sample absorbance reading and the calibration curve.
b. Converting the volume of gas sampled to the volume at
standard temperature and pressure using the perfect
gas equation.
8. Ability to distill water so that it is deionized and nitrate-
free.
9. Ability to accurately titrate solutions and detect the subtle
color change representing the end point.
10. Ability to create a partial vacuum in the isopropyl absorber
and rinse the filter tube before suction is lost.
D-15
-------
Knowledge Requirements
1. Knowledge of general chemical nomenclature in the following areas:
a. The metric system of measurement
b. Standard analytical laboratory apparatus (e.g., flasks,
burettes, absorbers, pumps, etc.)
c. Standard analytical laboratory instrumentation (e.g.,
colorimeter, spectrophotometer, rotameter, etc.)
d. Standard chemical processes (e.g., filtration, titration,
precipitation, etc.)
e. Commonly used reagents?
f. Commonly measured pollutants
g. Computations (e.g., standard temperature and pressure,
calibration plot, line of best fit, etc.)
2. Knowledge of the composition of required reagents, the procedures
for their preparation, the cautions attending preparation and
use, method of their storage, and their shelf life.
3. Knowledge of the apparatus required for the task and how it is
configured.
4. Knowledge of the task procedure with all steps in their proper
sequence.
5. Knowledge of the procedure for distilling deionized and
nitrate-free water.
i
6. Knowledge of the procedure for operating and adjusting a
laboratory balance.
7. Knowledge of the procedure for calculating the pollutant
concentration including the correction to standard temperature
and pressure as required.
D-16
-------
References
1. Shell Development Co., Anal. Dept. Shell development company
method for determination of sulfur dioxide and sulfur trioxide.
4S16/59a. Emeryville, California: Author, 1959. pp. 85-87.
Special Staffing Guidance
Except for the need to perform a titration, the general skills and knowledge
required to perform this task are similar to those required for the other
standard wet test analyses. It can be assigned in combination with these
other analyses as desired.
D-17
-------
Determination of Suspended Particulate Concentration
in the Atmosphere by Means of High Volume Sampling
Task Overview
The purpose of this task is to obtain an indication of the amount of
solid particles suspended in the atmosphere. The task description below
is representative of the way the task is performed in the agencies. It
is also similar to the descriptions found in Reference 1 and 2. The
actual collection of the sample using the high volume air sampler will
be covered within Air Monitoring (see Volume E).
Occupational Category; Chemical Laboratory Technician or Equipment Technician
t
Task Description
Prepare filter:
1. Obtain high volume sample filter and dry in an oven
for 24 hours. Cool filter in a desiccator.
2. Weigh the dry filter on an analytical balance.
Determine particulate concentration:
1. Dry the exposed filter for 24 hours; cool the filter;
and obtain the new weight.
2. Calculate the total volume of air sampled by multiplying
the average flow rate by the total sampling time.
3. Divide the particulate weight by the total volume of air
sampled and express the concentration in ug/m .
Skill Requirements
1. Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability to:
a. Zero the balance.
b. Adjust sensitivity range without extreme changes
which might damage the balance.
c. Read and interpret the indicated mass.
»
D-18
-------
2. Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given
the sample absorbance reading and the calibration
curve.
b. Converting the volume of gas sampled to the volume
at standard temperature and pressure using the perfect
gas equation.
3. Ability to transport and handle filtering media using forceps
if required so as not to contaminate it or lose material from
it prior to weighing and analysis.
Knowledge Requirements
1. Knowledge of the apparatus required for the task and how it is
configured.
2. Knowledge of the task procedure with all steps in their proper
sequence.
3. Knowledge of the procedure for operating the drying oven and
desiccator.
4. Knowledge of the procedure for operating and adjusting a
laboratory balance.
5. Knowledge of the procedure for calculating the pollutant con-
centration including the correction to standard temperature
and pressure as required.
References
1. Environmental Protection Agency. Reference method for the
determination of suspended particulates in the atmosphere
(high volume method). Federal Register, Vol. 36, No. 84,
Friday, April 30, 1971, pp. 8191-2.
D-19
-------
2. Jacobs, M. B. The chemical analysis of air pollutants, New
York: Interscience Publishers, Inc., 1970, pp. 93-96.
Special Staffing Guidance
1. Because of the relative simplicity of this task it could effectively
be performed by an inexperienced employee with a modest amount of
on-the-job training.
2. Since this task does not require skills and knowledge necessary
for wet test chemical analyses it could also be assigned to an
•Equipment Technician instead of the Chemical Laboratory Technician.
t
3. The following tasks also involve analysis of particulate matter
as collected by the high volume air sampler and might also be
assigned to the same person who performs this task:
a. Metal Concentration Analysis (see D-37).
b. Sulfates Analysis Csee Page D-32).
c. Nitrates Analysis Csee Page D-27).
D-20
-------
Determination of Hydrogen Sulfide Concentration
in the Atmosphere Using the Methylene Blue Method
Task Overview
The Metihylene Blue Method is the method typically used to measure the
concentration of hydrogen sulfide in the atmosphere. Other methods
available include the Cadmium Sulfide Method and the Impregnated Ceramic
Tile Method.
The analysis procedure described below was derived from field observation
and the description contained in Reference 1. The preparation and oper-
ation of the apparatus for collecting the sample is considered within
Air Monitoring (see Volume E).
Occupational Category; Chemical Laboratory Technician
Task Description
Prepare the following reagents:
1. Absorbing Reagent. Dissolve 4.3 g of cadmium sulfate in
water. Add 0.3 g of sodium hydroxide and 10 g of STRACTAN.
Dilute the solution to one liter with freshly distilled
water and mix.
2. Amine Acid Stock Solution. Add 50 ml of concentrated
sulfuric acid to 30 ml of water and cool. Dissolve 12 g
of N, N-dimethyl^p-phenylenediamine in the solution and
refrigerate.
3. Amine Acid Working Solution. Dilute 25 ml of stock amine
acid solution to one liter with 1:1 sulfuric acid and
refrigerate.
4.. Ferric Chloride Stock Solution. Dissolve 100 g of ferric
chloride in water and dilute to 100 ml. Refrigerate.
D-21
-------
5. Sodium Hydroxide Stock Solution, 1 Normal. Dissolve 40 g of
sodium hydroxide in water and dilute to one liter.
6. Sodium Hydroxide Working Solution, 0.1 Normal. Dilute 100 ml
of sodium hydroxide stock solution to one liter with water.
Prepare standard curve:
7. Purge a 100 ml, graduated Goetz tube with nitrogen gas and
seal with a rubber septum. Using a syringe, add 100 ml of
0.1 N sodium hydroxide to the Goetz tube. Place the tube in
cooling bath and cool to 4°C.
8. Withdraw 1.5 ml of hydrogen sulfide from a tank of purified
hydrogen sulfide gas, using a syringe. Inject the hydrogen
sulfide into the Goetz tube, vigorously shake, and cool again
to 4°C. (This solution is stable for only 30 minutes. There-
fore, it is required that two personnel complete the standardi-
zation process.).
9. Purge a 250 ml Erlenmeyer flask with nitrogen. Pipette 50 ml
of the hydrogen sulfide solution to the flask. Then, add 10 ml
of 0.01 N potassium iodate solution and about 100 mg of potas-
sium iodide crystals. After the crystals have dissolved, add
2 ml of 2 N sulfuric acid. Mix the solution, stopper the flask,
and set the flask in a cold water bath for 5 minutes.
10. Titrate the sulfide solution against a solution of 0.02 N sodium
thiosulfate. Then, titrate distilled water against the same
solution. Titrate the solutions to a pale yellow color; add a
small amount of thyodine and titrate until clear.
11. Pipette 5 ml of standard hydrogen sulfide solution from the
Goetz tube into a 50 ml volumetric flask. Dilute the solution
to 50 ml with water. From this flask pipette 0, 1, 2, 3, 4, i
5, 10, and 15 ml samples into 50 ml volumetric flasks with 30 ml
of absorbing reagent each. To each flask add 0.6 ml of amine
acid working solution and one drop of ferric chloride working
solution, and dilute to 50 ml with water. Allow solution to
stand for 30 minutes for color development.
D-22
-------
12. Place each sample in a 10 cm tubular cell. Using a spectro-
photometer (such as the Hitachi-Perkin-Elmer 130 U.V. Visible
Spec tropho tome ter.) obtain the absorbance reading for each
sample at 670 mu.
13. Calculate the normality of the hydrogen sulfide from the
results of the titration, using the equation: N x ml (thio-
sulfate) = N x ml (hydrogen sulfide). Convert the result
to ug/ml and correct for the 1 to 10 dilution.
14. Plot a standard curve of absorbance vs. ug/ml of hydrogen
sulfide. Compute the slope of the best fitting straight line.
Analyze air sample:
15. Add 0.6 ml of amine acid'working solution and one drop of
ferric chloride working solution to the sample. Dilute the
sample to 50 ml with water in a volumetric flask. Also,
prepare a blank using 30 ml of absorbing reagent, 0.6 ml
of amine acid working solution, and one drop of ferric
chloride working solution. (This is used for zeroing the
spectrophotometer.) Allow the solutions to stand for 30
minutes.
16. Obtain the absorbance of the sample, using the spectro-
photometer.
17. Determine the amount (ug) of hydrogen sulfide in the sample,
using the absorbance reading and the standard curve. Cal-
culate the volume of the sample from the sampling rate and
time. Calculate the concentration of hydrogen sulfide in
parts-per-billion.
Skill Requirements
1. The ability to prepare reagents and handle caustic or other-
wise dangerous chemicals without splattering acid, precip-
itating an explosion, or otherwise injuring personnel or
damaging equipment.
-------
Ability to accurately obtain definite volumes of solutions
using apparatus such as a pipette, syringe, volumetric flask,
or burette.
Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability
to:
a. Zero the balance.
b. Adjust sensitivity range without extreme changes
which might damage the balance.
c. Read and interpret the indicated mass.
Ability to clean glassware and other apparatus without break-
age or injury to oneself.
Ability to operate a colorimeter or spectrophotometer in
order to obtain absorbance readings of sample and standard
solutions. This includes the ability to correctly input
sample to the instrument and recognize signs of instrument
malfunction.
Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given the
sample absorbance reading and the calibration curve.
b. Converting the volume of gas sampled to the volume at
standard temperature and pressure using the perfect gas
equation.
Ability to prepare a calibration curve and compute the slope
of the best fitting straight line, following a detailed step-
by-step procedure. This may require the use of regression
analysis by the least squares method.
Ability to read and interpret data from a table, psychometric
chart, or a nomograph.
D-24
-------
9. Ability to distill water so that it is deionized and nitrate-
free.
10. Ability to handle pressurized gas without endangering personnel
or equipment.
11. Ability to proficiently purge and seal a Goetz tube or Erlenmeyer
flask with nitrogen gas.
12. Ability to accurately titrate solutions and detect the subtle
color change representing the end point.
Knowledge Requirements
1. Knowledge of general chemical nomenclature in the following areas:
a. The metric system of measurement.
b. Standard analytical laboratory apparatus (e.g., flasks,
burettes, absorbers, pumps, etc.).
c. Standard analytical laboratory instrumentation (e.g.,
colorimeter, spectrophotometer, rotameter, etc.).
d. Standard chemical processes (e.g., filtration, titration,
precipitation, etc.).
e. Commonly used reagents.
f. Commonly measured pollutants.
g. Computations (e.g., standard temperature and pressure,
calibration plot, line of best fit, etc.).
2. Knowledge ,of the composition of required reagents, the pro-
cedures for their preparation, the cautions attending prep-
aration and use, method of their storage, and their shelf life.
3. Knowledge of the apparatus required for the task and how it
is configured.
4. Knowledge of task procedure with all steps in their proper
sequence.
5. Knowledge of the procedure for operating a spectrophotometer
or colorimeter.
D-25
-------
6. Knowledge of the procedure for distilling deionized and nitrate-
free water.
7. Knowledge of the procedure for operating and adjusting a
laboratory balance.
8. Knowledge of the procedure for calculating the pollutant
concentration including the correction to standard temperature
and pressure as required.
References
1. Jacobs, M. B. The chemical analysis of air pollutants.
New York: Interscience Publishers, Inc. 1970, pp. 182-188.
Special Staffing Guidance
The following tasks also involve the use of the colorimeter (or
spectrophotometer) and require similar skills and knowledge and
so may be efficiently performed by the same person who performs the
task considered here:
a. The West-Gaeke Analysis (see Page D-9).
b. The Saltzman Analysis (see Page D-4).
c. Sulfates Analysis (see Page D-32).
d. Nitrates Analysis (see Page D-27).
D-26
-------
Determination of Nitrate Concentration in
Suspended Atmospheric Participates Using the 2, 4 Xylenol Method
Task Overview
This task is very similar to the determination of sulfates in suspended
atmospheric participates and it is also performed routinely in many
agencies. The task involves obtaining a 2, 4 xylenol treated water
sample from a high volume air sampler filter. The Nitrated 2, 4 xylenol
is extracted from the sample, purified, and analyzed colorimetrically.
The analysis can be outlined as follows:
1. Preparation of the chemical reagents required for performance
of the task.
2. Assembly of the refluxing apparatus.
3. Preparation of the sample for analysis.
4. Colorimetric analysis of the sample.
5. Preparation of standardized curve.
6. Calculation of the nitrate concentration.
The actual collection of the sample using the high volume air sampler
will be covered within Air Monitoring (see Volume E).
Occupational Category; Chemical Laboratory Technician
Task Description
The procedure for this method of determining nitrate concentration
is presented in usable form in Reference 2. An abbreviated description
appears in Reference 1.
Skill Requirements
1. The ability to prepare reagents and handle caustic or otherwise
dangerous chemicals without splattering acid, precipitating an
explosion, or otherwise injuring personnel or damaging equipment.
D-27
-------
2. Ability to accurately obtain definite volumes of solutions
using apparatus such as a pipette, syringe, volumetric flask,
or burette.
3. Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability to:
a. Zero the balance.
b. Adjust sensitivity range without extreme changes which
might damage the balance.
c. Read and interpret the indicated mass.
4. Ability to clean glassware and other apparatus without breakage
or injury to oneself.
5. Ability to assemble sampling apparatus with each component
-in proper sequence using butt-to-butt connections, tygon tubing,
and silicone or florocarbon grease as appropriate to create
a leak-proof assembly.
6. Ability to filter precipitate out of sample solution and wash
the filter and apparatus so as to recover all of the filtrate.
7. Ability to operate a colorimeter or spectrophotometer in
order to obtain absorbance readings of sample and standard
solutions. This includes the ability to correctly input
sample to the instrument and recognize signs of instrument
malfunction.
8. Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure•
Such equations Include:
a. Calculating the concentration of a pollutant given the
sample absorbance reading and the calibration curve.
b. Converting the volume of gas sampled to the volume at
standard temperature and pressure using the perfect gas
equation.
D-28
-------
9. Ability to prepare a calibration curve and compute the slope
of the best fitting straight line, following a detailed step-
by-step procedure. This may require the use of regression
analysis by the least squares method,
10. Ability to read and interpret data from a table, psychometric
chart, or a nomograph.
11. Ability to transport and handle filtering media using forceps
if required so as not to contaminate it or lose material from
it prior to weighing and analysis.
12. Ability to draw off the various layers of a separated solution.
t
13. Ability to^prevent the formation of emulsions in the sample
by means of proper agitation.
Knowledge Requirements
1. Knowledge of general chemical nomenclature in the following
areas:
a.. The metric system of measurement.
b. Standard analytical laboratory apparatus (e.g., flasks,
burettes, absorbers, pumps, etc.)
c. Standard analytical laboratory instrumentation (e.g.,
colorimeter, spectrophotometer, rotameter, etc.)
d. Standard chemical processes (e.g., filtration, titration,
precipitation, etc.)
e. Commonly used reagents
f. Commonly measured pollutants
g. Computations (e.g., standard temperature and pressure,
calibration plot, line of best fit, etc.)
D-29
-------
2. Knowledge of the composition of required reagents, the procedures
for their preparation, the cautions attending preparation and
use, method of their storage, and their shelf life.
3. Knowledge of the apparatus required for the task and how it
is configured.
4. Knowledge of the task procedure with all steps 'in their proper
sequence.
5. Knowledge of the procedure for operating a spectrophotometer
or colorimeter.
6. Knowledge of the procedure for operating the drying oven
and desiccator.
7. Knowledge of the procedure for operating the refluxing
apparatus.
8. Knowledge of the procedure for operating and adjusting a
laboratory balance.
9. Knowledge of the procedure for calculating the pollutant
concentration including the correction to standard temperature
and pressure as required.
10. Knowledge of the procedure for removing or adjusting for
nitrates pre-existing on the filter medium.
References
1. Jacobs, M. B. The chemical analysis of air pollutants. New
York: Interscience Publishers, Inc., 1970, pp. 117-118.
2. U. S. Department of Health, Education, and Welfare. Selected
methods for the measurement of air pollutants. PHSP #999-AP-ll,
1965, pp. Jl-4.
D-30
-------
Special Staffing Guidance
1. The following tasks also involve the use of the colorimeter (or
spectrophotometer) and require similar skills and knowledge and
so may be efficiently performed by the same person who performs
the task considered here:
a. The West-Gaeke Analysis (see Page D-9).
b. The Saltzman Analysis (see Page D-4).
c. The Hydrogen Sulfide Analysis Csee Page D-21)
d. Sulfates Analysis (see Page D-32).
f
2. The following tasks also involve analysis of particulate matter as
collected by the high volume air sampler and might also be assigned
to the same person who performs this task:
a. Suspended Particulate Concentration Analysis (see Page D-42).
b. Metal Concentration Analysis (see Page D-37).
c. Sulfates Analysis ( see Page D-32).
3. Because of the similarity between this task and the Sulfates
Analysis (see D-32), both could be performed by the same person.
D-31
-------
Determination of Sulfate Concentration in
Suspended Atmospheric Participates Using the
Turbidimetric Barium Sulfate Method
Task Overview
This task is routinely performed in several agencies and involves colori-
metric analysis of a barium chloride treated water sample obtained from
a high volume air sampler filter. The outline of the procedure is as
follows:
1. Preparation of the chemical reagents required for performance
of the task.
t
2. Assembly of the refluxing apparatus.
3. Preparation of the sample for analysis.
4. Colorimetrie analysis of the sample.
5. Preparation of standardized curve.
6. Calculation of the sulfate concentration.
The actual collection of the sample using the high volume air sampler
will be covered within Air Monitoring (see Volume E).
Occupational Category; Chemical Laboratory Technician
Task Description
The procedure for this method of determining sulfate concentration
is presented in usable form in Reference 2. An abbreviated description
appears in Reference 1.
Skill Requirements
1. The ability to prepare reagents and handle caustic or otherwise
dangerous chemicals without splattering acid, precipitating
an explosion, or otherwise injuring personnel or damaging
equipment.
D-32
-------
2. Ability to accurately obtain definite volumes of solutions
using apparatus such as a pipette, syringe, volumetric' flask,
or burette.
3. Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability to:
a. Zero the balance.
b. Adjust sensitivity range without extreme changes which
might damage the balance.
c. Read and interpret the indicated mass.
4. Ability to clean glassware and other apparatus without breakage
or injury to oneself.
5. Ability to assemble sampling apparatus with each component in
proper sequence using butt-to-butt connections, tygon tubing,
and silicone or florocarbon grease as appropriate to create
a leak-proof assembly.
6. Ability to filter precipitate out of sample solution and
wash the filter and apparatus so as to recover all of the
filtrate.
7. Ability to operate a colorimeter or spectrophotometer in
order to obtain absorbance readings of sample and standard
solutions. This includes the ability to correctly input sample
to the instrument and recognize signs of instrument malfunction.
8. Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given the
sample absorbance reading and the calibration curve.
b. Converting the volume of gas sampled to the volume at
standard temperature and pressure using the perfect .
gas equation.
D-33
-------
9. Ability to prepare a calibration curve and compute the slope
of the best fitting straight line, following a detailed step-
by-step procedure. This may require the use of regression
analysis by the least squares method.
10. Ability to read and interpret data from a table, psychometric
chart, or a nomograph.
11. Ability to transport and handle filtering media using forceps
if required so as not to contaminate it or lose material from
it prior to weighing and analysis.
Knowledge Requirements
1. Knowledge of general chemical nomenclature in the following
areas:
a. The metric system of measurement
b. Standard analytical laboratory apparatus (e.g., flasks,
burettes, absorbers, pumps, etc.)
c. Standard analytical laboratory instrumentation (e.g.,
colorimeter, spectrophotorneter, rotameter, etc.)
d. Standard chemical processes (e.g., filtration, titration,
precipitation, etc.)
e. Commonly used reagents
f. Commonly measured pollutants
g. Computations (e.g., standard temperature and pressure,
calibration plot, line of best fit, etc.)
2. Knowledge of the composition of required reagents, the pro-
cedures for their preparation, the cautions attending prepara-
tion and use, method of their storage, and their shelf life.
3. Knowledge of the apparatus required for the task and how it
is configured.
D-34
-------
4. Knowledge of the task procedure with all steps in thed,r proper
sequence.
5. Knowledge of the procedure for operating a spectrophotometer
or colorimeter.
6. Knowledge of the procedure for operating the refluxing
apparatus,
7. Knowledge of the procedure for operating and adjusting a
laboratory balance.
8. Knowledge of the procedure for calculating the pollutant
concentration including the correction to standard temperature
and pressure as required.
9. Knowledge of • the procedure for removing or adjusting for
sulfates pre-existing on the filter medium.
References
1. Jacobs, M. B. The chemical analysis of air pollutants. New
York: Interscience Publishers, Inc., 1970, pp. 116-117.
2. U. S. Department of Health, Education, and Welfare. Selected
methods for the measurement of air pollutants. PHSP 0999-AP-ll,
1965, pp. 11-4.
Special Staffing .Guidance
1. The following tasks also involve the use of the colorimeter (or
spectrophotometer) and require similar skills and knowledge and
so may be efficiently performed by the same person who performs
the task considered here:
a. The West-Gaeke Analysis (see Page D-9).
b. The Saltzman Analysis (see Page D-4).
c. The Hydrogen Sulfide Analysis (see Page D-21).
d. The Nitrates Analysis (see Page D-27).
D-35
-------
2. The following tasks also involve analysis of particulate matter
as collected by the high volume air sampler and might be assigned
to the same person who performs this task:
a. Suspended Particulate Concentration Analysis (see Page D-18)
b. Metal Concentration Analysis (see Page D-37).
c. Nitrates Analysis (see Page D-27).
3. Because of the similarity between this task and the Nitrates
Analysis (see D-27), both could be performed by the same person.
D-36
-------
Determination of Metal Concentration in
Suspended Atmospheric Particulates by
Means of High Volume Sampling
Task Overview
The task described below is representative of various methods for measuring
the concentration of metals in the suspended atmospheric particulates from
a high volume sample. The method is based on the use of an atomic absorp-
tion spectrophotometer. Other methods include the use of an emission
spectrograph or a photofluorimeter. Each method is based on specific
atomic properties whose characteristics vary among different types of atoms,
e
The task as described below is concerned with the analysis of a sample.
The actual collection o*f the sample using the high volume air sampler will
be covered within Air Monitoring (see Volume E).
Occupational Category: Chemical Laboratory Technician
Task Description
1. Take an aliquot of the sample filter and place it in an
extraction cup.
2. Prepare a 20 ml solution of acid in an extracting flask
(four parts, by volume, of 1:1 nitric acid to one part of 1:1
hydrochloric acid).
3. Assemble refluxing apparatus.
a. Condenser.
b. Extraction cup.
c. Extracting Flask.
d. Hot plate.
Reflux the acid solution for two hours.
4. Add an additional 15 ml of acid and reflux for another two
hours.
D-37
-------
5. Allow the assembly to cool overnight.
6. Prepare vacuum-distillation apparatus:
a. Pump.
b. Primary and secondary traps.
c. Extracting flask.
d. Warm water bath.
7. Run distillation to completion, periodically replenishing
dry ice in traps and warm water in the bath.
8. Remove the extraction flask from the apparatus.
9. Prepare one liter of acid solution (43 ml of concentrated
hydrochloric apid to 33 ml of concentrated nitric acid,
diluted to one liter with water) and add 40 ml of the solution
to the sample in the extraction flask.
10. Swirl the suspension in the flask. Cover the flask with
parafilm and allow it to sit overnight.
11. Transfer the sample to a volumetric flask and dilute it to
100 ml with water.
12. Prepare four standard solutions by adding graduated amounts
of metal salts (known concentration) to 8 ml aliquots of the
sample.
13. Prepare atomic absorption spectrophotometer for the .specific
metal.
14. Take three absorbance readings on each standard solution and
calculate the average.
15. Plot the absorbance against the concentration of metal added
in each standard.
16. Construct a best fitting straight line and calculate the slope
of the line using regression analysis by the least squares
method.
iJ-38
-------
17. Calculate the X-intercept of the curve and correct it, using
the value obtained on a blank filter.
18. Obtain the volume of air sampled and compute the ambient
3
concentration of the metal in ug/m .
19.- Obtain the average residue concentration of the particulate
and calculate the weight percentage of metal in the average
residue.
Skill Requirements
1. The ability to prepare reagents and handle caustic or other-
wise dangerous chemicals without splattering acid, precipitating
an explosion, or otherwise injuring personnel or damaging
equipment.
2. Ability to accurately obtain definite volumes of solutions
using apparatus such as a pipette, syringe, volumetric flask,
or burette.
3. Ability to clean glassware and other apparatus without breakage
or injury to oneself.
4. Ability to assemble sampling apparatus with each component in
proper sequence using butt-to-butt connections, tygon tubing,
and silicone or florocarbon grease as appropriate to create
a leak-proof assembly.
5. Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given
the sample absorbance reading and the calibration
curve.
b. Converting the volume of gas sampled to the volume
at standard temperature and pressure using the perfect
gas equation.
D-39
-------
6. Ability to prepare a calibration curve and compute the slope
of the best fitting straight line, following a detailed step-
by-step procedure. This may require the use of regression
analysis by the least squares method.
1'. Ability to transport and handle filtering media using forceps
if required so as not to contaminate it or lose material from
it prior to weighing and analysis.
8. Ability to insert a Gooch crucible into a vacuum^jacketed
extractor without damaging the extractor.
9. Ability to operate the atomic absorption spectrophotometer
so as to obtain accurate absorption readings of samples and
standards. This includes the ability to correctly input
sample to the instrument and to detect instrument malfunction.
10. Ability to perform a quantitative transfer of a solution from
one container to another without losing any of the sample.
11. Ability to clean grease from the neck of a flask without
contaminating the contained sample with the cleaning agent.
Knowledge Requirements
1. Knowledge of general chemical nomenclature in the following areas:
a. The metric system of measurement.
b. Standard analytical laboratory apparatus (e.g., flasks,
burettes, absorbers, pumps, etc.)
c. Standard analytical laboratory instrumentation (e.g.,
colorimeter, spectrophotometer, rotameter, etc.)
d. Standard chemical processes (e.g., filtration, titration,
precipitation, etc.).
e. Commonly used reagents.
f. Commonly measured pollutants.
g. Computations (e.g., standard temperature and pressure,
calibration plot, line of best fit, etc.).
D-40
-------
2. Knowledge of the composition of required reagents, the pro-
cedures for their preparation, the cautions attending prepara-
tion and use, method of their storage, and their shelf life.
3. Knowledge of the apparatus required for the task and how it
is configured.
4. Knowledge of the task procedure with all steps in their proper
sequence.
5. Knowledge of the procedure for operating the refluxing
apparatus.
"• Knowledge of the procedure for operating the vacuum distillation
apparatus.
\
7. Knowledge of the procedure for operating the atomic absorption
spectrophotometer.
References
1. Jacobs, M. B. The chemical analysis of air pollutants. New
York: Tnterscience Publishers, Inc., 1970, pp. 98-101.
Special Staffing Guidance
The following tasks also involve analysis of particulate matter as
collected by the high volume air sampler and might also be assigned
to the same person who performs this task:
1. Suspended Particulate Concentration Analysis (see Page D-18).
r,
2. Sulfates Analysis (see Page D-32).
3. Nitrates Analysis (see Page D-27).
D-41
-------
Determination of Particulate Concentration
in Stack Emissions
Task Overview
The lab support requirement for determining the particulate concentration
in $tack emission depends on what method of particulate collection is
employed. In general the analysis procedure involves the following steps:
1. Drying, weighing, and otherwise preparing the alundum or paper
thimble filter, cyclone collector or electrostatic precipitator
to be used in the sampling train.
2. Adding measured amounts of water to the impingers to be used
in the sampling train.
3. Determining the particulate concentration of the dry collector
and impingers after sampling.
The assembly and operation of the sampling train used for collecting
the particulate sample will be covered under Source Testing (see Volume F)
Occupational Category; Chemical Laboratory Technician
Task Description
Procedures covering the various techniques for analysis of
particuiate concentration is provided in references 1, 2, 4, 5, 6,
7, 10, and 11. The remainder of the publications listed (References
3, 8, and 9) contain useful information with regard to stack testing
equipment and selected testing techniques.
Skill Requirements
1. Ability to accurately obtain definite volumes of solutions
using apparatus such as a pipette, syringe, volumetric flask,
or burette.
D-42
-------
2. Ability to use an analytical balance to obtain an accurate
weight of a dry reagent or filter. This includes the ability
to:
a. Zero the balance,
b. Adjust sensitivity range without extreme changes
which might damage the balance.
c. Read and interpret the indicated mass.
3. Ability to clean glassware and other apparatus without breakage
or injury to oneself.
c
4. Ability to assemble sampling apparatus with each component in
proper sequence using butt-to-butt connections, tygon tubing,
and silicone of florocarbon grease as appropriate to create
a leak-proof assembly.
5. Ability to filter precipitate out of sample solution and wash
the filter and apparatus so as to recover all of the filtrate.
6. Ability to quickly and correctly solve an algebraic equation
in several unknowns using a detailed step-by-step procedure.
Such equations include:
a. Calculating the concentration of a pollutant given
the sample absorbance reading and the calibration curve.
b. Converting the volume of gas sampled to the volume at
standard temperature and pressure using the perfect gas
i
equation.
7. Ability to sand the lip of a alundum thimble to assure a good
seal, removing all loose material.
Knowledge Requirements
1. Knowledge of the apparatus required for the task and how it
is configured.
D-43
-------
2. Knowledge of the task procedure with all steps in their proper
sequence.
3. Knowledge of the procedure for operating the drying oven
and desiccator.
4. Knowledge of the procedure for operating and adjusting a
laboratory balance.
5. Knowledge of the procedure for obtaining the particulate
weight trapped by both the dry collector and the impingers
and combining these to obtain the total particulate weight.
6. Knowledge of the procedure for calculating:
a. Gas volume, corrected to standard conditions of temperature
and pressure.
b. Particulate concentration.
c. Emission rate.
7. Knowledge of procedure for draining the sampling train of
moisture and measuring the condensate.
References
1. American Society for Testing and Materials. Standard method
for sampling stacks for particulate matter. Philadelphia:
Author, 1971. D2928-71.
2. American Society of Mechanical Engineers. Determining dust
concentration in a gas stream. New York: Author, 1957.
3. Committee on Industrial Ventilation. Industrial ventilation.
A manual of recommended practice. Lansing, Michigan: American
Conference of Governmental Industrial Hygienists, 1970 (llth
Edition), pp. 9(1-8).
4. Devorkin, H., Chass, R., Fudurich, A., & Kanter, C. R. Holmes
(Ed.) Air pollution source testing manual. Los Angeles: Air
Pollution Control District, Los Angeles County, November 1965.
D-44
-------
5. Environmental Protection Agency. Standards of performance for
new stationary sources. Federal Register. Volume _36_, Number 159,
August 17, 1971.
6. Haaland, H. H, (Ed.) Methods for determination of velocity.
dust and mist content of gases. Bulletin WP-50. Seventh
Edition. Los Angeles: Western Precipitation Division/Joy
Manufacturing Company, 1968.
7. Jacobs, M. B. The chemical analysis of air pollutants. New
York: Interscience Publishers, Inc., 1960. pp. 140-155.
8. Joy Manufacturing Company, Western Precipitation Division.
Gas velocity and dust determination equipment. Catalog GV22.
Los Angeles," Author.
9. Kimura, G. Emission control of flue-fed incinerators by use
of air pollution control devices. Chicago: Department of
Air Pollution Control, City of Chicago, November 1969. pp. 87-90.
10. PEDCo-Environmental Specialists, Inc. Administrative and
technical aspects of source sampling for particulates. Contract
No. CPA 70-124. Research Triangle Park, North Carolina:
Environmental Protection Agency, May 1971.
11. Weisburd, M. (Ed.) Air pollution control field operations manual.
A guide for inspection and enforcement. Washington, D. C.:
U. S. Department of Health, Education, and Welfare; Public Health
Service, Division of Air Pollution,. 1962. PHSP #937. pp. 167-176.
i
Special Staffing Guidance
The task of determining the particulate concentration in the dry collector
is similar in its general form to the suspended particulate concentration
analysis (see D-37). The determination of the particulates trapped by
the impingers is a relatively simple task requiring the manipulation of
wet test analysis apparatus. Thus this task can be assigned to
D-45
-------
a relatively inexperienced employee with moderate on-the-job training.
This is especially true where the employee has already learned the
suspended particulate concentration analysis and it is desired to
introduce him to wet test analysis concepts, apparatus, and techniques,
D-46
-------
Identification of the Constituents of Dust Particles
Task Overview
The objective of this task is to identify the constituents of dust par-
ticles so that the dust can be associated with a specific source. The
dust sample is usually collected as a result of a citizen complaint or
a routine patrol inspection.
The analysis of the dust sample consists of three parts:
1. An approximate identification is made through the use of a
stereo microscope.
2. All compounds are identified using an X-ray defractometer.
3. A picture is taken of the sample for later use as a comparison
standard.
Occupational Category: Chemical Laboratory Technician or Equipment Technician
Task Description
Perform initial identification using a stereo microscope:
1. Place the dust sample on a card or piece of filter paper and
position it under a stereo microscope. (Choose the color
of the card so as to provide a contrasting background for the
sample.)
2. Adjust the light, focus, and magnification of the microscope
until a clear image is obtained.
3. Identify the sample according to particle shape, texture, size,
and color. Use standardized comparison samples as an aid to
identification.
4. If the sample cannot be identified treat it physically or chemically
under the microscope and observe the reaction:
a. Use a magnet in order to detect the presence of iron.
D-47
-------
b. Apply a drop of phenolpthalene to ascertain alkalinity
which might, indicate lime or cement dust.
c. Apply a drop of hydrochloric acid and look for a bubbling
reaction which would indicate the presence of a carbonate.
Use X-ray defractometer to identify or verify dust constituents:
5. Grind a portion of the sample down to a size which is appropriate
for X-ray analysis. Use a grinding machine such as the Wig L Bug.
6. Place a thin layer of the ground sample on a slide and insert
it into the X-ray defractometer.
7. Start up the instrument, being sure to turn on cooling water
and recorder, and adjust the voltage to the required setting.
CAUTION: Wear X-ray badge.
8. Open the lead shield and start the instrument at 5 and allow
the arm to run through the entire arc. Close the lead shield
and shut down the instrument.
9. Remove the recorder chart and mark the degrees of arc on the
chart.
10. Choose a peak on the chart and look up the angle (degrees of
arc) on a table which describes the angle as a function of the
distance between atoms of a compound. Obtain the value of the
distance between atoms which corresponds to the angle.
11. Using the value of the distance between atoms (- .01 A*), find
the corresponding compounds on the table which lists compounds
(and their X-ray defraction characteristics) as a function of
distance between atoms. (This step narrows it down to a few
pages of compounds.)
12. Based on the observation's made under the stereo microscope,
choose a compound from the table and note its peak strength.
Compare the peak strength to that found on the chart. If it
does not match, choose another compound.
D-48
-------
13. If the peak strengths do match, note the other peaks caused
by that compound. Check out each peak by working backwards
through the tables, thus finding the corresponding angle and
comparing it with the one on the chart. If all peak positions
and strengths match, then the compound has been identified.
If there is a discrepancy, choose another compound.
14. All peaks on the chart must be checked out until all constituent
compounds are identified.
Photograph the sample:
15. Place a portion of the sample on a slide and place it under a
polarizing microscope mounted with a Polaroid camera.
16. Turn on the light source and adjust voltage so that it corres-
ponds with that indicated on the light meter.
17. Arrange the sample so as to best show all of the physical charac-
teristics of the particles. This may require additional lighting
or background.
18. Adjust the shutter time according to brightness and size of the
particles.
19. Take the picture and treat the print with the chemicals provided
by Polaroid.
Skill Requirements
1. Ability toi adjust the light, focus, and magnification of a
stereo microscope in order to obtain a clear image of a sainple.
2. Ability to recognize the similarities and differences between
the characteristics of a sample dust particle and the charac-
teristics of SL standard comparison sample. The important
characteristics are particle shape, size, texture, and color.
3. Ability to determine how long a sample should be ground before
it is ready for X-ray analysis.
D-49
-------
4. Ability to, spread the ground sample in a layer of the appropriate
thickness on a slide.
5. Ability to accurately mark the recorder chart with the degrees
of arc.
6. Ability to read the recorder chart interpreting the position
and slope of the tracing in terms of the variables represented
on the ordinate and absissa (i.e., the pollutant concentration
over time or the strength of X-ray detraction as a function
of beam angle).
7. Ability to find the compounds which correspond the the peak
characteristics (location and strength) on the recorder chart,
using the recorder chart and X-ray defraction tables. This
involves a trial and error technique, enlightened by the knowl-
edge gained from the preliminary analysis performed with the
stereo microscope.
8. Ability to arrange the sample, the background, and lighting so
as to best show the physical characteristics of the sample in
a photograph taken with a polaroid camera mounted on a polarizing
microscope.
9. Ability to determine the appropriate shutter speed in order to
obtain an acceptable photograph of a dust sample, using a Polaroid
camera mounted on a polarizing microscope. (The decision is based
on the brightness and size of the dust particles.)
10. Ability to service and operate a chart recorder, including
replacing chart roll, resupplying ink (if required), and
adjusting the baseline (zero) point, line density, chart speed,
and sensitivity range.
Knowledge Requirements
1. Knowledge of the apparatus required for the task and how;it is
configured.
D-50
-------
2. Knowledge of the task procedure with all steps in their proper
sequence.
3. Knowledge of the procedure for operating the stereo microscope.
4. Knowledge of the procedure for operating the grinding machine.
5. Knowledge of the procedure for operating the X-ray defractometer.
6. Knowledge of the procedure for using the X-ray defraction tables.
7. Knowledge of the procedure for operating the polarizing
microscope with Polaro.id camera.
8. Knowledge of the procedure for coating Polaroid prints.
Special Staffing Guidance
Since this task does not require skills and knowledge associated
with wet test chemical analyses it could be as efficiently performed by
either an Equipment Technician or a Chemical Laboratory Technician.
D-51
-------
Maintenance of Laboratory Devices
Task Overview
This task involves performance of various maintenance related activities
on the instruments and equipment used in performing the laboratory
analyses in order to maintain the accuracy and reliability of these
devices. The instruments and equipment concerned include:
1. Colorimeters or spectrophotometers
2. Atomic absorption spectrophotometer
'<•
3. X-ray defractometers
4. Analytical balances
5. Drying ovens
6. Flowmeters
7. Vacuum pumps
8. Chart recorder
Occupational Category: Equipment Technician
Task Description
Due to the variety of kinds and types of devices included within
this task it is not possible to state a step-by-step procedure for
performing it. The task, however, does entail the following activities:
1. Installation, which involves unpacking, checking the device
for damage, leveling, and making electrical and/or tubing
connections.
The maintenance of the various laboratory devices has not been analysed
in detail. Therefore, the skills and knowledge presented in the task
package must be considered only as representative.
D-52
-------
2. Servicing, which includes checking, cleaning, lubricating,
adjusting, refilling and simple replacement operations
performed on a scheduled basis.
3. Troubleshooting, i.e., identifying the cause of a malfunction
through evaluation of symptoms and a systematic elimination
of possible causes.
4. Repair, including repair, replacement, cleaning, and adjustment
operations performed to rectify a specific malfunction.
5. Calibration, i.e., adjusting the performance of the device
(e.g., a meter reading) to agree with some standard or
developing a means of converting the performance of the device
to the standard (e.g., development of a conversion chart or
table).
6. Operation, including starting up, operating in various modes,
and shutting off as necessary to perform the other activities.
Skill Requirements
1. Ability to read indicating devices, such as a thermometer,
manometer, dry gas meter, and flow meter, and to interpret
meter readings against a calibration plot as required.
2. Ability to prepare a calibration curve and compute the slope
of the best fitting straight line, following a detailed step-
by-step procedure. This may require the use of regression
analysis by the least squares method.
3. Ability to read and interpret data from a table, psychometric
chart, or a nomograph.
4. Ability to calibrate a sampling train or analyzer rotameter
or flowmeter by making use of a wet test meter.
5. Ability to coordinate adjustment screw or hand knob movements
with meter or chart recorder reading to quickly achieve and
maintain the desired reading.
D-53
-------
6. Ability to level instrument or analyzer during installation
using a level, plumb, screw adjusters, and/or shims.
7. Ability to detect instrument damage caused by shipping, including
dents, breakage, components knocked out of position, loose
electrical and mechanical connections, and hairline cracks
in glass parts.
8. Ability to detect leaks in hose, tubing, and piping connectors
carrying liquids, gases, or vacuum using simple leak detection
aids as appropriate.
9. Ability to disconnect and'connect standard hose tubing and
piping connectors without injury to threads and achieving
leakproof connections. This includes the use of thread
compound and teflon tape as appropriate.
10. Ability to disconnect and connect standard electrical connectors.
This includes identifying leads to facilitate correct connection
and achieving tight connections without damage to the leads or
terminals.
11. Ability to correctly interpret function diagrams, wiring and
tubing diagrams, simple electrical schematics, and trouble-
shooting charts.
12. Ability to use electrical test instruments such as:
1. AC/DO Voltmeter
2. Ammeter
3. Ohnnaeter
to achieve accurate circuit measurements without damage to the
test instruments.
13. Ability to solder and unsolder electrical terminals making
a good electrical and mechanical connection without shorting
or grounding the connection or damaging circuit components.
D-54
-------
Knowledge Requirements
For each device to be maintained:
1. Knowledge of the name and location of each part or
component.
2. The location and function of each operating control.
3. The procedures for:
a. Installation
b. Servicing
c. Troubleshooting
d. Repair
e. Calibration
f. Operation
4. Knowledge of the tools, test instrumentation, supplies
and materials necessary to perform the various procedures
and where they are stored.
Special Staffing Guidance
The skills and knowledge required for this task are similar to
those required for the operation and maintenance of the various analyzers
described under Air Monitoring (see Volume E) and the same person could
perform some, all, or some combination of these tasks.
D-55
-------
Supervision of Laboratory Support Tasks
Task Overview
The function of lab task supervision is to direct, support, and evaluate
the performance of the analysis and maintenance tasks carried out by
the Chemical Laboratory Technicians and Equipment Technicians. The Supervisor
further serves as an interface between the lab personnel and the users
of lab services in other parts of the agency (e-g-> air monitoring and
source testing personnel) coordinating routine and special request
analysis and advising users on proper sampling techniques.
f
Occupational Category: Chemist
Task Description
The procedure for supervising lab support tasks cannot be set down
in a step-by-step sequence but involves various steps which are
performed as often as the supervisor deems necessary in achieving
timely and high quality results. These steps include:
1. Initiate the performance of the sampling and analysis
activities or assure that the activities are performed as
scheduled. This includes making work assignments,
2. Supervise the conduct of the activities, providing assistance
as required.
3. Advise of special problems or contingencies which might
affect when and how the activities are performed in. a given
instance (e.g., the need for non-scheduled sampling or the
temporary presence of an interferent, the effect of which
must be overcome or allowed for by special procedures).
4. Review the written report of the analyses for inconsistencies,
mistakes, variations from the procedure, etc.
D-56
-------
5. Work with professional level staff from other parts of the
agency in planning and scheduling non-routine analysis
(e.g.,. stack test analysis).
6. Assure that records of all analyses are in proper form,
complete, and correctly filed.
7. Provide on-the-job training for all tasks in support of
or in lieu of formal training provided elsewhere.
Skill Requirements
1. Ability to evaluate the quantity and quality of work produced
by the staff and discriminate acceptable from unacceptable
performance. This skill assumes the ability to use criteria
of performance acceptability for all tasks supervised.
2. Ability to make work assignments and establish and maintain
work schedules such that deadlines are met consistently.
3. Ability to develop work procedures which provide detailed
step-by-step guidance in the performance of the analysis
and instrument maintenance tasks.
4. Ability to document all procedures, findings, ideas, and
decisions in writing which communicates clearly and completely
to the intended audience, (e.g., Chemical Laboratory Technicians
and Equipment Technicians).
5. Ability to effectively communicate verbally with Chemical
Laboratory Technicians and Equipment Technicians concerning
details of task performance.
6. Ability to co-operate with air monitoring and source testing
personnel in planning tests so as to assure proper co-ordination
of analysis and sample collection activities.
7. Ability to express technical theory and data in a concise,
intelligent manner.
D-57
-------
8. Ability to choose a sampling time length and flow rate in
accordance with requirements for sample reliability and
representativeness and to avoid overloading the capacity
of the various reagents, filters, traps, etc., in the
sampling train.
9. Ability to determine the extent to which equipment and
instrument installation, troubleshooting, maintenance, and
calibration should be performed by agency personnel given:
a. The frequency with which these functions must be per-
formed.
te
b. The availability of the required skills and knowledge
in-house or the cost of providing them through training
or selection.
c-. The availability of the required test instruments,
tools, and materials or the cost of providing them.
d. The cost and delay associated with having some part
of these functions performed outside the agency.
10. Ability to calculate a reasonable estimate of the total amount
of moisture expected to be condensed from the gas sampled.
Knowledge Requirements
1. Knowledge of the capabilities and work loads of the personnel
under his direction sufficient to permit the making of work
assignments.
2. Knowledge of the sampling and analysis procedures, reagents,
apparatus, and calculations for all analyses normally performed.
3. Knowledge of the theoretical background for the analyses and
instruments of concern.
4. Knowledge of the service, maintenance, and calibration
requirements of all lab instruments of concern.
D-58
-------
5. Knowledge of the limitations associated with the analysis
techniques being employed including:
a. Range of ambient concentration of the pollutant
for which the technique can be employed and means
of modifying its sensitivity.
b. Other constituents which interfere with the accuracy
of the technique and methods for controlling their
effect.
c. Shelf life of the sample and correction for aged samples.
d. Critical aspects of the technique (e.g., the need for
nitrate-free water or the porosity requirements of
the fritted bubbler) and means of assuring that these
aspects are adequately provided for.
6. Knowledge of American Chemical Society reagent grade system
and the effects of typical reagent impurities on the outcome
of the analysis of concern.
7. Knowledge of factors surrounding the choice of appropriate
sampling- technique (e.g., the use of direct sampling,
syringes, grab bottles, etc.).
8. Knowledge of each source which is pertinent to identifying
analytical methodology, its use and location.
9. Knowledge of the meaning of the following terms which are
used in the evaluation of a method:
a. Validity
b. Reliability
c. Accuracy
d. Precision
D-59
-------
10. Knowledge of hazards involved with performing specific types
of analytical tasks, such as:
a. Presence of volatile or explosive chemicals
b. Poisonous substances
c. High temperatures or pressures
11. Knowledge of proper analytical laboratory procedures for
obtaining valid results.
12. Knowledge of relevant factors sufficient to permit the
development and periodic revision of a sampling schedule
f
giving the times, durations, and locations of sampling for each
ambient air sampling and analysis procedure to be employed.
Relevant factors affecting the schedule include:
a. Agency policy
b. Current pollution levels
c. Expected pollution levels
d. Changes in the set of pollutants for which analyses
are routinely performed
e. Changes in sampling or analysis procedures
f. Initiation of experimental monitoring programs
13. Knowledge of the relevant factors sufficient to permit the
establishment and periodic revision of the sample flow rate
to be maintained in the various sampling procedures. Relevant
factors.affecting flow rate include:
a. Instrument manufacturers* recommendations
b. Expected pollutant concentrations
c. Efficiency of the sample and analyses processes
D-60
-------
14. Knowledge of the analysis procedures sufficient to:
a. Identify errors possible in each step of the procedure
and their effect on the final outcome of the analysis.
b. Identify critical steps in the procedure. A critical
step is one in which
(1) Errors are known to frequently occur
(2) Little margin for error exists
(3) Errors are likely to go undetected
c. Revise procedures so as to reduce the possibility of
error.
15. Knowledge of the chemical, electrical, and mechanical principles
of operation of the various analysis instruments sufficient to:
a. Identify instrument malfunctions which could go undetected
and result in inaccurate read-out (to the extent not
already documented in existing service manuals).
b. Develop procedures for the timely discovery of such
malfunctions.
c. Identify the effects of incorrect instrument operation
on instrument read-out.
16. Knowledge of the theoretical basis of stack testing procedures.
17. Knowledge of the procedure for determining the chemical com-
position (percent CCL, CO, 0«, and N_) of stack gas.
18. Ability to design a sampling train which is appropriate for
a specific stack test with regard to the following criteria:
a.. Stack temperature.
b. Particle size.
c. Moisture content of gas.
d. Corrosive nature of the gas.
e. Type of analysis to be performed.
D-61
-------
19 Knowledge of the procedure for calculating the expected
sample weight.
20. Knowledge of the procedure for selecting an appropriate
filtering media, given the expected sample weight, stack
temperature, and the moisture content of the gas.
21. Knowledge of the efficiency, use restrictions, advantages,
and disadvantages of each type of filtering media.
22. Knowledge of the procedure for selecting an appropriate
condenser, based on the expected quantity of condensed moisture
and cooling requirements for preventing further condensation.
-------
5. Environmental Protection Agency. Standards of performance for
new stationary sources. Federal Register, Volume J6j Number 159,
August 17, 1971.
6. Haaland, H. H. (Ed.) Methods for determination of velocity,
dust and mist content of gases. Bulletin WP-50. Seventh
Edition. Los Angeles: Western Precipitation Division/Joy
Manufacturing Company, 1968.
7. Jacobs, M. B. The chemical analysis of air pollutants. New
York: Interscience Publishers, Inc., 1960. pp. 140-155.
8. Joy Manufacturing Company, Western Precipitation Division.
Gas velocity and dust determination equipment. Catalog GV22.
Los Angeles: Author.
9. Kimura, G. Emission control of flue-fed incinerators by use
of air pollution control devices. Chicago: Department of
Air Pollution Control, City of Chicago, November 1969. pp. 87-90.
10. PEDCo-Environmental Specialists, Inc. Administrative and
technical aspects,of source sampling for ^articulates.
Contract No. CPA 70-124. Research Triangle Park, North
Carolina: Environmental Protection Agency, May 1971.
11. Weisburd, M. (Ed.) Air pollution control field operations
manual. A guide for inspection and enforcement. Washington,
D. C.: U. S. Department of Health, Education, and Welfare;
Public Health Service, Division of Air Pollution, 1962.'
PHSP #937. pp. 167-76.
Special Staffing Guidance
The supervisor should be able to perform all the analyses and main-
tenance tasks performed by the Equipment Technicians and Chemical
Laboratory Technicians under his supervision. But.he needs, in addition,
D-63
-------
familiarity with general laboratory techniques, the theoretical back-
ground of the analyses to be performed and the principles of operation
of the laboratory instruments used. A Bachelor's Degree in Chemistry
will provide many of the required skills and knowledge. It also should
provide the background necessary for using technical literature and
interaction with other Chemists to fill any skill and knowledge gaps.
D-64
-------
Development of New Methods
for the Analysis of Air Pollutants
Task Overview
Development of new analytical methods is a task which is found to occur
frequently only in the older and larger agencies. It is a task which is
difficult to describe in terms of steps, since it may involve different
procedures adapted to solve different types of problems. For instance,
a "new" method may simply involve a modification of an off-the-shelf
instrument or it may involve an entirely unique approach to the measure-
ment of air pollutants. The following task description identifies some
of the typical requirements for method development.
Occupational Category: Chemist (Senior)
Task Description
1. Define the problem in terms of:
a. What pollutant is to be measured.
b. Requirements for precision and accuracy.
c. Budget restrictions.
2. Investigate literature and personnel sources for existing methods
of measurement pertaining to the pollutant. Possible sources
include:
a. Journals - air pollution control, analytical chemistry,
occupational health.
b. Technical magazines.
c. Textbook materials.
d. Environmental Protection Agency.
e. Colleagues in other agencies and universities.
f. Manufacturers of analytical instruments.
D-65
-------
3. Evaluate each method and Identify deficiencies according to
the following criteria:
a. Does the method provide a valid and reliable measurement
of the pollutant?
b. Does the method meet the requirements for precision and
accuracy?
c. Are there interferences from other pollutants?
d. Is the method cost/effective and within the budget
restrictions?
e. Is the method extremely hazardous?
4. If there are no existing methods which can be used or modified
in order to measure the pollutant, then construct an entirely
new method. This method must be based on physical or chemical
properties of the pollutant, which might include:
a. Spectrographic emission.
b. Flourescence.
c. Molecular structure.
d. Spectrophotometric absorption.
e. Reactions with other compounds.
f. lonizatlon.
g. Chromatographic properties.
5. Choose the best suited method based on the evaluation criteria
described in Step 3.
6. Obtain the necessary reagents and apparatus and place the
method into a trial operation.
7. Observe the method in operation and identify unanticipated
difficulties, e.g., inadequate filter media in a sampling
train, or possibly an insufficient peak separation on a
chromatogram.
D-66
-------
8. Modify the method in order to compensate for the shortcomings
identified.
9. Continue to test and modify the method until it meets the
original requirements for measurement of the pollutant.
10. Develop a procedure for performing the new analysis such
that a determination can be made of the problem which might
arise in putting the technique into practice (e.g., special
training required or unusual hazards present).
Skill Requirements
e
1. Ability to read, understand, interpret, and criticize technical
ddcuments which describe analytical chemistry laboratory techniques,
2. Ability to locate technical literature using abstracts and author
or subject indexes.
3. Ability to effectively communicate with knowledgeable persons
on the subject of analytical chemistry.
4. Ability to apply the knowledge of physical and chemical
properties of pollutants, along with the knowledge of proper
analytical procedure, to a new situation.
5. Ability to perform analytical laboratory procedures. This
may. include:
a. Construction of apparatus.
b. Sampling.
c. -Preparation of reagents.
d. Operation of analytical instruments.
e. Mathematical or statistical calculations.
This skill is at least a composite of the skills required by
the Chemical Laboratory Technician in the performance of the
various analyses (see Pages D-4 through D-51).
D-67
-------
6. Ability to identify and correct procedural difficulties which
might affect the overall adequacy of a method.
7. Ability to develop a detailed step-by-step work procedure for
the performance of the new analysis sufficient to permit the
determination of the skills and knowledge required in carrying
it out. Ability to evaluate the practicalities of the new
technique based on:
a. Required skills and knowledge not now possessed by
laboratory staff.
b. Unusual or extreme hazards.
c. Complexity of the procedure.
d. Overlong performance times.
e. Steps in the procedure which have little margin for
error (e.g., require extremely precise measurement).
Knowledge Requirements
1. Knowledge of each source which is pertinent to identifying
analytical methodology, its use and location.
2. Knowledge of the meaning of the following terms which are
used in the evaluation of a method:
a. Validity
b. Reliability
c. Accuracy
d. Precision
3. Knowledge of hazards involved with performing specific types
of analytical tasks, such as:
a. Presence of volatile or explosive chemicals.
b. Poisonous substances.
c. High temperatures or pressures.
D-68
-------
4. Knowledge of chemical and physical properties of pollutants
and how they can be manipulated and recorded so as to provide
a unique indication of the presence and concentration of a
specific pollutant. This requires extensive knowledge of:
a. Atomic and molecular structure.
b. Chemical reactions.
c. Electro-chemical reactions.
d. Reaction of atoms to excitation caused by burning,
light, or X-rays.
. '.. t
e. Other chemical or physical properties.
5. Knowledge of proper analytical laboratory procedures for
obtaining valid results.
6. Knowledge of the limitations associated with the analysis
techniques being employed including:
a. Range of ambient concentration of the pollutant for
which the technique can be employed and means of
modifying its sensitivity.
b. Other constituents which interfere with the accuracy
of the technique and methods for controlling their
effect.
c. Shelf life of the sample and correction for aged
samples.
d. Critical aspects of the technique (e.g., the need for
nitrate-free water or the porosity requirements of the
fritted bubbler) and means of assuring that these
aspects are adequately provided for.
7. Knowledge of American Chemical Society reagent grade system
and the effects of typical reagent impurities on the outcome
of the analysis of concern.
D-69
-------
8. Knowledge of factors surrounding the choice of appropriate
sampling technique (e.g., the use of direct sampling,
syringes, grab bottles, etc.)
Special Staffing Guidance
This task requires a broad background of theory and technique in analytical
chemistry much greater than that required for the day-to-day supervision
of routine analyses. A thorough familiarity with existing techniques
for analysis of air pollutants is, however, required to provide a
basis for comparing the advantages and disadvantages of new methods.
A familiarity with agency resources is also required to properly
evaluate new methods. This implies that the person to whom this task
is assigned should:
a. Be experienced in performing and supervising the standard
analyses.
b. Have a thorough knowledge of the capabilities and limitations
of the laboratory staff and equipment and budget restrictions
affecting the possibility of increasing such capability.
c. Have advanced education and/or experience in the theory and
techniques of analytical chemistry involving air pollutants.
It is for these reasons that the assignee be a senior Chemist.
D-70
------- |