EPA-600/4-77-027b
August 1977
QUALITY ASSURANCE HANDBOOK
FOR
AIR POLLUTION MEASUREMENT SYSTEMS
Volume III — Stationary Source Specific Methods
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Environmental Monitoring and Support Laboratory
Research Triangle Park, North Carolina 27711
-------
ACKNOWLEDGMENTS
This volume of the Quality Assurance Handbook has been
prepared by the Quality Assurance Branch of the Environmental
Monitoring and Support Laboratory, Research Triangle Park, North
Carolina in cooperation with PEDCo-Environmental, Inc., of
Cincinnati, Ohio.
DISCLAIMER
Mention of trade names or commercial products does not
constitute EPA endorsement or recommendation for use.
-------
VOLUME III
Revision No. 1
Date January 15, 1981
Page 1 of 4
TABLE OF CONTENTS
Section
Pages
5
PURPOSE AND OVERVIEW OF THE
QUALITY ASSURANCE HANDBOOK
3.0 GENERAL ASPECTS OF QUALITY
ASSURANCE FOR STATIONARY
SOURCE EMISSION TESTING
PROGRAMS
3.0.1 Planning the Test Program 19
3.0.2 General Factors Involved 5
in Stationary Source
Testing
3.0.3 Chain-of-Custody Procedure 13
for Source Sampling
3.0.4 Traceability Protocol for 9
Establishing True Concen-
tration of Gases Used For
Calibration and Audits of
Continuous Source Emission
Monitors (Protocol No. 1)
3.1 METHOD 2--DETERMINATION OF STACK
GAS VELOCITY AND VOLUMETRIC FLOW
RATE
3.1.1 Procurement of Apparatus 15
and Supplies
3.1.2 Calibration of Apparatus 21
3.1.3 Presampling Operations 7
3.1.4 On-Site Measurements 12
3.1.5 Postsampling Operations 3
3.1.6 Calculations 4
3.1.7 Maintenance 1
3.1.8 Auditing Procedure 5
3.1.9 Recommended Standards for 1
Establishing Traceability
3.1.10 Reference Method 11
3.1.11 References 2
3.1.12 Data Forms 8
Revision
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Date
1-15-81
5-01-79
5-01-79
5-01-79
6-15-78
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
1-15-80
-------
Revision No. 1
Date January 15, 1981
Page 2 of 4
TABLE OF CONTENTS (continued)
Section Paqes Revision Date
3.2 METHOD 3--DETERMINATION OF CARBON
DIOXIDE, OXYGEN, EXCESS AIR, AND
DRY MOLECULAR WEIGHT
3.2.1 Procurement of Apparatus 15 0 1-15-80
and Supplies
3.2.2 Calibration of Apparatus 4 0 1-15-80
3.2.3 Presampling Operations 6 0 1-15-80
3.2.4 On-Site Measurements 12 0 1-15-80
3.2.5 Postsampling Operations 2 0 1-15-80
3.2.6 Calculations 3 0 1-15-80
3.2.7 Maintenance 1 0 1-15-80
3.2.8 Auditing Procedure 5 0 1-15-80
3.2.9 Recommended Standards for 1 0 1-15-80
Establishing Traceability
3.2.10 Reference Method 3 0 1-15-80
3,2.11 References 1 • 0 1-15-80
3.2.12 Data Forms 6 0 1-15-80
3.3 METHOD 4—DETERMINATION OF
MOISTURE IN STACK GASES
3.3.1 Procurement of Apparatus 9 0 1-15-80
and Supplies
3.3.2 Calibration of Apparatus 19 0 1-15-80
3.3.3 Presampling Operations 7 0 1-15-80
3.3.4 On-Site Measurements 10 0 1-15-80
3.3.5 Postsampling Operations 4 0 1-15-80
3.3.6 Calculations 8 0 1-15-80
3.3.7 Maintenance 3 0 1-15-80
3.3.8 Auditing Procedure 4 0 1-15-80
3.3.9 Recommended Standards for 1 0 1-15-80
Establishing Traceability
3.3.10 Reference Method 5 0 1-15-80
3.3.11 References 1 0 1-15-80
3.3.12 Data Forms 14 0 1-15-80
3.4 METHOD 5--DETERMINATION OF PAR-
TI CULATE EMISSIONS FROM STATIONARY
SOURCES
3.4.1 Procurement of Apparatus 15 0 1-15-80
and Supplies
3.4.2 Calibration of Apparatus 22 0 1-15-80
3.4.3 Presampling ,Operations 20 0 1-15-80
3.4.4 On-Site Measurements 19 0 1-15-80
3.4.5 Postsampling Operations 15 0 1-15-80
-------
Revision No. 1
Date January 15, 1981
Page 3 of 4
TABLE OF CONTENTS (continued)
Section Pages Revision Date
3.4.6 Calculations 10 0 1-15-80
3.4.7 Maintenance 3 0 1-15-80
3.4.8 Auditing Procedure 7 0 1-15-80
3.4.9 Recommended Standards for 1 0 1-15-80
Establishing Traceability
3.4.10 Reference Method 6 0 1-15-80
3.4.11 References 2 0 1-15-80
3.4.12 Data Forms 21 0 1-15-80
3.5 METHOD 6—DETERMINATION OF
SULFUR DIOXIDE EMISSIONS FROM
STATIONARY SOURCES
3.5.1 Procurement of Apparatus 15 0 5-01-79
and Supplies
3.5.2 Calibration of Apparatus 15 0 5-01-79
3.5.3 Presampling Operations 6 0 5-01-79
3.5.4 On-Site Measurements 12 0 5-01-79
3.5.5 Postsampling Operations 16 0 5-01-79
3.5.6 Calculations 6 0 5-01-79
3.5.7 Maintenance 3 0 5-01-79
3.5.8 Auditing Procedure 7 0 5-01-79
3.5.9 Recommended Standards for 1 0 5-01-79
Establishing Traceability
3.5.10 Reference Method 3 0 5-01-79
3.5.11 References 2 0 5-01-79
3.5.12 Data Forms 13 0 5-01-79
3.6 METHOD 7—DETERMINATION OF
NITROGEN OXIDE EMISSIONS FROM
STATIONARY SOURCES
3.6.1 Procurement of Apparatus 13 0 5-01-79
and Supplies
3.6.2 Calibration of Apparatus 7 0 5-01-79
3.6.3 Presampling Operations 9 0 5-01-79
3.6.4 On-Site Measurements 11 0 5-01-79
3.6.5 Postsampling Operations 14 0 5-01-79
3.6.6 Calculations 6 0 5-01-79
3.6.7 Maintenance 2 0 5-01-79
3.6.8 Auditing Procedure 8 0 5-01-79
3.6.9 Recommended Standards for 1 0 5-01-79
Establishing Traceability
3.6.10 Reference Method 3 0 5-01-79
3.6.11 References 2 0 5-01-79
3.6.12 Data Forms 16 0 5-01-79
-------
Revision No. 1
Date January 15,
Page 4 of 4
1981
Section
TABLE OF CONTENTS (continued)
Pages
Revision
3.7
METHOD 8--DETERMINATION OF
SULFURIC ACID MIST AND SULFUR
DIOXIDE EMISSIONS FROM STATIONARY
SOURCES
3.7.1 Procurement of Apparatus 13
and Supplies
3.7.2 Calibration of Apparatus 20
3.7.3 Presampling Operations 7
3.7.4 On-Site Measurements 18
3.7.5 Postsampling Operations 17
3.7.6 Calculations 10
3.7.7 Maintenance 3
3.7.8 Auditing Procedure 7
3.7.9 Recommended Standards for 1
Establishing Traceability
3.7.10 Reference Method 4
3.7.11 References 1
3.7.12 Data Forms 20
METHOD 10--DETERMINATION OF CARBON
MONOXIDE EMISSIONS FROM STATIONARY
SOURCES
METHOD 13B—DETERMINATION OF TOTAL
FLUORIDE EMISSIONS FROM STATIONARY
SOURCES (SPECIFIC-ION ELECTRODE
METHOD)
3.10 METHOD ISA—DETERMINATION OF TOTAL
FLUORIDE EMISSIONS FROM STATIONARY
SOURCES (SPADNS ZIRCONIUM LAKE
METHOD)
3.11 METHOD 17--DETERMINATION OF
PARTICULATE EMISSIONS FROM
STATIONARY SOURCES (IN-STACK
FILTRATION METHOD)
3.8
3.9
0
0
0
0
0
0
0
0
0
0
0
0
Date
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
5-01-79
Currently under
development
Currently under
development
Currently under
development
Currently under
development
-------
Revision No. 1
Date January 15, 1981
Page 1 of 5
PURPOSE AND OVERVIEW OF THE QUALITY ASSURANCE HANDBOOK
The purpose of this Quality Assurance Handbook for Air
Pollution Measurement Systems is to provide guidelines and
procedures for achieving quality assurance in air pollution
measurement systems. It is intended to serve as a resource
document for the design of quality assurance programs and to
provide detailed method descriptions for certain measurement
processes that can be used directly in implementing the quality
assurance program.
This Handbook should be particularly beneficial to opera-
tors, project officers, and program managers responsible for
implementing, designing, and coordinating air pollution emission
source tests. The contents of each volume are briefly described
in the following paragraphs.
Volume I - Principles
Volume I contains brief discussions of the elements of
quality assurance. Expanded discussions of technical points and
sample calculations are included in the Appendixes. The discus-
sion of each element is structured to be brief and to highlight
the most important features. Organizations developing and
implementing their own quality assurance plans will find Volume
I useful for general guidance.
Volume II - Ambient-Air-Specific Methods
Volume II contains quality assurance guidelines on ambient
air measurement systems. Regardless of the scope and magnitude
of ambient air measurement systems, there are a number of common
considerations pertinent to the production of quality data.
These considerations are discussed in Section 2.0 of Volume II,
and include quality assurance guidelines in the areas of:
-------
Revision No. 1
Date January 15, 1981
Page 2 of 5
1. Sampling network design and site selection - monitor-
ing objectives and spatial scales; representative sampling;
meteorological and topographical constraints; and sampling
schedules.
2. Sampling considerations - environmental controls;
probe and manifold design; maintenance; and support services.
3. Data handling and reporting considerations - data
recording systems, data validation, and systematic data manage-
ment.
4. Reference and equivalent methods.
5. Recommended quality assurance program for ambient air
measurements.
6. Chain-of-custody procedure for ambient air samples -
sample collection; sample handling; analysis of the sample;
field notes; and report as evidence.
7. Traceability protocol for establishing true concen-
trations of gases used for calibrations and audits - establish-
ing traceability of commercial gas cylinders and of permeation
tubes.
8. Calculations to assess monitoring data for precision
and accuracy for SLAMS and PSD automated analyzers and manual
methods.
9. Specific guidance for a quality control program for
SLAMS and PSD for automated analyzers and manual methods -
analyzer selection, calibration, zero and span checks; data
validation and reporting; quality control program for gaseous
standards and flow measurement devices.
10. EPA national performance audit program.
11. System audit criteria and procedures for ambient air
monitoring programs.
12. Audit procedures for use by State and local air moni-
toring agencies.
The remainder of Volume II contains method and/or principle
description and quality assurance guidelines for specific pollu-
tants. Each pollutant-specific section contains the following
information.
-------
Revision No. 1
Date January 15, 1981
Page 3 of 5
1. Procedures for procurement of equipment and supplies.
2. Calibration procedures.
3. Step-by-step descriptions of sampling, reagent prepa-
ration, and analysis procedures, as appropriate, depending upon
the method or principle in the case of equivalencies.
4. Method of calculation and data processing checks.
5. Maintenance procedures.
6. Recommended auditing procedures to be performed during
the sampling, analysis, and data processing.
7. Recommended procedure for routine assessment of accu-
racy and precision.
8. Recommended standards for establishing traceability.
9. Pertinent references.
10. Blank data forms for the convenience of the Handbook
user (data forms are partially filled in within the text for
illustration purposes).
Matrix tables at the ends of appropriate sections summarize
the quality assurance functions therein. Each matrix includes
the activities, the acceptance limits, method and frequency of
the each quality assurance check, and the recommended action if
the acceptance limits are not satisfied.
Volume II contains quality assurance guidelines for pollu-
tant-specific measurement systems. The measurement systems
planned for Volume II include:
1. Reference Method for the Determination of Sulfur Diox-
ide in the Atmosphere (Pararosaniline Method).
2. Reference Method for the Determination of Suspended
Particulates in the Atmosphere (Hi-Vol Method).
3. Reference Method for the Determination of Nitrogen
Dioxide in the Atmosphere (Chemiluminescence).
4. Equivalent Method for the Determination of Nitrogen
Dioxide in the Atmosphere (Sodium Arsenite).
5. Equivalent Method for the Determination of Sulfur
Dioxide in the Atmosphere (Flame Photometric Detector).
-------
Revision No. 1
Date January 15, 1981
Page 4 of 5
6. Reference Method for the Determination of Carbon
Monoxide in the Atmosphere (Nondispersive Infrared Spectrome-
try).
7. Reference Method for the Determination of Ozone in the
Atmosphere (Chemiluminescence).
8. Reference Method for the Determination of Lead in
Suspended Particulate Matter Collected from Ambient Air (Atomic
Absorption Spectrometry).
9. Method for the Determination of Sulfates in the Atmos-
phere (Methythymol Blue Automated Analysis).
As methods are added to Volume II, these will be sent to
Handbook users through the document control system, as described
in Section 1.4.1 of Volume I of this Handbook.
Volume III - Stationary-Source-Specific Methods
Volume III contains quality assurance guidelines on sta-
tionary-source-specific methods. The format for Volume III is
patterned after that of Volume II.
Regardless of the scope and purpose of the emissions-test-
ing plan, there are a number of general considerations pertinent
to the production of quality data. These considerations are
discussed in Section 3.0 of Volume III and include quality
assurance guidelines in the areas of:
1. Planning the test program - preliminary plant survey;
process information; stack data; location of sampling points;
cyclonic gas flow.
2. General factors involved in stationary source test-
ing -tools and equipment; standard data forms; and identifica-
tion of samples.
3. Chain-of-custody procedures for source sampling -
sample collection; sample analysis; field notes; and report as
evidence.
4. Traceability protocol for establishing true concentra-
tions of gases used for calibrations and audits of air pollution
analyzers - establishing traceability of commercial gas cylin-
ders.
-------
Revision No. 1
Date January 15, 1981
Page 5 of 5
The remainder of Volume III contains quality assurance
guidelines for specific measurement methods. The measurement
systems planned for Volume III include:
Method 2 -
Determination of Stack Gas Velocity and Volumet-
ric Flow Rate (Type-S Pitot Tube).
Gas Analysis for Carbon Dioxide, Oxygen, Excess
Air, and Dry Molecular Weight.
Determination of Moisture in Stack Gases.
Determination of Particulate Emissions from Sta-
tionary Sources.
Determination of Sulfur Dioxide Emissions from
Stationary Sources.
Determination of Nitrogen Oxide Emissions from
iStationary Sources.
Determination of Sulfuric Acid Mist and Sulfur
Dioxide from Stationary Sources.
Determination of Carbon Monoxide Emissions from
Stationary Sources.
Determination of Fluoride Emissions from Station-
ary Sources (SPADNS and Specific Ion Electrode).
Determination of Particulate Emissions from Sta-
tionary Sources (In-Stack Filtration Method).
As methods are added to Volume III, these will be sent to
the users through the document control system used for the Hand-
book.
Method 3 -
Method 4 -
Method 5 -
Method 6 -
Method 7 -
Method 8 -
Method 10 -
Methods 13A -
and 13B
Method 17
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 1 of 9
Section 3.1
METHOD 2 - DETERMINATION OF STACK GAS VELOCITY
AND VOLUMETRIC FLOW RATE
OUTLINE
Number of
Section Documentation Pages
SUMMARY 3.1 1
METHOD HIGHLIGHTS 3.1 7
METHOD DESCRIPTION
1. PROCUREMENT OF APPARATUS
AND SUPPLIES 3.1.1 15
2. CALIBRATION OF APPARATUS 3.1.2 21
3. PRESAMPLING OPERATIONS 3.1.3 7
4. ON-SITE MEASUREMENTS 3.1.4 12
5. POSTSAMPLING OPERATIONS 3.1.5 3
6. CALCULATIONS 3.1.6 4
7. MAINTENANCE 3.1.7 1
8. AUDITING PROCEDURE 3.1.8 5
9. RECOMMENDED STANDARDS
FOR ESTABLISHING TRACE-
ABILITY 3.1.9 1
10. REFERENCE METHOD 3.1.10 11
11. REFERENCES 3.1.11 2
12. DATA FORMS 3.1.12 8
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 2 of 9
SUMMARY
Method 2 outlines a procedure for determining stack gas
velocity and volumetric flow rate from stationary sources. A
Type S (stauscheibe or reverse) pitot tube or a standard pitot
tube meeting the criteria in Section 3.1.1, calibrated according
to the procedures outlined in Section 3.1.2, and operated in
accordance with Section 3.1.4 is used to measure velocity pres-
sure (Ap); this pressure measurement, along with gas density, is
used to determine the stack gas velocity.
If the minimum criteria of Method 1 are not met or if the
measurement site has a swirling or cyclonic gas stream, the pro-
cedures outlined in Method 2 for stack gas velocity and volu-
metric flow rate determination are not applicable. When unac-
ceptable flow conditions exist, alternative procedures such as
the use of flow-straightening devices or stack extensions must be
employed as necessary to make accurate flow rate determinations.
These alternative procedures are subject to approval by the ad-
ministrator.
The Method Description which follows is based on the Refer-
ence Method published August 18, 1977. A complete copy of the
Reference Method is contained in Section 3.1.10. Data forms are
provided in Section 3.1.12 for the convenience of the Handbook
user. Reference 1 was used extensively in preparing the Method
Description and the data forms. References 2, 3, 4, and 5 sum-
marize collaborative tests conducted to determine the usefulness
and accuracy of this method.
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 3 of 9
METHOD HIGHLIGHTS
Section 3.1 describes specifications for determination of
stack gas velocity and volumetric flow rate from stationary
sources. The sampling apparatus consists of a pitot tube and
a differential pressure gauge. Stack gas velocity and volumetric
flow rate can be determined in conjunction with other EPA Re-
ference Methods (i.e., Method 5) if the sampling components are
mounted in an interference-free manner.
The results of collaborative tests have shown that the pre-
cision of this test method is adequate for use with other test
methods in determining pollutant emission rates; collaborative
tests also showed that the method is not subject to large biases
2 5
from one user to another. '
The blank data forms at the end of the highlights section
may be removed from the Handbook and used in the pretest, test,
and posttest operations. Each form has a subtitle (e.g.,
Method 2, Figure 2.4) to assist the user in finding a similar
filled-in form in the Method Description (e.g., in Section
3.1.2). On the blank and filled-in forms, the items/parameters
that can cause the most significant errors are indicated with an
asterisk.
1. Procurement of Equipment
Section 3.1.1 (Procurement of Apparatus and Supplies) gives
the specifications, criteria, and design features for equipment
and materials required for performing Method 2 tests. The sam-
pling apparatus can be used in conjunction with sampling equip-
ment required for other methods such as Methods 5 and 8 pre-
sented in this Handbook. This section is designed as a guide in
the procurement and initial check of equipment and supplies. The
activity matrix (Table 1.1) at the end of Section 3.1.1 can be
used as a quick reference; it follows the same order as the
written description in the main text.
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 4 of 9
2. Pretest Preparations
Section 3.1.2 (Calibration of Apparatus) provides a step-
by-step description of the required calibration procedures.
Detailed methods and equipment are described for calibrating
pitot tubes in the laboratory and in the field. The calibration
section can be removed and compiled, along with calibration sec-
tions from all other methods, into a separate quality assurance
reference manual for use by calibration personnel. A pretest
checklist (Figure 3.1) or similar form should be used to sum-
marize the calibration data.
Section 3.1.3 (Presampling Operations) provides the tester
with a guide for supplies and equipment preparation for field
tests. The pretest preparation form (Figure 3.2) can be used as
an equipment checkout and packing list. The method for packing
and the description of packing containers should help to protect
the equipment, but are not required.
3. On-Site Measurements
Section 3.1.4 (On-Site Measurements) contains a step-by-step
procedure for performing velocity measurements. Precautions must
be taken to ensure that the pitot tube is aligned with the stack
gas flow. Also a check for cyclonic flow must be made. The
on-site measurement checklist (Figure 4.2) is provided to assist
the tester with a quick method of checking requirements.
4. Posttest Operations
Section 3.1.5 (Postsampling Operations) gives the posttest
equipment check procedures. Figure 5.1 or a similar form should
be used to summarize the posttest calibration checks, and should
be included in the emission test report.
Section 3.1.6 (Calculations) provides the tester with the
required equations, nomenclature, and the suggested number of
significant digits. It is suggested that a programmed calculator
be used if available to reduce the chance of calculation error.
Section 3.1.7 (Maintenance) provides the tester with a guide
for a routine maintenance program. This program is not required,
but should reduce equipment malfunctions.
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 5 of 9
5. Auditing Procedure
Section 3.1.8 (Auditing Procedure) provides a description
of necessary activities for conducting performance and system
audits. The performance audits of the data processing and a
systems audit of the on-site measurements should provide the
independent assessment of the quality of data needed.
Section 3.1.9 (Recommended Standards for Establishing
Traceability) recommends the primary standards to which the
working standards should be traceable.
6. References
Sections 3.1.10 and 3.1.11 contain the Reference Method and
the suggested references.
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 6 of 9
PRETEST SAMPLING CHECKS
(Method 2, Figure 3.1)
Date Completed by
Pitot Tube
Identification number Date
Dimension specifications checked?* yes no
Calibration required? yes no
Date C
P
Temperature Sensor
Identification number
Calibrated?* yes no
Was a pretest temperature correction used? yes no
If yes, temperature correction °C (°F)
Barometer
Was the pretest field barometer reading correct?* yes no
Differential Pressure Gauge
Was pretest calibration acceptable?* yes no
*Most significant items/parameters to be checked.
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 7 of 9
PRETEST PREPARATIONS
(Method 2, Figure 3.2)
Apparatus check
Pitot Tube
Type S
Standard
Length m(ft)
Calibrated*
Differential
Pressure Gauge
Inclined manom-
eter sensitivity
cm ( in. )
Other
Stack Temperature
Sensor
Type
Calibrated*
Orsat Analyzer
Orsat
Fyrite
Other
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Loaded
and packed
*Most significant items/parameters to be checked.
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 8 of 9
ON-SITE MEASUREMENTS CHECKLIST
(Method 2, Figure 4.2)
Sampling
Pitot tube, lines, and manometer assembled correctly?*
Pitot tube and components mounted in an interference free man-
ner?*
Differential pressure gauge has correct sensitivity?*
Differential pressure gauge leveled and zeroed?*
Pretest leak check?
(optional) Cyclonic flow checked?*
Pitot tube parallel to gas flow?*
Static pressure measured? Temperature measured?
Moisture content determined?
Orsat samples taken?
Method
If no, explain:
Posttest leak check performed?*
Data recorded properly?
(mandatory)
*Most significant items/parameters to be checked.
-------
Section No. 3.1
Revision No. 0
Date January 15, 1980
Page 9 of 9
POSTTEST SAMPLING CHECKS
(Method 2, Figure 5.1)
Pitot Tube
Initial pitot tube coefficient
Was pitot tube damaged prior to start of any test runs? yes
no
If yes, was pitot tube calibrated prior to repair?* yes no
Pitot tube coefficient (damaged) (this value must
be used for runs started with the damaged pitot tube)
Temperature Sensor
Was a pretest temperature correction used? yes ^ no
If yes, temperature correction °C (°F) (within 1.5%
of readings in K (°R) over range)
Average stack temperature of compliance test (T ) K (°R)
Temperature of reference thermometer or solution for recalibra-
tion* K (°R)
Temperature of stack thermometer for recalibration K (°R)
Difference between reference and stack thermometer temperatures
(AT ) K (°R)
Do values agree within ±1.5%?* yes no
If yes, no correction necessary for calculations
If no, calculations must be done twice, once with recorded,
values and once with average stack temperature corrected to
correspond to reference temperature differential (AT ). Both
values of final results must then be reported since there is no
way to determine which is correct
Barometer
Was pretest field barometer reading correct? yes r_ no
Posttest comparison mm (in.) Hg (within ±5.0 mm (0.2 in.)
Hg of mercury-in-glass barometer)
Was recalibration required? yes no
If yes, no correction needed when field barometer has the lower
reading
If mercury-in-glass reading is lower, subtract the difference
from the field data readings for the calculations
*Most significant items/parameters to be checked.
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 1 of 15
1.0 PROCUREMENT OF APPARATUS AND SUPPLIES
Figure 1.1 shows a diagram of the Type S pitot tube-manom-
eter assembly used in this method. Specifications, criteria and/
or applicable design features are given in this section to aid in
the selection of equipment which will produce accurate data.
Selection procedures and applicable limits for acceptance checks
are also included. During procurement of equipment and supplies,
it is suggested that a procurement log (Figure 1.2) be used to
record the descriptive title of equipment; the identification
number, if applicable; and the results of the acceptance check.
Also, if calibration is required as part of the acceptance check,
the data are to be recorded in the calibration log book. Table
1.1 at the end of this section contains a summary of quality
assurance activities for procurement and acceptance of apparatus
and supplies.
1.1 Pitot Tube
A Type S pitot tube shown in Figure 1.1 is required. The
pitot tube should be constructed of metal tubing (e.g., 304 or
316 stainless steel) with an external tubing diameter (Dt) be-
tween 0.48 and 0.95 cm (3/16 and 3/8 in.). The major criteria in
pitot tube construction material are durability and corrosion
resistance. Upon receiving a new pitot tube, inspect it to
determine if it was constructed according to the configuration in
Figure 1.3. Repair, replace, or return to the manufacturer any
Type S pitot tube which does not meet the face opening specifica-
tions outlined in Figure 1.4. One method of inspecting the con-
struction details is as follows:
1. Obtain a section of angle aluminum approximately 20 cm
(8 in.) long by 1.3 x 2.5 cm (0.5 x i.o in.). Mount a bull's eye
level (with ±1° accuracy) to the angle aluminum, as shown in
Figure 1.5.
2. Place the pitot tube in the angle aluminum as shown in
Figure 1.5, and level the pitot tube as indicated by the bull's
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 2 of 15
1.90-2.54 CM
(0.75-1.0 IN.)
FLEXIBLE TUBING
6.25 MM (1/4 IN.)
TEMPERATURE SENSOR
TYPE S PITOT TUBE
*L - DISTANCE TO FURTHEST SAMPLING
POINT PLUS 30 CM (12 IN.)
**PITOT TUBE - TEMPERATURE SENSOR SPACING
Figure 1.1 Type S pitot tube-manometer assembly.
-------
Item description
?,+&T- hbe-
Quantity
/
Purchase
order
number
7i->/^3F
Vendor
Ace A^kl
Date
Ordered
9, /. - "79
/ 'f ' I
Cost
^2 ' ^ , /*-.
K'C<
Comments
*tJ O pd en
(V (U (D ft
ua rt < o
ro (t> H- rt
en H-
W (L| H- O
») ss
H O
CO
Figure 1.2 Example of a procurement log.
Ul
CX)
o
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 4 of 15
A-SIDE PLANE
LONGITUDINAL '
TUBE AXIS
y
\
Dt
f
A
B
NOTE:
PA
0.48 CM
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 5 of 15
TRANSVERSE
TUBE AXIS
LONGITUDINAL
TUBE AXIS
(e)
~i
(f)
(g)
Figure 1.4. Types of face-opening misalignment that can result
from field use or improper construction of Type S pitot tubes.
These will not affect Cp so long as a, and cu <10°, p7 <5°,
z <0.32 cm (1/8 in.) and w<0.08 cm (1/32 In.).
-------
ALUMINUM "L" ANGLE
SIDE
VIEW
END
VIEW
BULL'S EYE LEVEL-
ALUMINUM "L" ANGLE
PI TOT TUBE
PROBE
DEGREE INDICATING'
LEVEL
^SS&r ^Si
Figure 1.5 Type S pitot tube dimension specialization measurements
hj D 5d tn
CD ft) CD (^
vQ ft < O
0) rt> H- ft
V> H-
cn c-i H- o
H? o 3
033
Hi C 2
QJ 2; O
H- rj O •
l_j o •
Ul M
OO
O
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 7 of 15
eye level. A vise may be used to hold the angle aluminum and
pitot tube. Note: A permanently mounted pitot tube and probe
assembly may require a shorter section of angle aluminum to allow
proper mounting on the assembly.
3. Place a degree indicating level in the various posi-
tions, as illustrated in Figure 1.6.
4. Measure distances P and P,.
5. Measure the external tube diameter (D..) with a microm-
eter. Record all data on a data form such as Figure 1.7.
6. Calculate dimensions w and z using the following equa-
tions:
z = A sin y Equation 2-1
w = A sin 0 Equation 2-2
where,
z = alignment dimension, cm (in.)
w = alignment dimension, cm (in.)
A = distance between tips, (P_ + PK), cm (in.)
a D
y = angle in degrees
6 = angle in degrees.
Note; Pitot tubes with bent or damaged tubing may be difficult
to check using this procedure. If the Type S pitot tube meets
the face alignment criteria, an identification number should be
assigned and permanently marked or engraved on the body of the
tube.
A standard pitot tube (Figure 1.8) may be used instead of a
Type S for conducting velocity traverses. Upon receiving a new
standard pitot tube, inspect it to determine if it meets the fol-
lowing design criteria:
1. The tip is of the hemispherical (shown in Figure 1.8),
ellipsoidal, or conical design.
2. There is a minimum of six diameters straight run (based
upon D-,, the external diameter of the tube) between the tip and
static pressure holes.
-------
DEGREE INDICATING LEVEL POSITION
FOR DETERMINING 81 and 62
*
DEGREE INDICATING LEVEL
POSITION FOR DETERMINING
ai and 0,2
O jd en
PJ (T) (D
ri- < O
fl> H- rt
W H-
d, H'O
^03
o
Figure 1.6
Position of dimension measurement.
(continued)
3 O
O •
u>
00
O
-------
DEGREE INDICATING LEVEL POSITION
FOR DETERMINING y, THEN CALCULATING Z
DEGREE INDICATING LEVEL
POSITION FOR DETERMINING
0, THEN CALCULATING W
Figure 1.6 (continued)
nj o » %
to fa (D £
IQ ft- C_( H-2
&> o
033^
H.C 5
I-1 O
Ul
vo
oo
o
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 10 of 15
Pitot tube assembly level?
Pitot tube openings damaged?
yes
yes (explain below)
= O.O
Y = 3- 5 °, 0 =
, A =
cm (in.)
= A sin y = (p. 063} cm (in.); <0.32 cm (
-------
SECTION AA
1
r*~A
( D i — ;
t
L*-A
MANOMETER
CURVED OR
MITERED JUNCTION
90° BEND
STATIC
HOLES
(MJ.1D)
IN OUTSIDE
TUBE ONLY
HEMISPHERICAL TIP
IMPACT OPENING-
INNER TUBE ONLY
w o # w
ju JU 0> (D
*Q rt < O
(D (D H- ^
. 0) H-
Figure 1.8 Standard pitot tube design specifications.
CO
O
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 12 of 15
3. There is a minimum of eight diameters straight run
between the static pressure holes and the centerline of the
external tube, following the 90° bend.
4. The static pressure holes are of equal size (approxi-
mately 0.1 D), equally spaced in a piezometer ring configuration.
5. It has a 90° bend, with curved or mitered junction.
Repair, replace or return to the manufacturer any standard pitot
tube which does not meet the above criteria.
1.2 Differential Pressure Gauge
A liquid-filled inclined manometer or an equivalent device
should be used to measure the velocity head. Most preassembled
sampling trains are equipped with a 10-in. (water column) in-
clined-vertical manometer that has 0.01-in. divisions on the
0-to-l-in. inclined scale and 0.1-in. divisions on the 1-to-
10-in. vertical scale. This type manometer (or other gauge of
equivalent sensitivity) is satisfactory for measurements of Ap
values as low as 1.3 mm (0.05 in.) H20. However, a gauge of
greater sensitivity (e.g., with 6.4 mm (0.25 in.) H20 full scale)
is required for stacks with velocity pressures below 1.3 mm
(0.05 in.) H20.
Upon receipt of a new manometer, leak check it using the
following procedure:
1. Level and zero the manometer.
2. Vent both sides of the manometer to the atmosphere.
3. Place tygon tubing, or equivalent on the positive leg
of the manometer, and blow into the tubing to displace the liquid
to at least 30% of scale.
4. Close off the open end of the tubing, and observe the
manometer for 15 s. If there is no change in the reading, the
positive side of the manometer is leak free.
5. Repeat steps 3 and 4 for the negative side of the man-
ometer, but use suction to produce the manometer reading.
Repair, replace, or return to the manufacturer any manometer
which does not pass the leak check.
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 13 of 15
If differential pressure gauges other than inclined mano-
meters are used (e.g., magnehelic or electronic gauges), cali-
brate the gauges upon receipt using the procedure in Section
3.1.2.
1.3 Temperature Gauge
A thermocouple, liquid-filled bulb thermometer, or other
means capable of measuring temperature to within 1.5% of the
minimum absolute stack temperature is required. Upon receipt,
check the temperature gauge for damage, and then calibrate it
according to the procedure in Section 3.1.2.
1.4 Pressure Probe and Gauge
Leak-free tubing and a mercury-or water-filled U-tube manom-
eter capable of measuring stack pressure to within 2.5 mm (0.1
in. ) Hg is required. The static tap of a standard type pitot
tube or one leg of a Type S pitot tube with the face openings
positioned parallel to the gas flow may also be used as the
pressure probe. The differential pressure gauge used for veloc-
ity measurements can be used to measure static pressure.
Upon receipt of a U-tube manometer, leak check according to
the procedure in Subsection 1.1.2.
1.5 Barometer
A mercury, aneroid, or other barometer capable of measuring
atmospheric pressure to within 2.5 mm (0.1 in.) Hg is required.
Upon receipt of a new barometer, check it against a mercury-in-
glass barometer or the equivalent. If the barometer cannot be
adjusted to agree within 2.5 mm (0.1 in.) Hg of the reference
barometric pressure, it should be returned to the manufacturer.
1.6 Gas Analyzer
To analyze gas composition for determining dry molecular
weight of the gases from combustion or other unknown streams, use
Method 3. For processes emitting essentially air, use a dry
molecular weight of 29.0. Use Method 4 or Method 5 for moisture
content determinations.
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 14 of 15
1.7 Calibration Pitot Tube
Standard type, to calibrate the Type S pitot tube. The
standard type pitot tube should have a known coefficient obtained
from the National Bureau of Standards (NBS), Route 70 S, Quince
Orchard Road, Gaithersburg, Maryland, or the standard pitot tube
must be calibrated against another standard pitot tube with an
NBS-traceable coefficient. Alternatively, a standard pitot tube
designed according to the criteria given in Subsection 1.1.1 and
illustrated in Figure 1.8 may be used. Be sure to inspect the
standard type pitot tube for any damage upon receipt.
1.8 Differential Pressure Gauge
An inclined manometer or equivalent is used for Type S pitot
tube calibration. This should be an easily readable, sensitive
gauge for laboratory use. If the single-velocity calibration
technique is used (Section 3.1.2), the calibration differential
pressure gauge should be readable to the nearest 0.13 mm (0.005
in.) H20. For multivelocity calibrations, the gauge shall be
readable to the nearest 0.13 mm (0.005 in.) H20 for Ap values
between 1.3 and 25 mm (0.05 and 1.0 in.) H2O, and to the nearest
1.3 mm (0.05 in.) E^O for Ap values above 25 mm (1.0 in.) H20. A
special, more sensitive gauge will be required to read Ap values
below 1.3 mm (0.05 in.) H20. Visually check and leak check the
calibration differential pressure gauge upon receipt.
-------
Section No. 3.1.1
Revision No. 0
Date January 15, 1980
Page 15 of 15
Table 1.1 ACTIVITY MATRIX FOR PROCUREMENT OF APPARATUS
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
All apparatus
No visible damage
Visual check when
purchased
Return to
supplier
immediately
Pitot tube
(Type S or
equivalent)
See Figs 1.3 and 1.4
for acceptance limits
Measure dimensions
and alignment;
identify upon
receipt
Do not use
if alignment
is not within
limits; repair
or replace
Differential
pressure
gauge
No leaks
When purchased,
visually inspect
and leak check
Adjust or re-
turn to sup-
plier
Temperature
gauge
Capable of measuring
temperature within 1.5%
of minimum absolute
stack temperature
Calibrate according
to Section 3.1.2
Return to
supplier or
repair
Pressure probe
and gauge
Capable of measuring
stack pressure within
2.5 mm Hg (0.1 in.)
Hg; no leaks
Visual inspection
and leak check
Adjust to
correct for
error, or re-
turn to sup-
plier
Calibration
pitot tube
Meet design specifi-
cations with known
coefficient from
NBS, or see Sec 1.1
Visual check
Return to
supplier
Calibration
differential
pressure
gauge
No leaks; single point-
capable of measuring Ap
to within 0.13 mm
(0.005 in.) H20; multi-
point readable within
0.13 mm (0.005 in.)
H90 for Ap values be-
tween 1.3 and 25 mm
(0.05 and 1.0 in.) and
to nearest 1.3 mm
(0.05 in.) H20 for Ap
values >25 mm (110 in.);
special sensitivity for
values <1.3 mm (0.05
in.) H20
Visual check and
leak check
Repair or
replace
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 1 of 21
2.0 CALIBRATION OF APPARATUS
Calibration of apparatus is one of the most important func-
tions in maintaining data quality. The detailed calibration
procedures in this section are designed for the equipment speci-
fied by Method 2 and described in the previous section. A labo-
ratory log book of all calibrations must be maintained.
Table 2.1 at the end of this section summarizes the quality
assurance activities for calibration.
2.1 Type S Pitot Tube
A pitot tube that meets the face opening specifications in
Section 3.1.1 (Figures 1.3 and 1.4) and that has the following
dimensions—external tubing diameter (D. ) between 0.48 and 0.95
cm (3/16 and 3/8 in.) and Pa and Pn equal and between 1.05 and
£\ 13
1.50 D.—either may be assigned a baseline (isolated tube) coef-
ficient value of 0.84 or may be calibrated. Note, however, that
if the pitot tube is mounted on a probe thermocouple assembly and
if the components of the assembly do not meet the interference
free criteria in (Subsection 2.1.1), calibration will be required
despite knowledge of the baseline coefficient value.
If D. , P , and P_ are outside the specified limits, the
pitot tube must be calibrated as outlined in Subsection 2.1.2.
2.1.1 Pitot Tube Assemblies - Interference-free assemblies—that
is, pitot tubes mounted with a temperature sensor, probe, and
nozzle—are shown in Figures 2.1 and 2.2. When the pitot tube
meets the previously described dimensions and specifications and
is mounted according to the specifications in Figures 2.1 and
2.2, no calibration is required and the baseline (isolated tube)
coefficient of 0.84 may be used. Dimensions of the pitot tube -
probe sampling assembly must be carefully measured with an in-
ternal caliper or a steel machinist's rule.
Note; Only pitot tubes constructed of 0.48 to 0.95 cm (3/16 to
3/8 in.) tubing can be used in interference-free assemblies. All
other assemblies must be calibrated.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 2 of 21
TYPE S PITOT TUBE
I
" x > 1.90 cm (3/4 in.) for D' = 1.3 cm (1/2 in.)
>f "
SAMPLING NOZZLE
(a) BOTTOM VIEW: SHOWING MINIMUM PITOT-NOZZLE SEPARATION.
SAMPLING NOZZLE
SAMPLING PROBE
FD:
I
TYPE S PITOT TUBE ,
STATIC PRESSUR'E
'OPENING
IMPACT PRESSURE
OPENING
NOZZLE OPENING
(b) SIDE VIEW: TO PREVENT PITOT TUBE FROM INTERFERING WITH
GAS FLOW STREAMLINES APPROACHING THE NOZZLE, THE IMPACT
PRESSURE OPENING PLANE OF THE PITOT TUBE SHALL BE EVEN
WITH OR DOWNSTREAM FROM THE NOZZLE ENTRY PLANE
Figure 2.1 Required pitot tube-sampling nozzle configuration
to prevent aerodynamic interference; buttonhook-type nozzle;
centers of nozzle and pitot opening aligned; in respect to flow
direction, Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
-------
W >_ 7.62 cm
! (3 in.)|
'« »•
Z > 5.08 era
I(2 in.)|
THERMOCOUPLE
£
tz > 1.90cm(3/4 in.)
THERMOCOUPLE
I Dt
TYPE S PITOT TUBE
OR
TYPE S PITOT TUBE
SAMPLE PROBE
SAMPLE PROBE
Y > 7.62 cm (3 in.)
Figure 2.2 Required thermocouple and probe placement to prevent
interference: D. between 0.48 and 0.95 cm (3/16 and
3/8 in.).
n^ & CD CD
id r+ < o
CD CD H- ft
w p-
co M p- o
SOP
0^3
i-1 o
I-1
00
o
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 4 of 21
2.1.2 Calibration Setup - A test setup for calibrating the
pitot tube can be constructed in the laboratory from a straight
section of duct that is 10 to 12 duct diameters long, as shown
in Figure 2.3. The diameter of a circular duct must be at least
30.5 cm (12 in.), and the width (shorter side) of a rectangular
duct of the same area must be at least 25.4 cm (10 in.). For a
rectangular cross section, an equivalent circular diameter calcu-
lated from the following equation should be used to determine the
required minimum length.
De = (L + W) Equation 2-1
where
D = equivalent diameter,
L = length of one side of duct, and
W = width of other side of duct
To ensure stable, fully developed flow patterns at the cali-
bration site or at the "test section," this site must be located
at least eight diameters downstream and two diameters upstream
from any flow disturbance such as a bend, change in cross sec-
tion, fan, or opening.
The eight- and two-diameter criteria are not absolute, and
other test section locations may be used (subject to approval of
the administrator), provided that the flow at the test site is
stable and parallel to the duct axis. This may be achieved
by using flow straighteners.
The flow system should generate a test section velocity of
about 915 m/min (3000 ft/min); this velocity must be constant
with time to guarantee steady flow during calibration. Type S
pitot tube coefficients obtained by single-velocity calibration
at 915 m/min (3000 ft/min) will generally be valid to within +3%
for the measurement of velocities above 305 m/min (1000 ft/min)
and to within +6% for those between 180 and 305 m/min (600 and
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 5 of 21
Q
oo
E
(U
4->
03
>i
U)
o
•H
-P
XI
-H
.H
O
Q)
•s
-p
-p
O
•H
CM
ro
CM
0)
H
3
Cn
•H
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 6 of 21
1000 ft/min). A more precise correlation between C and velocity
can be obtained if at least four distinct velocities ranging from
180 to 1525 m/min (600 to 5000 ft/min) are used.7'8
Two entry ports—one each for the standard and for the
Type S pitot tubes — should be cut in the test section, as shown
in Figure 2.4. The standard pitot entry port should be slightly
downstream of the Type S port, so that the standard and Type S
impact openings will lie in the same cross-sectional plane during
calibration. The exact distance between openings depends on the
standard pitot tube diameter. To facilitate alignment of the
pitot tubes during calibration, the test section should be con-
structed of plastic or some transparent material.
A permanently mounted manometer should be provided near the
calibration site. Plastic tubing and two-way valves will faci-
litate connecting the manometer to the pitot tubes and in
switching from one pitot tube to another. Pitot tube holders
should be used to maintain the alignment and location of each
pitot tube during calibration.
2.1.3 Calibration Procedure - One leg of the Type S pitot tube
should be marked with an "A" and the other with a "B." To
obtain calibration data for both the A and B sides, proceed as
follows:
1. Clean and fill the manometer with clean fluid of the
proper density. Inspect and leak check all pitot lines and
fittings; repair or replace if necessary.
2. Assemble the apparatus, as shown in Figure 2.4.
3. Level and zero the inclined manometer. Turn on the
fan, and allow the flow to stabilize. Seal the Type S entry port
with duct tape.
4. Position the standard type pitot tube near the center
of the duct, and seal the entry port with duct tape or other
means. Check to be sure that the pitot tube is properly aligned
and perpendicular to the duct.
-------
HOLDER
VSET SCREWS
f
\>
STANDARD
PITOT TUBE
D
o
iQ ft
n> n> H- rt
en H
-J C( H- O
&> O 3
033
o
o
Figure 2.4 Pitot tube calibration set-up,
CO
o
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 8 of 21
5. Adjust the fan speed or intake area to give a desired
velocity head, as measured by the standard pitot tube, and record
Ap td on a form such as Figure 2.5. Check the reading again;
withdraw this pitot tube; and seal the opening.
6. Connect the Type S pitot tube to the manometer. Insert
the Type S tube, and locate the tip at the same point in the duct
as that measured by the standard tube.
7. Align the Type S tube with leg A facing directly up-
stream. Alignment of the pitot tube along the roll and pitch
axes is best accomplished by visually aligning it against the
duct. Seal the entry port with a rag or duct tape. Figures 2.6
and 2.7 illustrate the magnitude and characteristics of measure-
ment errors in C associated with varying degrees of nonalignment
on the roll (yaw) and pitch axes, respectively.
8. Read and record the velocity head, Apg in Figure 2.5.
Remove the Type S tube from the duct, and disconnect the manom-
eter.
9. Repeat steps 4 through 8 above until three sets of
velocity head measurements are obtained.
10. Repeat the complete procedure with leg B of the Type S
pitot tube facing upstream.
11. Calculate the Type S pitot tube coefficient, Cp/sw for
each set of measurements, using Equation 2-2.
Cp(S) ~ Cp(std)\/ A Equation 2-2
where
c /$\ = Type S pitot tube coefficient,
C , . ,x = standard pitot tube coefficient (use 0.99 if
p(std) c
coefficient is unknown and tube is designed
according to guidelines in Section 3.1.1),
Ap ., = velocity head measured by the standard pitot tube,
cm (in.) H20, and
Apc = velocity head measured by the Type S pitot tube,
O
cm (in.) H20.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 9 of 21
Calibration pitot tube: type
Type S pitot tube ID number _
Calibration: date Ss,0~F / ,
size (OD) -Vg ID number
3¥- c
'p(std)
performed by //-
A-Side Calibration
APstd'
cm (in. )
H2°
0 . 0 t, 0
on OY;5T
o,o?o
APs,
cm (in. )
H2°
fr, ;-) 5? 5"
r^ .. / o ;>
TT / J 2,"
Average
c a
CP(S)
n . S 3 ^
rT R3V
:~> S^/5
r
:-^.r5j-/
DEV.b
o . uo r<
f) Ot>~<
6 z
0. JOtf
B-Side Calibration
APstd'
cm (in. )
H2°
0- i^5
n. o^o
b.o^S
Aps,
cm (in. )
H2°
p>.D9
/: ii
0.1 :i
Average
c a
CP(S)
p.BHi
n.314
0 . S 4 L
D.SH
DEV.b
C'.DM
0 CC H
fN. OOU
0 DD37
Cp(S) cp(std)
DEV = C_,c, - C
P v& /
Cp(A) - C (B) =
Ap
std
(, (must be £0.01)
O (must be £0.01)
Figure 2.5 Pitot tube calibration data.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 10 of 21
o
CE
o;
-80
-60
+40
+60
+80
0, DEGREES
Figure 2.6 Example of error in measured stack gas velocity as a
function of tube misalignment along its roll axis (yaw).
Figure 2.7 Example of error in measured stack gas velocity as a
function of tube misalignment along its pitch axis.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 11 of 21
12. Calculate C (A) and C (B), the average A-side and
B-side coefficients, and the difference between these two
averages.
13. Calculate the deviation of each of the three A-side
values of C ,_, from C (A), and the deviation of each B-side
P\ s) _ P
value of C , . from C (B), using Equation 2-3.
P(*>) p
Deviation = C /c, - C (A or B). Equation 2-3
P \ & I P
14. Calculate s, the estimated standard deviation of the
deviations from the mean for both the A and B sides of the pitot
tube using Equation 2-4.
s (A or B) = \ 1
Equation 2-4
Use the Type S pitot tube assembly only if the values of s for
both A and B are £0.02 and if the absolute value of the differ-
ence between C (A) and C (B) is £0.01.
2.1.4 Special Calibration Considerations - The pitot tube-probe
assembly may block a significant part of the flow in ducts <91 cm
(36 in.) in diameter. This blockage, in turn, affects the pitot
tube calibration factor. To check for any blockage effects, use
the following procedure:
1. Make a projected-area model of the pitot tube assembly
with the Type S pitot tube impact opening positioned at the
center of the duct (Figure 2.8). This model represents the
approximate "average blockage" of the duct cross section during
calibration or during a sample traverse. Although the actual
blockage will be less than this for sample points close to the
near stack wall and more than this for points close to the far
wall, the model approximates the average condition.
2. Calculate the theoretical average blockage by taking
the ratio of the projected area of the probe sheath to the cross
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 12 of 21
o
o
UJ
OL
e
to
CD 3
•Si O
UJ X
oo to
oo
-H
Cn
cn
4J
o
•• X
UJ UJ
O O
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 13 of 21
sectional area of the duct (use consistent units of measure), and
multiply by 100. If the theoretical blockage is either <2% for
an assembly with an external sheath or <_3% for an assembly with-
out an external sheath, the decrease in C will be <1% and no
adjustment in the pitot tube coefficients will be necessary. If
the theoretical blockage exceeds these values, apply a correction
factor, as shown in Figure 2.9. During calibration, the blockage
effect can be minimized by keeping the pitot tube approximately
halfway between the near side wall and the center.
2.1.5 Recalibration - After each field use, the isolated pitot
tubes must be carefully examined and their dimensions checked, as
specified in Section 3.1.1. If damaged, a tube must either be
repaired to conform with the acceptable dimensions or be dis-
carded. Pitot tube assembly dimensions must also be carefully
checked. If the component spacings have not changed and if
alignment is intact, the assembly may be reused with the same
correction factor. If the spacings have changed, either restore
the original spacing or recalibrate. No correction to the field
data is required for runs that were started with acceptable pitot
tubes. If the pitot tube is damaged, it may be replaced using an
interference-free spacing, as shown in Section 2.1; otherwise,
the assembly should be recalibrated.
Standard pitot tubes need not be recalibrated. If they are
damaged, they should be replaced.
2.2 Stack Temperature Sensor
The stack temperature sensor should be calibrated upon
receipt or checked before field use. Each sensor should be
uniquely marked for identification. The calibration should be
performed at three points and then extrapolated over the range of
temperatures anticipated during actual sampling. For the three
point calibration, a reference mercury-in-glass thermometer
should be used.
The following procedure is recommended for calibrating stack
temperature sensors (thermocouples and thermometers) for field
use.11
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 14 of 21
d*
«•.
<
LU
<
o
LLJ
to
I
co
co
O
cc.
CJ
USE FOR ASSEMBLIES WITH
EXTERNAL SHEATH
O
_J
CO
<
CJ
a:
o
USE FOR ASSEMBLIES WITH
NO EXTERNAL SHEATH
0.99 0.98 0.97 0.96
CORRECTION FAC OR FOR PITOT TUBE COEFFICIENT
0.95
Figure 2.9
Adjustment of Type S pitot tube coefficients to
account for blockage effects in duct <91 cm in
diameter.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 15 of 21
1. For the ice point calibration, form a slush from
crushed ice and liquid water (preferably deionized, distilled) in
an insulated vessel such as a Dewar flask.
Taking care that they do not touch the sides of the flask,
insert the stack temperature sensor into the slush to a depth of
at least 2 in. Wait 1 min to achieve thermal equilibrium, and
record the readout on the potentiometer. Obtain three readings
taken in 1-min intervals. Note: Longer times may be required
to attain thermal equilibrium with thick-sheathed thermocouples.
2. Fill a large Pyrex beaker with water to a depth >4 in.
Place several boiling chips in the water, and bring the water to
a full boil using a hot plate as the heat source. Insert the
stack temperature sensor(s) in the boiling water to a depth of at
least 2 in. , taking care not to touch the sides or bottom of the
beaker.
Alongside the sensor(s), an ASTM reference thermometer
should be placed. If the entire length of the mercury shaft in
the thermometer cannot be immersed, a temperature correction will
be required to give the correct reference temperature.
After 3 min, both instruments will attain thermal equilib-
rium. Simultaneously record temperatures from the ASTM reference
thermometer and the stack temperature sensor three times at 1-min
intervals.
3. For thermocouple, repeat Step 2 with a liquid that has
a boiling point (such as cooking oil) in the 150° - 250°C (300° -
500°F^ range. Record all data on Figure 2.10. For thermometers,
other than thermocouples, repeat Step 2 with a liquid that
boils at the maximum temperature that the thermometer is to be
used, or place the stack thermometer and reference thermometer in
a furnace or other device to reach the required temperature.
Note: If the thermometer is to be used at temperatures higher
than the reference thermometers will record, the stack thermom-
eter may be calibrated with a thermocouple previously calibrated
with the above procedure.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 16 of 21
Date
T
Thermocouple number
Ambient temperature J.J. / °C Barometric pressure
Calibrator 77 faJfrrzi/vj Reference: mercury-in-glass £S TH
other
in. Hg
Reference
point
number
Source
(specify)
Reference
thermometer
temperature,
Thermocouple
potentiometer
temperature,
Temperature
difference,
0
o
/ o /. 6
%
*Every 30°C (50°F) for each reference point.
"*Type of calibration system used.
(ref temp, °C + 273) - (test thermom temp, °C + 273)
ref temp, °C + 273
_i
Figure 2.10 Stack temperature sensor calibration data form,
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 17 of 21
4. If the absolute temperature values of the reference
thermometer and thermocouple(s) agree within ±1.5% at each of the
three calibration points, plot the data on linear graph paper and
draw the best-fit line between the points or calculate the linear
equation using the least-squares method. The data may be extrap-
olated above and below the calibration points and cover the
entire manufacturer's suggested range for the thermocouple. For
the portion of the plot or equation that agrees within 1.5% of
the absolute reference temperature, no correction need be made.
For all other portions that do not agree within ±1.5% use the
plot or equation to correct the data.
If the absolute temperature values of the reference ther-
mometer and stack temperature sensor (other than the thermo-
couple) agree within ±1.5% at each of the three points, the
thermometer may be used over the range of calibration points for
testing without applying any correction factor. The data cannot
be extrapolated outside the calibration points.
2.3 Barometer
The field barometer should be adjusted initially and before
each test series to agree within 2.5 mm (0.1 in.) Hg of the mer-
cury-in-glass barometer or the station pressure value reported by
a nearby National Weather Service station corrected for eleva-
tion. The correction for elevation difference between the weath-
er station and sampling point should be applied at a rate of
-2.5 mm (0.1 in.) Hg/30 m (100 ft). Record the results on the
pretest sampling check form or on a similar form, as shown in
Section 3.1.3.
2.4 Differential Pressure Gauge
Differential pressure gauges other than inclined manometers
must be calibrated initially, and their calibration must be
checked after each test series. Calibrate and check the differ-
ential pressure gauge using the following procedure:
1. Connect the differential pressure qauge to a gauge-oil
manometer, as illustrated in Figure 2.11.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 18 of 21
TO PRESSURE SOURCE OR
VENTED TO ATfIC
DIFFERENTIAL PRESSURE
GAUGE
MANOMETER
TO VACUUM SYSTEM OR
VENTED TO ATMOSPHERE
Figure 2.11 Differential pressure gauge check.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 19 of 21
2. Vent the vacuum side to the atmosphere, and place a
pressure on each system.
3. Compare Ap readings of the differential pressure gauge
with those of the gauge-oil manometer at a minimum of three
points representing approximately the range of Ap values to be
encountered. Follow the same procedures on the vacuum side by
venting the pressure side to the atmosphere and by putting a
vacuum on the system.
4. The posttest calibration should be performed at the
average Ap. If the agreement is within ±5% the calibration is
acceptable; if not, void the data or consult the administrator to
determine acceptability.
5. Record the data on a form such as Figure 2.12. If, at
each point, the value of Ap as read by the differential pressure
gauge and the gauge-oil manometer agree within 5%, the differen-
tial pressure gauge should be considered properly calibrated.
-------
Gauge type /7)flq/J€
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 20 of 21
Serial or ID number 0 07 ^
Scale
Gauge-oil manometer Ap
C-- /
Side A ^'/6~
0. «u
c>. i
o.ao
Differential pressure
gauge Ap
0. /
0 • 1 ^
O ' 3 O
0-1
d itr
Pressure
difference
C)
Q
O
O
0
Calibration: initial
Date calibrated
posttest
by
77^
Figure 2.12 Differential pressure gauge calibration data form.
-------
Section No. 3.1.2
Revision No. 0
Date January 15, 1980
Page 21 of 21
Table 2.1 ACTIVITY MATRIX FOR CALIBRATION OF APPARATUS
Apparatus
Type S pi tot
tube and/or
probe
assembly
Stack gas tem-
perature
measurement
system
Barometer
Differential
pressure
gauge (does
not include
inclined
manometers)
Acceptance limits
All dimension speci-
fications met, or
calibrate according
to Sec 3.1.2, and
mount in an interfer-
ence free manner
Capable of measuring
within 1.5% of minimum
stack temperature
(absolute)
Agrees within 2.5 mm
(0.1 in.) Hg of
mercury- in-glass
barometer
Agree within ±5% of
inclined manometers
Frequency and method
of measurement
When purchased, use
method in Sees 3.1.1
and 3.1.2; visually
inspect after each
field test
When purchased and
after each field
test, calibrate
against ASTM 3C or
3F thermometer
Initially and after
every field use,
compare to a li quid-
in-glass barometer
Initially and after
each field use
Action if
requirements
are not met
Do not use
pitot tubes
that do not
meet face
opening
specifica-
tions; re-
pair or re-
place as re-
quired
Adjust to
agree with Hg
bulb thermom-
eter, or con-
struct a cal-
ibration
curve to cor-
rect the
readings
Adjust, re-
pair, or
discard
Reject test
results, or
consult
administra-
tor if post-
test calibra-
tion is out
of specifi-
cation
-------
Section No. 3.1.3
Revision No. 0
Date January 15, 1980
Page 1 of 7
3.0 PRESAMPLING OPERATIONS
The quality assurance activities for presampling prepara-
tions are summarized in Table 3.1 at the end of this section.
See Section 3.0 of this Handbook for details on preliminary site
visits.
3.1 Apparatus Check and Calibration
Figures 3.1 and 3.2 or similar forms are recommended to aid
the tester in recording calibration data and in preparing an
equipment checklist, status form, and packing list.
3.1.1 Type S Pitot Tube and Differential Pressure Gauge - For
the Type S pitot tube and inclined manometer assembly illustrated
in Figure 1.2, the following checks should be made before each
field test.
1. Visually inspect the pitot tube openings for damage
such as a scratch, nick, or dent that would tend to disrupt the
air flow pattern. Check for proper alignment; that is, the cen-
ters of the two openings should be in a straight line such that
when one opening is directed upstream, the other will be exactly
180° opposite, pointing downstream. If the damage or misalign-
ment is obvious when visually inspected, the pitot tube should be
replaced or repaired. Check the weld spots holding the two legs
together; if broken, repair. Calibration must be checked after
repair if the pitot tube does not conform to specifications.
2. Check the quick disconnects on the pitot tube and check
the connecting lines for proper operation. Clean the small metal
parts of the disconnect. Lubricate sparingly to help to keep
them free.
3. Blow out the pitot tube legs from the line ends with
compressed air, rinse with distilled water then with acetone, and
dry with compressed air.
4. Visually inspect the differential pressure gauge for
damage. Repair or replace as necessary. Level the inclined
-------
Section No. 3.1.3
Revision No. 0
Date January 15, 1980
Page 2 of 7
Date n^q^T / /f7f Completed by
/ / ~" ---— ---
Pitot Tube
Identification number 3 <£Date X/c/JT /,
Dimension specifications checked?* ix" yes
Calibration required? yes iX"
no
no
Date C &. %*£•
— • — — — n .
Temperature Sensor
Identification number /(s
Calibrated?* \^_ yes
no
Was a pretest temperature correction used? yes \ no
If yes, temperature correction ~^^_ °c (°F)
Barometer
Was the pretest field barometer reading correct?* ^X" yes no
Differential Pressure Gauge
Was pretest calibration acceptable?* \^ yes no
*Most significant items/parameters to be checked.
Figure 3.1 Pretest sampling checks
-------
Section No. 3.1.3
Revision No. 0
Date January 15, 1980
Page 3 of 7
Apparatus check
Pitot Tube
Type S
Standard
Length <" Hf(ft)
/
Calibrated* \/
Differential
Pressure Gauge
Inclined manom-
eter sensitivity
C'-.Zfr cnf (in. )
Other
Stack Temperature
Sensor
TypeTta-rrnc-copU.
Calibrated* N/?<
/
Orsat Analyzer
Orsat v/
/
Fyrite "
Other
Acceptable
Yes
V
/
V
/
/
No
Quantity
required
J
o
~;/
*>
^
^i
Ready
Yes
•/
./'
/
/
y
No
Loaded
and packed
u e^
— -~j
ye^
Je-
4^5
c^S
O
*Most significant items/parameters to be checked.
Figure 3.2 Pretest preparation check.
-------
Section No. 3.1.3
Revision No. 0
Date January 15, 1980
Page 4 of 7
manometer (if used as the differential pressure gauge), and fill
with the proper specific gravity fluid; this recommended fluid is
usually inscribed on the manometer. Check for leaks, especially
around the fluid level plunger and drain screws. Replace the
fluid level plunger or 0-rings if leaks are detected. Clean the
manometer when it is dirty and change the fluid at any sign of
fading. If other differential pressure gauges are used, follow
the manufacturer's check-out instructions.
5. Connect the pitot tube and differential pressure gauge
with the pitot tube lines. Check for obstructions by blowing
lightly on one pitot tube leg and then the other; watch the
responses of the gauge. Also check for leaks by blowing into the
downstream leg, sealing the opening, and noting any drop in the
pressure gauge reading. Check the upstream leg by drawing a
slight vacuum, sealing, and noting the gauge. If there are no
leaks, the gauge readings will remain constant. No change in the
differential pressure gauge reading should occur.
6. Check the manometer fluid reservoir for proper adjust-
ment. A standard 0-254 mm (0-10 in.) H~0 manometer should be
able to adjust ±1.3 mm (0.05 in.) H20.
3.1.2 Temperature Measurement System - The following temperature
gauge checks should be made before each field test:
1. Visually check the readout device, sensor, and inter-
connecting lines or wires as applicable for general appearance.
If damage is detected, repair or replace as necessary.
2. Compare the ambient temperature readings made with the
temperature measuring system to those made with a mercury-in-
glass thermometer. If the system does not agree within ±4°C
(this is less than ±1.5% at about 293K, which is near room tem-
perature) of the thermometer, the temperature measuring system
should be calibrated as directed in Section 3.1.2. Otherwise,
record the two readings in the calibration log book and date and
initial the entries.
3.1.3 Barometer - Check the field barometer reading against that
of a mercury barometer. If they disagree more than ±2.3 mm
-------
Section No. 3.1.3
Revision No. 0
Date January 15, 1980
Page 5 of 7
(0.1 in.) of mercury, adjust the field barometer until it agrees
with the mercury barometer. Record the two readings in the cali-
bration log book; date and initial the entries.
3.2 Packing Equipment for Shipment
The logistics, time of sampling, and quality of data of any
source testing method are dependent upon the packing of equip-
ment in regards to (1) accessibility, (2) ease of movement, and
(3) optimum functioning of measurement devices in the field.
Equipment should be packed under the assumption that it will
receive severe treatment during shipping and field operation.
3.2.1 Type S Pitot Tube - Pack the pitot tube in a case pro-
tected by styrofoam or other suitable packing material. The
case should have handles which can withstand hoisting and should
be rigid enough to prevent bending or twisting of the pitot tube
during shipping and handling.
3.2.2 Differential Pressure Gauge - Close all valves on the
pressure gauge and pack it in a suitable case for shipment.
Pack spare parts such as 0-rings and operating fluid (for in-
clined manometer).
3.2.3 Temperature Measurement System - Proper packing of the
temperature measuring systems depends on the type of system used.
In general, the sensor and leads can be protected from breakage
or other damage during shipment by securing them to the pitot
tube and enclosing them with suitable packing material. The
readout device, if detachable from the sensor, should be packed
in a separate packing case. Check batteries and include spares
prior to shipment if applicable.
3.2.4 Barometer - The barometer should be packed in a shock-
mounted (spring system) carrying case.
-------
Section No. 3.1.3
Revision No. 0
Date January 15, 1980
Page 6 of 7
Table 3.1 ACTIVITY MATRIX FOR PRE-SAMPLING
Operation
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Type S pitot
tube assembly
1. No evidence of
damage/misalignment
2. Proper operation
3. Cleaned accord-
ing to procedure
4. No Leaks
5. No visual damage
or leaks
6. Proper response
of the gauge
7. Sensitivity ±1.3
mm (0.05 in.) H0
1. Visually check
for damage, alignment
2. Check quick dis-
connects for proper
operation
3. Blow out tube
legs; rinse first
with distilled HO
and then with
acetone; dry with
compressed air
4. Check for leaks
5. Visually check
differential pres-
sure gauge for
damage or leaks
6. Check for ob-
struction by
blowing lightly
7. Check reservoir
for proper adjust-
ment range
1. Replace or
repair, and then
recalibrate
2. Clean, and
use a drop of
penetrating
oil
Reclean
4. Repair or
replace as
necessary
5. Repair
or replace
as necessary
6. Remove ob-
struction, and
repeat test
7. Add or
remove fluid
Temperature
measurement
system
Agreement within ±4°C
(7°F) (<1.5% at 293K)
(530°R); ^ room temp-
ature
Before each field
test, compare ab-
solute ambient
readings to those
with a Hg-in-glass
thermometer
Recalibrate
the system
(continued)
-------
Section No. 3.1.3
Revision No. 0
Date January 15, 1980
Page 7 of 1
Table 3.1 (continued)
Operation
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Barometer
Agreement within (2.5
mm) 0.1 in. Hg
Before each field
test, check against
a Hg barometer
Adjust until
agreement
attained
Packing equip-
ment for
shipment
Packed according
to specified
conditions
Visually check
Correct the
packing
procedure
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 1 of 12
4.0 ON-SITE MEASUREMENTS
The on-site measurement activities include transporting
equipment to the test site, unpacking and assembling equipment,
making duct measurements, measuring velocity, determining mole-
cular weight, and recording data. Table 4.1 at the end of this
section summarizes the quality assurance activities for on-site
measurements. A copy of all field data forms mentioned are in
Section 3.1.12.
4.1 Transport of Equipment to the Sampling Site
The most efficient means of transporting the equipment from
ground level to the sampling site should be decided during the
preliminary site visit (or prior correspondence). Care should be
exercised to prevent damage to the test equipment or injury to
test personnel during the moving phase.
4.2 Velocity Measurement
On-site measurements include the following steps:
1. Preliminary measurements and setup; this includes a
determination of acceptable flow conditions, as described in
Method 1 (Section 3.0.1).
2. Leak checking the pitot tube and differential pressure
gauge.
3. Insertion of the pitot assembly into the stack.
4. Sealing the port.
5. Measuring velocity pressure and temperature at de-
signated points.
6. Measuring the static pressure of the stack.
7. Determining the moisture content according to Method 4.
8. Determining the molecular weight according to Method 3.
A final leak check of the pitot tube and differential pressure
gauge assembly must always be performed upon completion of sam-
pling. Record all data on Figure 4.1 or similar form.
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 2 of 12
Plant and city
-LccCk-M L/;J ;,,r; t CO, ^jjC-p^Ll^ cN'/U-0
Run date
r>
/
/
>T S
-*•>
c. /
Sampling location
M.?;o Ok'rK
Clock
time 9 *D
Run
number
/
Operator
f r"^ ;
C- ,'->/-<'-', fO
Amb . temp . ,
°F
*7Q
; t
Bar. press. ,
in. Hg
^9 r>~V
Static press. ,
in. H20
-(). o,5~
Molecular
wt.
•-) ," --, +'~
„ > (- ' * >-«'- \ /
Stack inside dimension, in.
Diam. of side
y
i
^
side
2
Pitot
tube (C )
c
.
V
Ij
^ }
•
i\
*v
_tT
Position,
in.
7. C'
/-V ?
,-?A. !?•
_-\
/ .?
i
, ^
,•>
.X
^
i , i
i
Stack temp . ,
°F
,? ? "
..x-r
,^^
^•"#,•? j?
.,->
r> . .*r
:"/' 'T
^,.7
J7 - C -•
i'' /
t'. /
0 3
£' -^"
£• 5"
r^ .i
Average angle («)
Angle (°0
which yields
a null Ap
/
.0
z.
5
A
-"T
j
/
">
W.
^
v^T"
5~
•o
^
Average of tt raust be <10 degrees to be acceptable.
Figure 4.1 Method 2 gas velocity and volume data form.
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 3 of 12
4.2.1 Preliminary Measurements and Setup - An accurate determi-
nation of the stack's cross-sectional area is important when
calculating volumetric flow rate. Also, the inside dimensions
must be known to properly mark the pitot tube for making a veloc-
ity traverse and to calculate a total flow rate. Field team
members must use good judgement and experience in selecting the
best method of measuring stack dimensions for each particular
situation.
Two commonly used methods of measuring stack dimensions are:
1. Inserting a rigid rod made of metal or other material
that will, in most instances, withstand stack conditions through
a sampling port, is the easiest and most accurate method of mea-
suring the dimensions (i.e., diameter or length and width) of
small stacks . Caution: When testing a stack that has hot and/or
noxious gases at a positive pressure, use a packing gland to pre-
vent the gases from escaping from the sampling port. Also, wear
asbestos gloves when working around a hot stack.
Because all circular stacks are not perfect circles and
because all sides of a rectangular stack are not straight, best
results are obtained if the dimensions are measured from as many
sampling ports as available at the sampling site. Calculate the
average value for use in subsequent calculation of the volumetric
flow rate. Sketch the cross-sectional area of the stack on the
sample data form (Figure 4.1), and show all measured dimensions
and their values. Record the average value on the same form in
the blank space designated for stack dimension. (If the stack is
rectangular, record the average length and width in this space,
and mark out the diameter.) Determine all dimensions to the
nearest 3 mm (1/8 in.).
2. For stacks too large or too inconvenient for measuring
with a rod as described in (1) above, the next best method may be
to measure the outside circumference and to calculate the inside
diameter (d):
d = (C/7t) - 2t Equation 4-1
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 4 of 12
where
d = inside diameter of the stack,
C = outside circumference of stack,
n ^ 3.1416 * 22/7, and
t = stack wall thickness.
For rectangular stacks, measure the outside dimensions and
subtract the (2t) wall thickness; measure all lengths to the
nearest 3 mm (1/8 in). Note: In horizontal ducts, particulate
buildup may occur on the bottom of the duct; this buildup (deter-
mined visually or by probing with a rod) should be subtracted
from the duct cross section. Select the sampling site location
in accordance with Method 2; if this is not possible due to duct
configuration or other reasons, have the sampling site location
approved by the administrator. Determine the minimum number of
traverse points by Method 1, or check the traverse points deter-
mined from the preliminary site visit (Section 3.0 of this Hand-
book). Record all data on the traverse point location form, as
shown in Section 3.0. Use these measurements to locate the pitot
tube and the sampling probe during preliminary measurements and
actual sampling.
4.2.2 Stack Parameters - Check the sampling site for cyclonic or
nonparallel flow, as described in Method 1 (Section 3.0.1). The
sampling site must be acceptable before a valid measurement can
be made. Be sure that the proper differential pressure gauge is
chosen for the range of velocity heads encountered.
4.2.3 Velocity Measurement - Determine the number and location
of traverse points and sampling ports by Method 1. For circular
stacks <3 m (10 ft) in diameter, two ports along diameters at
right angles to each other and in the same plane are sufficient;
however, when the stack diameter is >3 m (10 ft), four ports—one
at each end of the two diameters—are desirable to avoid the use
of extra long pitot tubes. If it is necessary to use a Type S
pitot tube >3 m (10 ft) in length, it should be structurally re-
inforced to prevent bending of the tube and resulting in the type
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 5 of 12
error illustrated in Figure 2.7. Each sampling port and traverse
point should be identified by a number or letter and should be
so-designated on the sketch.
Measure the velocity head and temperature at each traverse
point accessible from a given port by measuring each point once
as the pitot tube is inserted into the stack and moved across the
stack's diameter. To prevent damage or clogging, be careful to
avoid touching the pitot tube tip to the side of the stack wall.
A standard pitot tube may be used instead of a Type S, for
conducting velocity traverses; however, the static and impact
pressure holes of standard pitot tubes are susceptible to plug-
ging in particulate-laden or moist gas streams. Therefore, when-
ever a standard pitot tube is used to perform a traverse,
adequate proof must be furnished to show that the openings of the
pitot tube did not plug up during the traverse period.
The following procedure will provide sufficient evidence
that plugging did not occur.
1. Measure the velocity head (Ap) reading at the final
traverse point.
2. Clean out the impact and static holes of the standard
pitot tube by "back purging" with pressurized air, and then re-
measure the Ap at the final point. If the Ap readings before and
after the air purge are the same (±5%), the traverse is accept-
able. Note; If Ap at the final point is unsuitably low, another
point may be selected.
If "back purging" at regular intervals is part of the pro-
cedure, comparative Ap readings should be taken (as above) for
the last two back purges at which suitably high Ap readings are
observed.
3. Record the clock time, Ap, and Tg for each traverse
point on the data form (Figure 4.1).
4. After the traverse, check the differential pressure
gauge zero setting and local indicator. If either has shifted,
reset and repeat the traverse.
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 6 of 12
If a more sensitive differential pressure gauge is required
after making a traverse because the velocity head readings were
<1.3 mm (0.05 in.), use a more sensitive manometer, as discussed
in Section 3.1.1. After completing the traverse, check the pitot
tube differential pressue gauge assembly again for leaks, as de-
scribed in Subsection 4.2.5.
4.2.4 Measurement of Low Velocities - A Type S pitot tube can
be used to measure velocities as low as 122 m/min (400 ft/min)
without affecting the calibration coefficient.
Most sampling trains are equipped with a 10-in. (H20 column)
inclined vertical manometer that has 0.01-in. divisions on the
0-to-l-in. inclined scale and 0.1-in. divisions on the 1-to-
10-in. vertical scale. This type of manometer (or other gauge
of equivalent sensitivity) is satisfactory for the measurement
of Ap values as low as 1.3 mm (0.05 in.) H20. However, a differ-
ential pressure gauge of greater sensitivity should be used (sub-
ject to the approval of the administrator) if any of the follow-
ing is found to be true:
1. The arithmetic average of all Ap readings at the tra-
verse points in the stack is <1.3 mm (0.05 in.) H90;
£*
2. More than 10% of the individual Ap readings are <1.3 mm
(0.05 in.) H-O points, for traverses of 12 or more points;
3. More than one Ap reading is <1.3 mm (0.05 in.) H?0 for
traverses of fewer than 12 points.
As an alternative to criteria (1) through (3) above, the
following calculation may be performed to determine the necessity
of using a more sensitive differential pressure gauge:
n ,
I |/Ap. + K
T = i = 1 r
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 7 of 12
where
Ap. = individual velocity head reading at a traverse point,
mm (in.) H20,
n = total number of traverse points, and
K = 0.13 mm (0.005 in.) H20.
If T is >1.05, the velocity head data are unacceptable, and a
more sensitive differential pressure gauge must be used.
4.2.5 Special Precautions - Before and during the traverse, a
number of precautions should be taken:
1. The pitot tube should be short enough for easy handling
from outside the stack when held at any traverse point for safety
reasons and for efficiency in the measurement process.
2. The alignment should be made visually with reference to
the stack geometry and not by rolling or tipping the pitot tube
until a maximum response is observed.
3. If the gas stream contains a significant concentration
of particulates, both legs of the pitot tube should be blown out
frequently during the velocity traverse.
4. All unused sampling ports must be plugged, and the port
being used should be sealed as tightly as possible to minimize
any disturbance on the gas flow pattern when making a velocity
measurement. The port being used can be sealed with asbestos
material, precut sponge, or duct tape depending on the tempera-
ture of the stack gas.
5. If liquid droplets are present in the gas stream, a
liquid trap should be inserted in the gauge line leading to the
upstream pitot tube leg (impact opening). A trap may be required
for both legs.
6. When testing a stack that has hot and/or noxious gases
under positive pressure, a packing gland and gate valve assembly
should be used to prevent the gases from escaping from the sam-
pling port. Caution: Asbestos gloves should be worn when work-
ing around a hot stack. Always wear safety glasses and under
hazardous conditions, fullface shields.
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 8 of 12
7. Damage or suspected damage to any item of equipment,
such as a pitot tube or an inclined manometer, during the test
should be fully documented at the time it occurs or at the first
awareness of its occurrence. The item should be replaced by a
spare if available. If it is necessary to continue using the
damaged item, a posttest calibration (as described in Section
3.1.2) should be performed, and the new calibration should be
used for the data collected after the damage occurred.
4.2.6 Measurement of the Static Pressure in the Stack - Three
acceptable methods for measuring static pressure are given in the
order of decreasing acceptability:
1. Install a tap perpendicular to the stack gas flow, or
insert a 6-mm (0.25-in.) steel tube into the sampling port while
maintaining a good seal. Connect one side of a U-tube manometer
to the tap, and vent the other side of the manometer to the
atmosphere. If the pressure is expected to be >63-75 cm (25-30
in.) H-O, a mercury-filled U-tube manometer should be used
instead of a water-filled U-tube.
2. Use the static pressure tap of a standard pitot tube
connected to one side of a manometer. (If the stack pressure is
obviously negative, connect the static pressure tap to the other
side of the manometer; otherwise trial and error will have to
suffice.) Vent the remaining side of the manometer to the
atmosphere. Point the pitot tube pressure opening (the uncon-
nected end) directly into the flow and seal the port around the
tube.
3. Use a Type S pitot tube with the pitot tube openings
facing perpendicular to the gas stream. Connect only one leg of
the pitot tube to the manometer; vent the other side of the
manometer to the atmosphere. Take extreme care to align the
probe properly and to seal the port around the pitot tube.
One static pressure reading is usually adequate for all
points within a stack; however, this must be confirmed by ran-
domly moving the pressure probe over the stack to see if there
are any significant variations—that is, a range of pressure
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 9 of 12
values >100 mm (4 in.) E^O. If there are significant variations,
visually check the location for physical flow disturbances. If
none are found, measure and record the static pressure at each
traverse point.
4. Measure the atmospheric pressure at the test site using
the barometer.
Record the static pressure, P , (be sure to include the plus
or minus sign for positive or negative pressure respectively) as
read from the manometer on the velocity data form, Figure 4.1.
4.2.7 Pitot Tube Calibration Check - If the pitot tube coef-
ficient were based on an acceptable geometry standard, be sure
that the pitot meets these standards prior to each run and that
no posttest data correction is required from any pitot tube
damages that may have occurred during testing.
4.2.8 Dry Stack Gas Molecular Weight Determination - For combus-
tion processes, use Method 3. For processes emitting essentially
air, an analysis need not be conducted and a molecular weight of
29 should be used. Moisture content can be measured by using
Method 4. For other processes, consult the administrator.
4.3 Sample Logistics (Data) and Packing of Equipment - Follow
the above procedures until the required number of runs are com-
pleted. Log all data on the form shown previously in Figure 4.1.
The following are recommended at the completion of the test
series:
1. Record and duplicate all data recorded during the field
test by the best means available. One set of data can then be
either mailed to the base laboratory, given to another team
member, or to the Agency; the original data should be hand-
carried.
2. Examine all sampling equipment for damage, and then
properly pack it for shipment to the base laboratory. All ship-
ping containers should be properly labeled to prevent loss of
equipment.
3. Quickly check sampling procedures using the data form,
Figure 4.2.
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 10 of 12
Sampling
Pitot tube, lines, and manometer assembled correctly?*
Pitot tube and components mounted in an interference free man-
ner?*
Differential pressure gauge has correct sensitivity?*
Differential pressure gauge leveled and zeroed?*
Pretest leak check? ij£S (optional) Cyclonic flow checked?
Pitot tube parallel to stack walls?*
Static pressure measured? t
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 11 of 12
Table 4.1 ACTIVITY MATRIX FOR ON-SITE MEASUREMENTS
Activity
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Type S pitot
tube and
differential
pressure
gauge
Leak-free connections;
manometer properly
leveled; oil column
zeroed
Visually check before
taking measurements
at each field test
Take cor-
rective
action
Temperature
measurement
system
No physical damage
Visually check for
damage
Take cor-
rective
action prior
to taking
measurements
Cross sectional
area of stack
All measurements
made to the nearest
3 mm (1/8 in.)
During each field
test, measure inside
diameter (or width)
and/or circumfer-
ence (perimeter)
Obtain data
as specified
Velocity
measurements
1. Number and lo-
cation of traverse
points (Method 1)
2. No leaks for 15 s
1. Check before
taking measurements
2. Apparatus leak
checked upon com-
pletion of tests
Repeat
traverse
Static
pressure
Variation in static
pressure Pg <10Q mm
(3.9 in.) H20 to make
a single point mea-
surement
Use one of three
means given in Sub-
sec 4.8; move probe
over cross section
to determine if
variation is
significant
Check the
location for
disturbances;
if none,
measure and
record the
static pres-
sure at
each point
(continued)
-------
Section No. 3.1.4
Revision No. 0
Date January 15, 1980
Page 12 of 12
Table 4.1 (continued)
Activity
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sample logis-
tics (data)
and packing
of equipment
1. All data recorded
correctly
2. All equipment
examined for damage
and labeled for
shipment
1. Upon completion
of each traverse and
before packing for
shipment
2. As above
1. Complete
required
number of
runs
2. Repeat the
sampling if
damage occurred
during testing
-------
Section No. 3.1.5
Revision No. 0
Date January 15, 1980
Page 1 of 3
5.0 POSTSAMPLING OPERATIONS
Table 5.1 at the end of this section summarizes the
quality assurance activities for postsampling operations.
5.1 Apparatus Checks
Disassemble, clean, and visually check each component of the
sample apparatus upon completion of sampling. Posttest cali-
bration must be performed on the pitot tube if damaged, and the
temperature sensor.
5.1.1 Pitot Tube - If the pitot tube is damaged, do not repair
if the sample runs were started with the unacceptable pitot tube.
Calibrate the pitot tube according to Section 3.1.2. For cali-
bration purposes, the pitot tube posttest coefficient should be
used for all data obtained using the damaged pitot tube only.
For any runs that started with an acceptable pitot tube no data
correction is required. After calibration, repair the pitot tube
and calibrate as initially (by dimensional specifications or
calibration). Record posttest calibration data on Figure 5.1.
If all runs were started with an acceptable pitot, and repairs
can be made, no field data correction is required.
5.1.2 Temperature Sensor - The stack temperature sensor readings
should be compared with the reference thermometer readings.
For thermocouples(s), compare the thermocouple and refer-
ence thermometer values at ambient temperature. If the values
agree within ±1.5% of the absolute temperature, the calibration
is considered valid. If the values do not agree within ±1.5%,
recalibrate the thermocouple as described in Section 3.1.2 to
determine the difference (AT ) at the average stack temperature
S
(T ). Note: This comparison may be done in the field immedi-
S -™-1-"1"-"™-""
ately following the tests.
For thermometers, compare the reference thermometer (1) at
ambient temperatures for average stack temperature below 100°C
(212°F), (2) in boiling water for stack temperatures from 100° -
200°C (212° - 390°F), and (3) in a boiling liquid with a boiling
-------
Section No. 3.1.5
Revision No. 0
Date January 15, 1980
Page 2 of 3
Pitot Tube
Initial pitot tube coefficient $. OT
Was pitot tube damaged prior to start of any test runs? yes
>X"n.o
If yes, was pitot tube calibrated prior to repair?* yes no
Pitot tube coefficient (damaged) ^___ (this value must
be used for runs started with the damaged pitot tube)
Temperature Sensor
Was a pretest temperature correction used? yes tX* no
If yes, temperature correction °C (°F) (within 1.5%
of readings in K (°R) over range) .—_
Average stack temperature of compliance test (T ) /^. K (f°R))
Temperature of referejice thermometer or solution for recalibra-
tion* rf^ K
-------
Section No. 3.1.5
Revision No. 0
Date January 15, 1980
Page 3 of 3
point >200° (390°F) for stack temperatures between 200° - 405°C
(390° - 760°F). For stack temperatures >405° (760°F), compare
the stack thermometer with a thermocouple at a temperature with-
in ±10% of the average absolute stack temperature. If the abso-
lute values agree within ±1.5%, the calibration is considered
valid. If not, determine the error (AT ) to correct the average
s
stack temperature.
5.1.3 Barometer - The field barometers are acceptable if they
agree within ±5 mm (0.2 in.) Hg when compared with the mercury-
in-glass barometer. When the comparison is not within this
range, the lesser calibration value should be used for the cal-
culations. If the field barometer reads lower, no correction is
necessary. When the mercury-in-glass barometer gives the lower
reading, subtract the difference from the field data readings
for the calculations.
Table 5.1 ACTIVITY MATRIX FOR POST-SAMPLING OPERATIONS
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Pi tot tube
If damaged, recali-
brate according to
Sec 3.1.2
After every field
test, visually
inspect for damage
Recalibrate,
and use cali-
bration fac-
tor for data
obtained by
using damaged
pi tot tube or
repeat the
tests
Temperature
sensor
Within ±1.5% of
absolute temperature
Calibrate with ASTM
mercury-in-glass
thermometer
Use correc-
tion factor
on tempera-
ture data
Barometer
Within ±2.5 mm (0.1
in.) Hg at ambient
pressure
Compare with mercury-
in-glass barometer
after each test
Recalibrate,
and use lower
barometric
values for
calculations
-------
Section No. 3.1.6
Revision No. 0
Date January 15, 1980
Page 1 of 4
6.0 CALCULATIONS
Calculation errors due to procedural or mathematical mis-
takes can be a large part of total system error. Therefore, it
is recommended that each set of calculations be repeated or spot
checked, preferably by a team member other than the one who per-
formed the original calculations. If a difference greater than
typical roundoff error is detected, the calculations should be
checked step-by-step until the source of error is found and cor-
rected. A computer program that prints the input data so that it
can be checked is advantageous in reducing calculation errors.
If a standardized computer program is used, the original data
entry should be checked; if differences are observed, a new com-
puter run should be made. Table 6.1 at the end of this section
summarizes the quality assurance activities for calculations.
Calculations should be carried out retaining at least one
significant digit beyond that of the acquired data and then
should be rounded off after final calculation to two significant
digits for each run or sample. All rounding off of numbers
should be in accordance with the ASTM 380-76 procedures. Record
all calculations on Figures 6.1A or B and on Figures 6.2A or B,
or on similar forms.
6.1 Nomenc1ature
The nomenclature used in the calculations that follow are
listed alphabetically.
2 2
A = Cross-sectional area of stack, m (ft )
B = Water vapor in the gas stream (Method 5 or Method 4), pro-
ws
portion by volume
C = Pitot tube coefficient, dimensionless
-------
Section No. 3.1.6
Revision No. 0
Date January 15, 1980
Page 2 of 4
= Pitot tube constant,
34.97
85.49
m
ft
(g/g-mole)(mm Hg)
(°K)(mm
1/2
for the-metrie system, and
(lb/lb-mole)(in. Hg)
in. H20)
1/2
for the English system
M
M
Ap =
bar
Ps =
rstd
Qstd
Ts =
Molecular weight of stack gas, dry basis, g/g-mole
(Ib/lb-mole)
Molecular weight of stack gas, wet basis, g/g-mole
(Ib/lb-mole), or
Md(l - Bws) + 18.0 Bws Equation 6-1
Velocity head of stack gas, mm (in.) H?0
Barometric pressure at measurement site, mm (in.) Hg
Stack static pressure, mm (in.) Hg
Absolute stack gas pressure, mm (in.) Hg, or
Pbar + P Equation 6-2
Standard absolute pressure, 760 mm (29.92 in.) Hg
Dry volumetric stack gas flow rate corrected to standard
conditions, dsm /h (dscf/h)
Stack temperature, °C (°F)
Absolute stack temperature, K (°R), or
273 + t for metric system
460 + t for English system
s
Equation 6-3
Equation 6-4
Astd ~
3600 =
18.0 =
Standard absolute temperature, 293K (528°R)
Average stack gas velocity, m/s (ft/s)
Conversion factor, s/h
Molecular weight of water, g/g-mole (Ib/lb-mole)
-------
Section No. 3.1.6
Revision No. 0
Date January 15, 1980
Page 3 of 4
6.2 Calculations
The following are the equations used to calculate the stack
gas velocity and the volumetric flow rate.
6.2.1 Average Stack Gas Velocity - Equation 6-5 is used to cal-
culate the average stack gas velocity at stack conditions.
vs = KpCP <^ Equation 6-5
This equation assumes that T , P , and M do not change appreci-
S S o
ably (i.e., <1%) with cross-sectional distance and with time. If
they do, consult the administrator to determine an acceptable
procedure.
The (/Ap)avg term is the average square root of each in-
dividual velocity head (Ap). Additionally, it should be noted
here that to be technically correct the term (^/T^)ava should be
used. However, since T is large, (usually >^289K (515°R), the
S
term V(T ) ' can be used with <1% error if the range of t is
s avg b
not XLO°C (50°F).
6.2.2 Average Stack Gas Dry Volumetric Flow Rate - Calculate
Q . , using Equation 6-6,
Qstd = 3600(1 - Bws)vs A IT&$ lip5—) Equation 6-6
-------
Section No. 3.1.6
Revision No. 0
Date January 15, 1980
Page 4 of 4
Table 6.1 ACTIVITY MATRIX FOR CALCULATION CHECKS
Characteristice
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Data analysis
form
All data and calcula-
tions given
Visually check
Complete the
missing data
values
Calculations
Difference between
check and original cal-
culations within round-
off error; at least one
decimal figure retained
beyond that of acquired
data
Repeat all calcula-
tions, starting with
raw data for hand
calculations; check
all raw data input
to computer calcu-
lations; hand cal-
culate one sample
per test
Indicate
errors on
analysis data
form
-------
Section No. 3.1.7
Revision No. 0
Date January 15, 1980
Page 1 of 1
7.0 MAINTENANCE
The normal use of emission testing equipment subjects it to
corrosive gases, extremes in temperature, vibrations, and shocks.
Keeping the equipment in good operating order over an extended
period of time requires a knowledge of the equipment and a pro-
gram of routine maintenance which is performed quarterly. Main-
tenance procedures for the various components are summarized in
Table 7.1 below.
The following procedures are not required, but are recom-
mended to increase the reliability of the equipment.
7.1 Pitot Tube
The pitot tube should be checked for dents, corrosion, and
dirt that may cause a complete restriction of pressure or cause
a leak in the system.
7.2 Inclined Manometer
The fluid in the inclined manometer should be changed
whenever there is discoloration or visible matter in the fluid,
and during the yearly disassembly. No other routine maintenance
is required since the inclined manometers will be leak checked
during both the leak check of the pitot tube and the leak check
of the entire control console.
Table 7.1 ACTIVITY MATRIX FOR EQUIPMENT MAINTENANCE CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Pitot tube
Check for dents, cor-
rosion, other damage,
or broken welds
Visually check before
and after each test
run
Use another
pitot tube
or clean, re-
pair, and
calibrate
Inclined mano-
meter
No discoloration or
visible matter in the
fluid
Check periodically
during disassembly
Replace parts
as needed
-------
Section No. 3.1.8
Revision No. 0
Date January 15, 1980
Page 1 of 5
8.0 AUDITING PROCEDURE
An audit is an independent assessment of data quality.
Independence is achieved if the individual(s) performing the
audit and their standards and equipment are different from those
used by the regular field crew. Routine quality assurance checks
by a field team are necessary in generation of good quality data,
but they are not part of the auditing procedure. Table 8.1 at
the end of this section summarizes the quality assurance activi-
ties for auditing, and Figure 8.1 suggest a checklist for the
auditor.
2
Based on the results of a collaborative test of Method 2,
two specific performance audits are recommended:
1. Audit of the measurement phase of Method 2, and
2. Audit of data processing.
In addition to these performance audits, a systems audit may be
conducted as specified by the quality assurance coordinator. The
performance audits and the systems audit are described in Subsec-
tions 8.1 and 8.2, respectively.
8.1 Performance Audits
Performance audits quantitatively evaluate the quality of
data produced by the total measurement system (sample collection,
data processing, etc.). It is recommended that these audits be
performed by the responsible control agency once during every
enforcement source test. A source test for enforcement comprises
a series of runs at one source.
8.1.1 Audit of Measurement Systems - A performance audit should
be performed on the geometric standards for the Type S pitot
tube, as described in Section 3.1.1.
8.1.2 Audit of Data Processing - Calculation errors are prev-
alent in Method 2. Data processing errors can be determined by
auditing the data recorded on the field and laboratory forms.
-------
Section No. 3.1.8
Revision No. 0
Date January 15, 1980
Page 2 of 5
The original and audit (check) calculations should agree within
roundoff; if not, all of the remaining data should be checked.
The data processing may also be audited by providing the testing
laboratory with specific data sets (exactly as would occur in the
field) and by requesting that the data calculation be completed
and that the results be returned to the agency/organization.
This audit is useful in checking both computer programs and
manual methods of data processing.
8.2 Systems Audit
A systems audit is an on-site qualitative inspection and
review of the total measurement system (sample collection, data
processing, etc.). Initially, a systems audit is recommended for
each enforcement source test, defined here as a series of three
runs at one source. After the test team gains experience with
the method, the frequency of audit may be reduced—once for every
four tests.
The auditor should have extensive background experience in
source sampling, specifically with the measurement system being
audited. The functions of the auditor are summarized in the
following:
1. Inform the testing team of the results of pretest
audits, specifying any area(s) that need special attention or
improvement.
2. Observe procedures and techniques of the field team
during sample collection.
3. Check/verify records of apparatus calibration checks
from previous source tests, where applicable.
4. Record the results of the audit and forward them with
comments to the team management so that appropriate corrective
action may be initiated.
While on site, the auditor observes the source test team's
overall performance including the following specific operations:
1. Determining stack dimensions and selecting the number
and position of traverse points.
-------
Section No. 3.1.8
Revision No. 0
Date January 15, 1980
Page 3 of 5
2. Checking the geometry criteria in the field using the
devices described in the calibration section.
3. Marking the pitot tube to ensure measurements at the
correct traverse points.
4. Checking for cyclonic flow.
5. Aligning the pitot tube properly along its roll and
pitch axes throughout the velocity traverse.
6. Clearing the pitot tube frequently when measuring in a
dust-laden gas.
7. Leak checking the sample apparatus.
-------
Section No. 3.1.8
Revision No. 0
Date January 15, 1980
Page 4 of 5
Yes
i/
iX
^
./'
v/
S
S
/
/
v/
/
t/
s
i/
v/
I/
y
No
Operation
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
Presampling preparation
Knowledge of process conditions
Calibration of pertinent equipment prior
to each field tests
On-site measurements
Pitot tube meets geometry requirements
Manometer should be carefully leveled and
the liquid column set exactly on zero
Check for cyclonic flow
Leak check after sample run
Sampling port adequately plugged
Process at correct operating level
Pitot tube properly aligned along its
roll and pitch axes throughout the
traverse
Pitot tube frequently cleared when
measuring in a dust- laden gas
Manometer has the correct sensitivity
Staying at each traverse point long enough
for the system to stabilize
Measuring the stack gas static pressure
and temperature
Postsampling
All information recorded on data form as
obtained
Any unusual conditions recorded
Independent check of calculations
Temperature sensor calibrated
COMMENTS
Figure 8.1 Stack gas velocity and volumetric flow rate
determination checklist to be used by auditor.
-------
Section No. 3.1.8
Revision No. 0
Date January 15, 1980
Page 5 of 5
Table 8.1 ACTIVITY MATRIX FOR AUDITING PROCEDURE
Audit
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Data processing
errors
Original and check
calculations agree
within roundoff error
Once during every
enforcement source
test, perform inde-
pendent calculations,
starting with re-
corded data
Check and
correct all
data for the
source test
Systems
audit
Operation technique
described in this sec-
tion of the Handbook
Once during every
enforcement test
until experience
gained; then every
fourth test; ob-
servation of tech-
nique, assisted by
audit checklist,
Fig 8.1
Explain to
team its de-
viations from
recommended
techniques,
and note on
Fig 8.1
-------
Section No. 3.1.9
Revision No. 0
Date January 15, 1980
Page 1 of 1
9.0 RECOMMENDED STANDARDS FOR ESTABLISHING TRACEABILITY
To achieve data of desired quality, two considerations are
necessary: (1) the measurement process must be in a state of
statistical control at the time of the measurement, and (2) the
systematic errors, when combined with the random variation
(errors of measurement), must result in a small uncertainty.
To ensure good quality data, it is necessary to perform
quality control checks and independent audits of the measurement
process; to document these checks and audits by recording the
results, as appropriate; and to use materials, instruments, and
measurement procedures that can be traced to an appropriate
standard of reference.
Working calibration standards should be traceable to
standards that are considered to be primary. Two primary
standards recommended for establishing traceability are:
1. Calibrate pitot tubes against a standard pitot tube
with a known coefficient obtained from the National Bureau of
Standards or standard measurement which has been shown to have
given acceptable coefficients.
2. Compare the stack temperature sensor to an ASTM re-
ference thermometer.
-------
Section No. 3.1.10
Revision No. 0
Date January 15, 1980
Page 1 of 11
10.0 REFERENCE METHOD
METHOD 2— DETERMINATION or PTACK O*s VELOCITY
AND VULUMKTKIC Kl.UW KATK (TYI'K S I'lTOT TlMIE)
1. Princlplt and ApjMcnbiUtt
I.I Principle. The average RAS velocity In a slack Is
determined from the KIU density and from meu'-nn'nient
of the aviTiMto velocity hend with a Typo 8 (Ktuus.scheil>e
or reverse type) pilot \\I\H\
1.2 Applicnhllily. ThN motliod \9 ftppllruhta for
tiirasunMtionl of (he Dvcnigo volocily of n giu slHMitu mid
fur untiiiltfydif' «'*s (tow.
This procedure is tn>( nppltraMo at nn-asiin'mrnt slii^
. Which full to inert Itin rui'-ijii of Method 1, Section 2.1.
Also, ilio niellmd i 'uuiol !>!• usi-d (or direct IIM-H nn-iucnt
In <>yclititle or swn iipf f i'^ *•! rciuns, Stx'tloit 2A of Met !i<»l
" 1 sh',.w, IIMW lo .It-i. ->,„„(• pyrlonic or swlilntf! Mctw con-
dilions. VMirii iiinici «'i'tillilt- iMitirliilon>. exist, ti]Irritative
pHK-fdiirc *, sn!>ji',-i ID i h.- iippruvul of the Adnnni-t nitor,
*'.S. I'lnxiro I'ftMitai rnUcction Agency, inu^l IK- nil-
ployed to ni'ikc nci tnme Mow rule (IctrnniMutiont;
cxuiiipli^ of stirli it t'•! i iiiv proccdtiics tin*' (I) to i MM nit
straightening VIHH-S, (V/ to paU'iilulo lite total volnuictrio
flow rule stoicltioinotnciilly, or (;*) to move to another
mcasurtimralUH that has boon demonstrated ('.ul)joct to
approval of the Administrator) to% ho raptiMf of mocting
the ^pcclUuatious will bo coiislderoxi ucccpluble.
Taken from the Federal Register, Vol. 42, No. 160—Thursday,
August 18, 1977, pp.41758-41768.
-------
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. 0
"Date January 15, 1980
Page 2 of 11
1.90- 2.54 cm*
(0.75 -1.0 in.)
7.62 cm (3 in.)
TEMPERATURE SENSOR
LEAK-FREE
CONNECTIONS
•SUGGESTED (INTERFERENCE FREE)
PITOT TUBE • THERMOCOUPLE SPACING
Figure 2-1. Type S pitot tube manometer assembly.
Type S pitot tube
al tubing (e.g., stain-
2.1 Type 8 Pitot Tube. The _
(Figure 2-1) shall be made of metal t. „ ......
less steel). It is recommended that the external tubing
diameter (dimension Z>i, Figure 2-2b) be between 0.48
and 0.95 centimeters (M« and 'A inch). There shall be
an equal distance from the base of each leg of the pitot
tub* to its face-opening plane (dimensions PA and Pa,
Figure 2-2b); It is recommended that this distance be
between 1.05 and 1.50 times the external tubing diameter.
The face openings of the pitot tube shall, preferably, be
aligned as shown In Figure 2-2; however, slight misalign-
ments of the openings are permissible (see Figure 2-3).
The Type S pitot tube snail have a known coefficient,
determined as outlined in Section 4. An identification
number shall be assigned to the pitot tube; this number
shall be permanently marked or engraved on the body
of the tube.
FEDERAL REGISTER, VOL. 42, NO. 160—THURSDAY, AUGUST 18, 1977
-------
417CO
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. 0
Date January 15, 1980
Page 3 of 11
TRANSVERSE
TUBE AXIS
FACE
•OPENING
PLANES
(a)
A SIDE PLANE
LONGITUDINAL
TUBE AXIS
NOTE:
PA
B-SIDE PLANE
(b)
A OR B
(c)
Figure 2-2. Properly constructed Type S pitot tube, shown
in: (a) end view; face opening planes perpendicular to trans-
verse axis; (b) top view; face opening planes parallel to lon-
gitudinal axis; (c) side view; both legs of equal length and
centerlines coincident, when viewed from both sides. Base-
line coefficient values of 0.84 may be assigned to pitot tubes
constructed this way.
FEDERAL RfGlSTER, VOl. 42, NO. 160—THURSDAY, AUGUST 1«, 1977
-------
TRANSVERSE-
TUBE AXIS "
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. 0
Date January 15, 1980
Page 4 -of n
LONGITUDINAL
TUBE AXIS—
(e)
t •
f
(f)
(a)
Figure 2-3. Types of face-opening misalignment that can result from field use or Im-
proper construction of Type S pitot tubes. These will not affect the baseline value
c7
-------
41762
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. 0
Date January 15, 1980
Page 5 of 11
A standard piioi tune may i*> uj~ •••»"«•« »• - - * «-- -•
provided that it meets the specificationsof Sections^
and 4.2; note, however, that tb« static and impact
pressure holes of standard pilot tubes are susccptibfe to
plugging in partlculate-ladcn gas streams. Therefore,
whenWer a standard pitot tube Is used to porform a
traverse, adequate proof must be furnished that the
openings of the pitot tube have not plugged up during the
traverse period; this can be done by taking a velocity
head (Ap) reading at the final traverse point, cleaning out
the impact and static holes of the standard pilot tube by
"back-purging" with pressurized air, and then taking
another Ap reading. If the Ap readings made before and
after the air purge are the same (t5 percent), the traycrso
is acceptable. Otherwise, reject the run. Note that if Ap
at the final traverse point is nnsuitab y low, another
point may be selected. If "back-purging" at .regular
intervals is part of the procedure, then comparative^Ap
readings shall be taken, as above, for the last two back
purges at which suitably high Ap readings are observed.
22 Differential Pressure Gauge. An Inclined manom-
eter or equivalent device is used. Most sampling trains
are equipped with a 10-in. (water •column) inclined-
vertical manometer, having 0.01-ln. H,O divisions on the
5. to 1-in inclined scale, and 0.1-in. H,O divisions on the
1- to 10-ln. vertical scale. This type of manometer (or
other gauge of equivalent sensitivity) is satisfactory for
the measurement of Ap values as low as 1.3 mm (0.05 in.)
HiO. However, a differential pressure gauge of greater
sensitivity shall be used (subject to the approval of the
Administrator), if any of the following is found to be
true: (1) the arithmetic average of all Ap readings at the
traverse points in the stack is less than 1.8 mm (O.OB in)
HiO- (2) for traverses of 12 or more points, more than 10
percent of the individual Ap readings are below 1.3 mm
toVOS to.) H,0; (3) lor traverses of fewer than12 points,
more than one Apreadingis below 1.3mm 0.05 in.) HjO.
Citation 18 in Section 6 describes commercially available
Instrumentation for the measurement of low-range gas
™As alternative to criteria (1) through (3) above, the
following calculation may be performed to determine the
necessity of using a more sensitive differential pressure
gauge:
perature gange need not be attached to the pilot tube;
this alternative Is subject to the approval of the
Administrator.
2.4 Pressure Probe and Oauge. A piezometer tube and
mercury- or water-filled U-tube manometer capable of
measuring stack pressure to within 2.5 mm (0.1 in.) Hg
is used. The static tap of a standard tj-pe pilot tube or
one leg of a Typo X pitot tube with the face opening
planes positioned parallel to the gas Dow may also be
used as the pressure probe.
2.5 Barometer. A mercury, aneroid, or other barom-
eter capable of measuring atmospheric pressure to
within 2.5 mm Hg (0.1 in. Hg) may be used. In many
cases, the barometric reading may bo obtained from a
nearby national weather service station, in which case
the station value (which Is the absolute barometric
pressure) shall be requested and an adjustment for
elevation differences between the weather station and
the sampling point shall be applied at a rate of minus
2.6 mm (0.1 in.) Ug per 30-meter (100 foot) elevation
Increase, or vice-versa lor elevation decrease.
2.6 Gas Density Determination Equipment. Method
3 equipment, if needed (see Section 3.6), to determine
the stack gas dry molecular weight, and Reference
Method 4 or Method 5 equipment for moisture content
determination; other methods may be used subject to
approval of the Administrator.
2.7 Calibration Pitot Tube. When calibration of the
Type S pitot tube is necessary (see Section 4), a standard
pitot tube Is used as a reference. The standard pitot
tube shall, preferably, have a known coefficient, obtained
either (1) directly from the National Bureau of Stand-
ards, Route 270, Quince Orchard Road, Qaithersburg,
T-=-
?-Individual velocity head reading at a traverse
point, mm HjO (In.H.G).
n=Total number of traverse points.
£•-0.13 mm HiO when metric units-are-used wid
0.005 In HiO when English units are used.
II T is greater than 1.05, the velocity head data are
unacceptable and a more sensitive differential pressure
gauge must be used. - it,
NOTE.—If differential pressure gauges other than
Inclined manometers are used (e.g., magnehelic gauges),
their calibration must be checked after each test series.
To check the calibration of a differential pressure gauge,
compare Ap readings of the gauge with those of a gauge-
oil manometer at a minimum of three points, approxi-
mately representing the range of Ap values in the stack.
If at each point, the values of Ap as read by the differen-
tial pressure gauge and gauge-oil manometer agree to
within 5 percent, the differential pressure gauge shall be
considered to be in proper calibration. Otherwise, the
test series shall either be voided, or procedures to adjust
the measured Ap values and final results shall be used,
sublect to the approval of the Administrator.
23 Temperature Oauge. A thermocouple, liquid-
filled bulb thermometer, bimetallic thermometer, mer-
cury-ln-glass thermometer, or other gauge capable of
measuring temperature to within 1.5 percent of the mini-
mum absolute stack temperature shall be used. The
temperature gauge shall be attached to the pilot tube
such that the sensor tip does not touch any metal; the
gauge shall be in an Interference-tree arrangement with
respect to the pitot tube face openings (see Figure 2-1
and also Figure 2-7 in Section 4). Alternate positions may
be used If the pitot tube-temperature gauge system is
calibrated according to the procedure of Section 4. Pro-
vided that a difference of not more than 1 percent in the
average velocity measurement is introduced, the tern-
Maryland, or (2) by calibration against another standard
pitot tube with an NBS-traceable coeflicient. Alter-
natively, a standard pitot tube designed according to
the criteria given In 2.7.1 through 2.7.5 below and illus-
trated In Figure 2-4 (see also Citations 7. 8. and 17 in
Section 6) may be used. Pitot tubes designed according
to these specifications will have baseline coefficients of
about 0.60±0.01.
2.7.1 Hemispherical (shown In Figure2-4),ellipsoidal,
or conical tip.
2.7.2 A minimum of six diameter" straight run (based
upon D, the external diameter of the tube) between tlie
tip and the static pressure holes.
2.7.3 A minimum of eight diameters straight run
between the static pressure holes and the. ccntcrhnc of
the external tube, following the 90 depree bend.
2.7.4 Static pressure holes of equnl size (approximately
0.1 D), equally spaced in a piezometer Ting configuration.
2.7.5 Ninety degree bend, with curved or milerod
Junction.
2.8 Differential Pressure Oauge for Typo S Pitot
Tube Calibration. An inclined manometer or equivalent
is used. If the single-velocity calibration technique Is
employed (see Section 4.1.2.3), the calibration differen-
tial pressure gauge shall be, readable to the nearest 0.13
mm HjO (0.005 in. HiO). For multivelocity calibrations,
the gauge shall be readable to the nearest 0.13 mm HjO
(0.005 in HiO) for Ap values between 1.3 and 25 mm IljO
(0.05 and 1.0 In. HjO), and to the nearest 1.3 mm lliO
(0.05 in. HiO) for Ap values above 25 mm HiO (1.0 In.
HiO). A special, more sensitive gauge will be required
to read Ap values below 1.3 mm HiO [0.05 In. HiO]
(see Citation 18 in Section 6).
CURVED OR
MITERED JUNCTION
HEMISPHERICAL
TIP
Figure 2-4.- Standard pitot tube design specifications.
STATIC
HOLES
3. Procedure _
3.1 Set up the apparatus as shown in Figure 2-1.
Capillary tubing or surge tanks installed between the
manometer and pitot tube may be used to dampen Ap
fluctuations. It Is recommended, but not required, that
a pretest leak-check be conducted, as follows: (1) blow
through the pitot impact opening until at least 7.6 cm
(3 in.) HjO velocity pressure registers on the manometer;
then, close off the impact opening. The pressure shall
remain stable for at least 15 seconds; (2) do the same for
the static pressure side, except using suction to obtain
the minimum of 7.6 cm (3 In.) HjO. Other leak-check
procedures, subject to the approval of the Administrator,
may be used. -
8.2 Level and wro the manometer. Because the ma
nometer lovcl and zero may drift due to vibrations and
temperature changes, make periodic checks during the
traverse. Record all necessary data as shown in the
example data sheet (Figure 2-5). .
- 3.3 Measure the velocity head and temperature at the
traverse points specified by Method 1. Ensure that the
proper differentia! pressure gauge is being used for the
range of Ap values encountered (see Section 2.2). If II is
necessary to change to a more sensitive gauge, do so, and
remeasure the Ap and temperature readings at each tra-
verse point. Conduct a post-test leak-check (mandatory),
as described in Section 3.1 above, to validate the traverse
run.
3.4 Measure the static pressure in the stack. One
reading is usually adequate.
3.5 Determine the atmospheric pressure.
FEDERAL REGISTER, VOL. 42, NO. 160—THURSDAY, AUGUST 18, 1977
-------
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. 0
Date January 15, 19SOTI
Page 6 of 11
PLANT.
DATE .
, RUN NO.
STACK DIAMETER OR DIMENSIONS, m(in.)
BAROMETRIC PRESSURE, nm Kg (in. Hg)__
CHOSS SECTIONAL ARE/X m2(fi2)
OPERATORS .
PITOTTUBEI.D.NO.
AVG. COEFFICIENT, Cp = .
LAST DATE CALIBRATED.
SCHEMATIC OF STACK
CROSS SECTION
Traverse
Pt. No.
Vel.Hd.,A{!
mm (in.) H20
Stack Temperature
Ts,0K{°fl)
mm Hg (in.Hg)
Average
Figure 2-5. Velocity traverse data.
r-I, VOL 42, NO. 160—THUII5DAY, AUGUST 1«, 1977
-------
41764
3.4 Determine the stock gas dry molecular weight.
y« combustion nrocease* or processes that emit essen-
tially COi Ot, CO. and Ni, ma Method 3. For processes
emitting essentially air, an analysis need not be con-
ducted; use a dry molecular weight of 29.0. For other
processes, other methods, subject to the approval of the
Administrator, must be used.
37 Obtain the moisture content from Reference
Method 4 (or equivalent) or from Method S.
3.8 Determine the cross-sectional area of the stack
or duct at the sampling location. Whenever possible,
physically measure tbe stack dimensions rather than
using blueprints.
4.1 Type 8 Pitot Tube. Before Its Initial use, care-
fnlrT examine the Type 8 pltot tube in top, side, and
end views to verify t£at the face openings of the tube
are aligned within the«pecfflcations illustrated In Figure
t-t or 2-4. The pltot tube shall not be used U It falls to
meet these alignment specifications.
After verifying tbe tact opening alignment, measure
and record the following dimensions of the pltot tube:
RULES AND REGULATIONS
0) the external tubing diameter (dimension Di, Figure
Z-2b); end (b) the base-to-opening plane distances
(dimension* P, and Pi, Figure 2-2b). If D, la between
0.48 and 0.95 era (M« and H In.) and If PA and Pe are
equal and between 1.05 and 1.50 K,, there are two possible
options: (1) the pltot tube may be calibrated according
to the procedure outlined In Sections 4.1.2 through
4.1.5 below, or (2) a baseline (isolated tube) coefficient
value of 0.84 may be assigned to the pitot tube. Note,
however, that If the pitot tube is part of an assembly,
calibration may still be required, despite knowledge
of the baseline coefficient value (see Section 4.1.1).
If D,, PA, and Pe are outside the specified limits, the
pitot tube must be calibrated as outlined In 4.1.2 through
4.1.5 below.
4.1.1 Type 8 Pltot Tube Assemblies. Daring sample
and velocity traverses, the Isolated Type 8 pltot tube is
not always used: in many instances, the pilot tube it
used in combination with other source-sampling compon-
ents (thermocouple, sampling probe, nozzle) as part of
an "assembly." The presence of other sampling compo-
nents can sometimes affect the baseline value of the Type
8 pitot tube coefficient (Citation 9 in Section 6); therefore
an assigned (or otherwise known) baseline coefficient
TYPES PITOT TUBE
Section No. 3.1.10
Revision No. 0
Date January 15, 1980
Page 7 of 11
value may or may not be Talld for a given assembly. The
baseline and assembly coefficient values will be identical
only when the relative placement of the components in
the assembly U such that aerodynamic interference
effects are eliminated. Figures 2-6 through 2-8 Illustrate
Interference-free component arrangements for Type 8
pilot tubes having eiternal tubing diameters between
0.48 and 0.95 cm (M« and H in.). Type S pilot tube assem-
blies that fail to meet any or all of the specifications of
Figures 2-6 through 2-8 shall be calibrated according to
the procedure outlined in Sections 4.1.2 through 4.1.5
below, and prior to calibration, the values of the inter-
component spacings (pitot-nozzle, pitot-thermocouple,
pitot'probe sheath) shall be measured and recorded.
NOTE.—Do not use any Type 8 pilot tube assembly
which is constructed such that the impact pressure open-
Ing plane of the pilot tube is below the entry plane of the
nozzle (see Figure 2-6b).
4.1.2 Calibration Setup. If the Type S pilot tube Is to
be calibrated, one leg of the tube shall be permanently
marked A, and the other, i. Calibration shall be done In
a flow system having the following essential design
features:
I
£1.90 em (3/4 in.) FOR On -1.3 cm (1/2 in.)
SAMPLING NOZZLE
A. BOTTOM VIEW; SHOWING MINIMUM PITOT-NOZZLE SEPARATION.
SAMPLING
PROBE
SAMPLING
NOZZLE
STATIC PRESSURE
OPENING PLANE
IMPACT PRESSURE
OPENING PLANE
JB—J
TYPES
PITOT TUBE
NOZZLE ENTRY
PLANE
SIDE VIEW; TO PREVENT PITOT TUBE
FROM INTERFERING WITH GAS FLOW
STREAMLINES APPROACHING THE
NOZZLE. THE IMPACT PRESSURE
OPENING PLANE OF THE PITOT TUBE
SHALL BE EVEN WITH OR ABOVE THE
NOZZLE ENTRY PLANE.
Figure 2-6. Proper pitot tube • sampling nozzle configuration to prevent
aerodynamic interference; buttonhook - type nozzle; centers of nozzle
and pitot opening aligned; Dt between 0.48 and 0.95 cm (3/16 and
3/8 in.).
FEDERAL REGISTER, VOL 42, NO. 160—THURSDAY, AUGUST 18, 1977
-------
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. ~0
Date January 15, 19$.0
Page 8 of 11
THERMOCOUPLE
W>7.62em
« ._. .—*
(3inJ
CIE
Z> 1.90 cm (3/4 in.)
THERMOCOUPLE
Z>S.Mmi i
(2 in.)
TYPES PITOT TUBE
SAMPLE PROBE
-3>
OR
r
-u-
TYPESPITOTTUBE
L SAMPLE PROBE
Figure 2-7. Proper thermocouple placement to prevent interference;
Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
TYPE SPITOT TUBE
T
I n;iii mi
SAMPLE PROBE
Y>7.62cm(3inJI
Figure 2-8. Minimum pitot-sample probe separation needed to prevent interference;
Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.}.
4.1.2.1 The flowing gas stream must be confined to *
duct of definite cross-sectional area, either circular or
rectangular. For circular cross-sections, the minimum
duct diameter shall be 30.5 cm (12 in.); for rectangular
cross-sections, the width (shorter side) shall be at least
25.4cm (10 in.).
4.1.2.2 The cross-sectional area of the calibration duct
must be constant over a distance of 10 or more duct
diameters. For a rectangular cross-section, use an equiva-
lent diameter, calculated from the following equation,
to determine the number of duct diameters.
__ 2LW
J'~(L+W)
Equation 2-1
where:
7J,= Equivalent diameter
7.= I.tnsth
IK=Width
To ensure the presence of stable, fully developed flow
patterns at the calibration site, or "lest section," the
site must be located at lea.st eight diameters downstream
and two diameters upstitara flora the nearest disturb-
ances.
NOTE.—The eight- and two-diameter criteria are not
absolute; other test section locations may be used (sub-
ject to apptoval of the Administrator), provided that the
flow at the test site 13 stable aud demonstrably parallel
to the duct axis.
4.1.2.3 The flow pystpm shall have the capacity to
generate a teat-section velocity around 915 m/tnm (3,000
ft/min). This velocity must be constant with time to
guarantee steady flow during calibration. Not* that
Type 8 pitot tube coefficients obtained by single-velocity
calibration at 915 m/min (3,000 ft/mm) will generally be
valid to within ±3 percent for the measurement o*
velocities above 305 m/min (1,000 ft/min) and to within-
±5 to 6 percent for the measurement of velocities be-
tween 180 and 305 m/min (600 and 1,000 ft/min). If a
more precise correlation between Cr and velocity is
desired, the flow system shall have the capacity to
generate at least four distinct, time-in variant test-section
velocities covering the velocity range from 180 to 1,525
m/min (600 to 5,000 ft/min), and calibration data shall
be taken at regular velocity intervals over this range
(see Citations 9 and 14 in Section 6 for details).
4.1.2.4 Two entry ports, one each for the standard
and Type S pitot tubes, shall be cut in the test section;
the standard pitot entry port shall be located slightly
downstream of the Type S port, so that the standard
and Type S impact openings will lie in the same cross-
sectional plane during calibration. To facilitate align-
ment of the pitot tubes during calibration, it is advisable
that the test section bo constructed of plexiglas or some
other transparent material.
4.1.3 Calibration 1'rocedure. Note that this procedure
is a general one and must not be used without first
referring to- the special considerations presented in Sec-
tion 4.1 5. Note also that this procedure applies only to
single-velocity calibration. To obtain calibration data
for the A aud D sides of the Type S pitot tube, proceed
as follows:
4.1.3.1 Make sure that the manometer is properly
filled and ttiat the oil is free from contamination and is of
the proper density. Inspect and leak-check all pitot lines;
repair or rpplaoe if ni1. e^ary.
4.1.3.2 Level and wro the manometer. Turn on the
tan and allow the flow to stabilize. Seal the Type S entry
port.
4.1.3.3 Ensure that the manometer Is level and teroed.
Position the standard pitot tube at the calibration point
(determined as outlined in Sction 4.1.5.1), and align the
tube so that its tip is pointed directly into the flow. Par-
ticular care should be taken in aligning the tube to avoid
yaw and pitch angles. Make sure that the entry port
surrounding the tube is properly sealed.
4.1.3.4 Read Aftm and record its value in a data table
similar to the one shown in Figure 2-9. Remove the
standard pitot tube from the duct and disconnect it from
the manometer. Seal the standard entry port.
4.1.3.5 Connect the Type S pitot tube to the manom-
eter. Open the Type S entry port. Check the manom-
eter level and zero. Insert and align the Type S pitot tube
so that its A side impact opening is at the same point as
was the standard pitot tube aud is pointed directly into
the How. Make sure that the entry port surrounding the
tube Is properly sealed.
4.1.3.6 Read Ap, and enter its value in the data table.
Remove the Type S pitot tube from the duct and dis-
connect it from the manometer.
4.1.3.7 Reiieat steps 4.1.3.3 through 4.1.3.6 above until
three pairs of Ap readings have been obtained.
4.1.3.8 Repeat steps 4.1.3.3 through 4.1.3.7 above for
the B side of the Type S pitot tube.
4.1.3.9 Perform calculations, as described in Section
4.1.4 below.
4.1.4 Calculations.
4.1.4.1 For each of the sii pairs of Ap readings (i.e.,
three from side A and three from side B) obtained m
Section 4.1.3 above, calculate the value of the Type 8
pilot tube cotliicient as follows:
FEDERAL REGISTER, VOL. 42, NO. 160—THURSDAY, AUGUST 18, 1977
-------
41766
PltOT TUBE IDENTIFICATION NUMBER:
CALIBRATED BY.'. :
RULES AND REGULATIONS
.DATE:.
RUN NO.
1
2
3
"A" SIDE CALIBRATION
' APstd
cm H20 '
(in. H20)
AP($)
emH20
(in. H20)
Cp (SIDE A)
Cp(s)
,
DEVIATION
Cp(s) • Cp(A)
RUN VO.
1
2
3
"B" SIDE CALIBRATION
Apstd
emH20
(in. H20)
AP(S)
cmH20
(ln.H20)
Cp (SIDE B)
Cp(s)
' DEVIATION
Cp(,)-Cp(B)
•
AVERAGE DEVIATION - o(AORB)
S jCp(j)-Cp(AORB)|
•MUSTBE from C, (slde_A),and the deviation of
each B-side value of C,M from C, (side B). Use the fol-
lowing equation:
Deviation = C,(,) — C,(A or B)
Equation 2-3
4.1.4.4 Calculate O)
Ap.=Veloclty head measured by the Type B pltot
tube, cm HiO (In. H|O)
4.13.2 Calculate C, (side A), the mean A-slde coef-
_ _ _
ftt.j-TypeSpflottabecoefficient ficient, and ff, (side B), the mean B-slde coefficient;
M) -Standard pltot tube coefficient; use 0.99 If the calculate the difference between these two average
coefficient b unknown and the tube la designed values.
o (side A or
Equation 2-4
4.1.4.5 Use the Type S pltot tube only if the values of
ff (side A) and a (side B) are less than or equal to 0.01
and if the absolute value of tho difference between Ct
(A) and Cp (B) is 0.01 or less.
4.1.5 Special considerations.
4.1.5.1 Selection of calibration point.
4.1.5.1.1 When an isolated Type S pitot tubo is cali-
brated, select a calibration point at or near the center of
the duct, and follow the procedures outlined tn Sections
4.1.3 and 4.1.4 above. The Type S pitot coefficients so
obtained, i.e., C, (side A) and ~C, (side B), will be valid,
so long as either: (1) the isolated pitot tube is used; or
(2) the pitot tube is used with other components (nozzle,
thermocouple, sample probe) in an arrangement that is
free from aerodynamic interference effects (see Figures
2-6 through 2-8).
4.1.5.1.2 For Type S pilot tube-thermocouple com-
binations (without sample probe), select a calibration
point at or near the center of the duct, and follow the
procedures outlined in Sections 4.1.3 and 4.1.4 above.
The coefficients so obtained will be valid so long as the
pitot tube-thermocouple combination is used by itself
or with other components in an interference-free arrange*
ment (Figures 2-6 and 2-8).
4.1.5.1.3 For assemblies with sample probes, the
calibration point should be located at or near the center
. of the duct; however, insertion of a probe sheath into a
small duct may cause significant cross-sectional area
blockage and yield incorrect coefficient values (Citation 9
in Section 6). Therefore, to minimize the blockage effect,
the calibration point may be a few inches off-center if
necessary. The actual blockage effect will be negligible
when the theoretical blockage, as determined by a
projected-area model of the probe sheath, is 2 percent or
less of the duct cross-sectional area for assemblies without
external sheaths (Figure 2-10a), and 3 percent or less for
assemblies with external sheaths (Figure 2-10b).
4.1.5.2 For those probe assemblies in which pilot
tube-nozzle interference is a factor (i.e., those in which
the pitot-nozzel separation distance fails to meet the
specification illustrated in Figure 2-6a), the value of
Cp(.) depends upon the amount of free-space between
the tube and nozzle, and therefore is a function of nozzle
size. In these instances, separate calibrations shall be
performed with each of the commonly used nozzle sizes
in place. Note that the single-velocity calibration tech-
nique is acceptable for this purpose, even though the
larger nozzle'sizes O0.635 cm or yt in.) are not ordinarily
used for isokinetic sampling at velocities around 915
m/min (3,000 ft/min), which is the calibration velocity;
note also that it is not necessary to draw an isokinetic
sample during calibration (see Citation 19 in Section 6).
4.1.5.3 For a probe assembly constructed such that
Itj pitot tube is always used in the same orientation, only
one side of the pitot tube need be calibrated (the side
which will face the flow). The pilot tube must still meet
the alignment specifications of Figure 2-2 or 2-3, however,
»nd must have an average deviation (a) value of 0.01 or
less (see Section 4.1.4.4).
FEDERAL REGISTER, VOL 42, NO. 160—THURSDAY, AUGUST 18, 1977
-------
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. 0
Date January 15, 1980
Page 10 of 11
ESTIMATED
SHEATH
BLOCKAGE
ElxW "I
UCTAREAJ
(b)'
x 100
Figure 2-10. Projected-area m.odels for typical pitot tube assemblies.
4.1.6 Field Use and Rccallbration.
4.1.6.1 Field Use.
4.1.6.1.1 When a Type 8 pilot tube (isolated tube or
assembly) is used in the field, the appropriate coefficient
value (whether assigned or obtained by calibration) shall
be used to perform velocity calculations. For calibrated
Type S pitot tubes, the A side coefficient shall be used
whon the A side of the tube faces the How, and the B side
coefficient shall be used when the B side faces the flow;
alternatively, the arithmetic average of the A and B side
coefficient values may be used, irrespective of which side
(aces the flow.
4.1.6.1.2 When a probe assembly is used to sample a
small duct (12 to 36 in. in diameter), the probe sheath
sometimes blocks a significant part of the duct cross-
section, causing a reduction in the effective value of
??„ (,). Consult Citation 9 in Section 6 for details. Con-
ventional pilot-sampling probe assemblies are not
recommended for use in ducts having inside diameters
smaller than 12 inches (Citation 16 in Section 6).
4.1.6.2 Becalibration.
4.1.6.2.1 Isolated Pitot Tubes. After each Held use, the
pitot tube shall be carefully reexammed in top, side, and
end views. If the pitot face openings are still aligned
within the specifications illustrated in Figure 2-2 or 2-3,
It can be assumed that the baseline coefficient of the pitot
tube has not ciianged. If, however, the tube has been
damaged to the extent that it no longer meets the specifi-
cations of Figure 2-2 or 2-3, the damage shall cither be
repaired to restore proper alignment of the face openings
or the tube shall bo discarded.
4.1.6.2.2 Pitot Tube Assemblies. After each field use,
check the face opening alignment of the pitot tube, as
in Section 4.1.6.2.1; also, rcmeasure the mtercomponerit
spacings of the assembly. If the intercomponent spacmgs
have not changed and the face opening alignment is
acceptable, it can be assumed that the coefficient of the
assembly has not (•hanged. If the face opening alignment
is no longer within tue speciJications of figures 2-2 or
2-3, either repair the damage or replace the pitot tube
(calibrating the new nsseinMy, if necessary). If the intrr-
componcnt spacings have changed, restore the original
spacmps or recalibrate the assembly.
4.2 Standard pitot tube (if applicable). If a standard
pitot tube is used for the velocity traverse, the tube shall
be constructed according to the criteria of Section 2.7 and
shall be assigned a baseline coefficient value of 0.99. If
the standard pitot tube is used as part of an assembly,
the tube shall be in an interference-free arrangement
(subject to the approval of the Administrator).
4.3 Temperature Oauges. After each field use, cali-
brate dial thermometers, liquid-filled bulb thermom-
eters, thermocouple-potentiometer systems, and other
gauges at a temperature within 10 percent of the average
absolute stack temperature. For temperatures up to
405° C (701° F), use an ASTM mercury-in-glass reference
thermometer, or equivalent, as a reference; alternatively,
either a reference thermocouple and potentiometer
(calibrated by NBS) or thermoinctric fixed points, e.g.,
ice bath and boiling water (corrected for barometric
pressure) may be used. For temperatures above 405° C
(761° F), use an NBS-calibrated reference thermocouplo-
potentiometer system or an alternate reference, subject
to the approval of the Administrator.
If, during calibration, the absolute temperatures meas-
ured with the gauge being calibrated and the reference
gauge agree within 1.5 percent, the temperature data
taken in the field shall be considered valid. Otherwise,
the poliutant emission test shall either be considered
invalid or adjustments (if appropriate) of the test results
shall be made, subject to the approval of the Administra-
tor.
4.4 Barometer. Calibrate the barometer used against
a mercury barometer.
5. Calculation!
Carry out calculations, retaining at least one extra
decimal figure beyond that of the acquired data. Round
oft figures after final calculation.
5.1 Nomenclature.
A - Cross-sectional area of stack, m' (ft1).
B«i=Water vapor in the gas stream (from Method 5 or
Reference Method 4), proportion by volume.
Cp=Pitot tube coefficient, dimensionless.
Kf = Pitot tube constant,
•U 07 — r(g/g-"i°Mf mm Hg )-]''»
sec L (°K)(mm H.O) J
for the metric system and
„, .„ ft_ r(lb/lh-mole)(in.nEQ-|'/»
sec L (°U)(in. HaO) J
for the English system.
Af
-------
RULES AND REGULATIONS
Section No. 3.1.10
Revision No. 0
Drta January 15, 1980
ppge 11 of 11
S. 8hlReh»r», R. T., W. F. Todd, and W. 8. Smllh.
Blfrnlflcnnc* of Errors In Stack Sampling Measurements
U.S. Environmental Protection Agency, Kcsenrch
Triangle Park, N.C. (Presented at ttie Annunl Meeting of
the Air Pollution Control Association, Bt. Louis, Mo.,
June 14-10, 1-.P70.)
4 Standard Method for Sampling Slacks for Paniculate
Mallrr. In: 1'I71 Hook o( ASTM Standards. Piirt 2S.
riilliulclphla, Pa. 1U7I. ASTM Designation 1) 'f.lM 71.
ft. Voiiiuinl, 3. K. Ktemi'iitary Fluid Mivlmiijcii. Nuw
York. John Wiley nnil Son*, liu< I'.>I7.
6. Fluid Motors-Their Theory and Application.
Amerli'iin Bocloty of Mocliiinhul Englneeri, Nuw York,
N.Y. l:i.vt.
7. AHII HAR Handbook of Pimdiitnentnli. I!I77. p. 708.
K. Annual llwk of AHTM Hliindurds, Part M. l'J74. p.
MH.
II. Viilliiro, K. K. Oiilili-lhiM fur Ty|w S IMIot Tnlxi
rallltr:illt)ii. 11.8. Knvlronmonlal Prolrcllon Atiency.
KcwiiH'li 'I'liumln I'urk, N.C. (PriMonlwl nl 1st Aniuial
MiHillnn, Hiniire Kvuluatlun Uwivty, Dujton, Ohio,
8i>|)li>niU-r IS, W7.V)
10. Vollarn, H. F. A Type 8 Pilot Tulw C.'alllirallon
Study. U H. KnvironnlcnttU Prolwlion An»ncy, Kim»-
sion Min H Punt
Tulx*. H H Knvlriiniiienlnl rriilivilon AKI-IICV, Knila-
mon Mfiksuii'iiicitl Hmncli, KfNiMiich TrliiMKio 1'urk,
N.C. Novi-mlH-r M70.
l:i. Volliuo, It K, An K/nluatlon of Hlmiln Vi-lm-lly
Citllhrahon 'I'i'flinitiiies a.1 a Moan.sof )>t-l<-roiliilnK TylMt
H Pilot Tlllii' ('iMiflliMi'iitii. H W. Klivlrnnmcnlal Prolir-
lion AKttury, Kutlhslon MfaMiifiut'iit llrtmdi, Hosuiu^ch
Tilaniile Pink N.C. Aiixnsl I'.I7S.
14 X'ollaro, It. K. Tim Use of Type S Pilot Tubes for
the MciiMinenipiitof Low V'elorlllea U.S. KnvironiniMilal
Prolecnon Anoitcy. Knilsslou Mi'i^un-im-nt Dninch,
Keararch Truumlu Park, N.C. November 1-J78.
15. 8milh, Miirvln L. Velocity Calllmillon of KPA
Tyiw Koun-e Knmpllnn Prolw. United TerhnoloxlM
ririmnillon, I'rait and Wlulroy Aircraft Division,
Kiwi Hurt ford. Conn. IU75.
18. \ ollnro, K. K. Ki»tT. K. and H. r. Pnnlthurxl. The Mi>it.suriri>itinon 1'ri-H.i I'.MKl
IK. Volliiro, K. K A Mirwyof (Vinimeri-lally Aviillulil*
Tn^lnniM-ntitllon f«r the Mni'UinMnmit of Ixtw-KunKO
«liw \ illiH'llu
-------
Section No. 3.1.11
Revision No. 0
Date January 15, 1980
Page 1 of 2
11.0 REFERENCES
1. Smith, F., D. E. Wagoner, and A. C. Nelson, Jr. Guide-
lines for Development of a Quality Assurance Program:
Volume I - Determination of Stack Gas Velocity and
Volumetric Flow Rate (Type S Pitot Tube).
EPA-650/4-74-005-a. February 1974.
2. Hamil, H. F. Laboratory and Field Evaluations of EPA
Methods 2, 6, and 7. Southwest Research Institute.
EPA Contract 68-02-0626. October 1973.
3. Hamil, H. F. and R. E. Thomas. Collaborative Study of
Method for the Determination of Particulate Matter
Emissions from Stationary Sources (Municipal Incinera-
tors). Southwest Research Institute. EPA-650/4-74-022.
July 1974.
4. Hamil, H. F. and R. E. Thomas. Collaborative Study of
Method for Determination of Stack Gas Velocity and
Volumetric Flow Rate in Conjunction with EPA Method 5.
Southwest Research Institute. EPA-650/4-74-033.
September 1974.
5. Hamil, H. F. and R. E. Thomas. Collaborative Study of
Particulate Emission Measurements by EPA Methods 2, 3,
and 5 using Paired Particulate Sampling Trains (Munici-
pal Incinerators). Southwest Research Institute
EPA-600/4-76-014.
6. Vollaro, R. F. A Survey of Commercially Available
Instrumentation for the Measurement of Low-Range Gas
Velocities. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park,
N.C. November 1976. (Unpublished Paper)
7. Vollaro, R. F. Guidelines for Type S Pitot Tube Cali-
bration. U.S. Environmental Protection Agency,
Research Triangle Park, N.C. (Presented at 1st
Annual Meeting, Source Evaluation Society, Dayton,
Ohio, September 18, 1975.)
8. Vollaro, R. F. The Use of Type S Pitot Tubes for the
Measurement of Low Velocities. U.S. Environmental
Protection Agency, Emission Measurement Branch,
Research Triangle Park, N.C. November 1976.
-------
Section No. 3.1.11
Revision No. 0
Date January 15, 1980
Page 2 of 2
9. Smith, F. and D. E. Wagoner. Guidelines for Develop-
ment of a Quality Assurance Program: Volume IV -
Determination of Particulate Emissions from Stationary
Sources. EPA-650/4-74-005-d. August 1974.
10. Quality Assurance Handbook for Air Pollution Measure-
ment Systems - Volume I, Principles. EPA-600/9-76-005.
March 1976.
11. Alexander, K. Thermocouple Calibration Procedure Evalu-
ation. U.S. Environmental Protection Agency, Emissions
Standards and Engineering Division, Research Triangle
Park, N.C. Source Evaluation Society Newsletter, June
1978.
-------
Section No. 3.1.12
Revision No. 0
Date January 15, 1980
Page 1 of 8
12.0 DATA FORMS
Blank data forms are provided on the following pages for the
convenience of the Handbook user. Many of these forms are taken
or adapted from EPA forms, Reference 1, and other references. No
documentation is given on these forms as it would detract from
their usefulness. The titles are also placed at the top of the
figure as is customary for a data form. In order to relate the
form to the text, a form number is given in the lower right-hand
corner, e.g., Form M2 - 2.5, indicates that the form is
Figure 2.5, the fifth figure in Section 3.1.2, of the written
description for Method 2 (M2). Future revisions of these forms,
if any, can be documented by 2.5A, 2.5B, etc. Seven of the data
forms listed below are included in this section. Four are in the
Method Highlights subsection as shown by the (MH) following the
form number.
Form Title
1.2 Example of a Procurement Log
1.7 Type S Pitot Tube Inspection Data Form
2.5 Pitot Tube Calibration Data
2.10 Stack Temperature Sensor Calibration Data Form
2.12 Differential Pressure Gauge Calibration Data Form
3.1 (MH) Pretest Sampling Checks
3.2 (MH) Pretest Preparations
4.1 Method 2 Gas Velocity and Volume Data Form
4.2 (MH) On-Site Measurements Checklist
5.1 (MH) Posttest Sampling Checks
8.1 Stack Gas Velocity and Volumetric Flow Rate
Determination Checklist to be Used by Auditor
-------
PROCUREMENT LOG
Item description
Quantity
Purchase
order
number
Vendor
Date
Ordered
?'
Received
Cost
Dispo-
sition
Comments
Quality Assurance Handbook M2-1.2
-------
TYPE S PI TOT TUBE INSPECTION DATA FORM
Pitot tube assembly level? _ yes _ no
Pitot tube openings damaged? _ yes (explain below) _ no
6 = _ °, A = _ cm (in.)
z = A sin y = cm (in.); <0.32 cm (
-------
PITOT TUBE CALIBRATION DATA
size (OD)
ID number
e S pitot tub
ibration: da
e ID number Cp(-td) ~
te performed by
A-Side Calibration
cm ( in . )
H2°
Aps,
cm (in. )
H2°
Average
c a
P(S)
DEV.b
B-Side Calibration
cm (in. )
H2°
Aps,
cm (in. )
H2°
Average
- r
\/Apstd _
cP(s)a
DEV.b
p(S)
DEV = CPO
Cp(A) - Cp(B) =
APC
- C , (must be £0.01)
(must be £0.01).
Quality Assurance Handbook M2-2.5
-------
STACK TEMPERATURE SENSOR CALIBRATION DATA FORM
Date
Thermocouple number
Ambient temperature
Calibrator
°C Barometric pressure
Reference: mercury-in-glass
other
in. Hg
Reference
point
number
Source
(specify)
Reference
thermometer
temperature,
°C
Thermocouple
potentiometer
temperature,
Temperature
difference,
Every 30°C (50°F) for each reference point.
3Type of calibration system used.
:F(ref temp, °C + 273) - (test thermom temp, °C + 273)
L ref temp, °C + 273
Quality Assurance Handbook M2-2.10
-------
DIFFERENTIAL PRESSURE GAUGE CALIBRATION DATA FORM
Gauge type
Scale
Serial or ID number
Gauge-oil manometer Ap
Differential pressure
gauge Ap
Pressure
difference
-------
METHOD 2 GAS1VELOCITY AND VOLUME DATA FORM
Plant and city
Run date
I
Sampling location
Clock
time
Run
number
Operator
Amb . temp . ,
°F
Bar. press . ,
in. Hg
Static press . ,
in. H20
Molecular
wt.
Stack inside dimension,
Diam. of side
1
in.
side 2
Pitot
tube (C
>)
Field data
Traverse
point
number
Position,
in.
Velocity
head
(ApJ,
in. H20
Stack temp . ,
°F
Cyclonic flow determination
Ap at 0°
reference
Average angle («)
Angle («)
which yields
a null Ap
Average of °c must be <10 degrees to be acceptable.
Quality Assurance Handbook M2-4.1
-------
STACK GAS VELOCITY AND VOLUMETRIC FLOW RATE
DETERMINATION CHECKLIST TO BE USED BY AUDITOR
Yes
No
Operation
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
Presampling preparation
Knowledge of process conditions
Calibration of pertinent equipment prior
to each field tests
On-site measurements
Pitot tube meets geometry requirements
Manometer should be carefully leveled and
the liquid column set exactly on zero
Check for cyclonic flow
Leak check after sample run
Sampling port adequately plugged
Process at correct operating level
Pitot tube properly aligned along its
roll and pitch axes throughout the
traverse
Pitot tube frequently cleared when
measuring in a dust-laden gas
Manometer has the correct sensitivity
Staying at each traverse point long enough
for the system to stabilize
Measuring the stack gas static pressure
and temperature
Posts ampling
All information recorded on data form as
obtained
Any unusual conditions recorded
Independent check of calculations
Temperature sensor calibrated
COMMENTS
Quality Assurance Handbook M2-8.1
-------
Section No. 3.2
Revision No. 0
Date January 15, 1980
Page 1 of 8
Section 3.2
METHOD 3 - DETERMINATION OF CARBON DIOXIDE, OXYGEN,
EXCESS AIR, AND DRY MOLECULAR WEIGHT
OUTLINE
Number
Section Documentation of Pages
SUMMARY 3.2 2
METHOD HIGHLIGHTS 3.2 5
METHOD DESCRIPTION
1. PROCUREMENT OF APPARATUS AND
SUPPLIES 3.2.1 15
2. CALIBRATION OF APPARATUS 3.2.2 4
3. PRESAMPLING OPERATIONS 3.2.3 6
4. ON-SITE MEASUREMENTS 3.2.4 12
5. POSTSAMPLING OPERATIONS 3.2.5 2
6. CALCULATIONS 3.2.6 3
7. MAINTENANCE 3.2.7 I
8. AUDITING PROCEDURE 3.2.8 5
9. RECOMMENDED STANDARDS FOR
ESTABLISHING TRACEABILITY 3.2.9 1
10. REFERENCE METHOD 3.2.10 3
11. REFERENCES 3.2.11 1
12. DATA FORMS 3.2.12 6
-------
Section No. 3.2
Revision No. 0
Date January 15, 1980
Page 2 of 8
SUMMARY
In this procedure, a gas sample is extracted from a stack
by one of the following methods: single-point grab sampling;
single-point integrated sampling; or multipoint integrated
sampling. The gas sample is then analyzed for carbon dioxide
(C02), oxygen (O?)' an<* if necessary carbon monoxide (CO).
Depending on the desired accuracy of the subsequent analysis,
either an Orsat or other type of gas absorption analyzer such as
a Fyrite analyzer may be used for the analysis.
This method is used for determining CO2 and 0- concentra-
tions >0.2% by volume and for calculating excess air and the dry
molecular weight of gas streams from combustion processes. The
method may also be applicable to other processes where it has
been determined that compounds other than C02, 02/ CO, and nitro-
gen (N2) are not present in concentrations sufficient to affect
the results. Sulfur dioxide (SO?), for example, can affect CO2
readings since it would be absorbed with the C02.
Other methods and modifications to measure these consti-
tuents include: a multipoint sampling method using an Orsat
apparatus to directly analyze individual grab samples obtained at
each point; assigning a value of 30.0 for dry molecular weight,
in lieu of actual measurements for processes burning natural gas,
coal, or oil; or a method using CO2 or O2 and stoichiometric cal-
culations to determine dry molecular weight and excess air.
These methods and modifications may be used, but are subject to
the approval of the administrator, U.S. Environmental Protection
Agency.
The Method Description which follows is based on the Re-
ference Method promulgated on August 18, 1977. A complete copy
Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
-------
Section No. 3.2
Revision No. 0
Date January 15, 1980
Page 3 of 8
of the Reference Method is in Section 3.2.10 of this document,
and data forms are provided in Section 3.2.12 for the convenience
of the user. Reference 1 was largely used in preparing the
Method Description. References 2 through 5 summarize collabora-
tive test studies of the method and other related methods. Data
from these test studies are used to the extent possible in estab-
lishing quality control limits.
-------
Section No. 3.2
Revision No. 0
Date January 15, 1980
Page 4 of 8
METHOD HIGHLIGHTS
Specifications described in this method (Section 3.2) are
for determining excess air and dry molecular weight of gas
streams from fossil-fuel combustion processes. This method may
also be applicable to other processes where it has been deter-
mined that compounds other than CO2, O-, CO, and N2 are not
present in sufficient concentrations to affect the results. A
gas sample is extracted from a stack by one of the following
methods: (1) single-point grab sampling; (2) single-point in-
tegrated sampling; or (3) multipoint integrated sampling. The
gas sample is analyzed for percent CO~, percent O~f and if
necessary percent CO.
Determination of dry molecular weight can be made using
either an Orsat or Fyrite analyzer and any of the three sampling
methods listed above. When using the single-point grab sampling
or single-point integrated sampling methods, the sampling point
should either be at the centroid of the cross section or at a
point >1.00 m (3.3 ft) from the stack wall, unless otherwise
specified by the administrator. The sample collected for molec-
ular weight determination must be analyzed within 8 h of collec-
tion.
Excess air or emission rate correction factors must be
determined using an Orsat analyzer and the sample collection pro-
cedure specified in the applicable subpart of the standard. When
using the single-point grab or single-point integrated sampling
method, the sampling point should be located as specified above
for molecular weight determinations. When using the multipoint
integrated sampling method, a minimum of eight and nine traverse
points should be used for circular and rectangular stacks,
Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
-------
Section No. 3.2
Revision No. 0
Date January 15, 1980
Page 5 of 8
respectively, with diameters <0.61 m (24 in.). A minimum of 12
traverse points shall be used for all other cases. The sampling
run must be simultaneous with and for the same total length of
time as the pollutant emission rate 'determination. The Orsat
analyzer must be leak checked before and after the analysis.
When analyzing low concentrations of C02 (<4.0%) or high concen-
trations of Op (>15.0%), the measuring burette of the Orsat must
have at least 0.1% subdivisions. The sample must be analyzed
within 4 h of collection.
The Method Highlights checklist at the end of this section
may be removed from the Handbook and used in pretest, test, and
posttest operations. Each form has a subtitle (i.e., Method 3,
Figure 3.1) to aid the user in finding a similar filled-in form
in the Method Description. Each item on the checklist that can
cause significant errors are designated with an asterisk. Most
of the Method Description and forms are designed for use in
calculating excess air corrections, and therefore contain many
more controls than would be required for molecular weight
determination only.
1. Procurement of Equipment
Section 3.2.1 (Procurement of Apparatus and Supplies) gives
the specifications, criteria, and design features of the equip-
ment and materials required to perform Method 3 tests. This sub-
section is designed to provide the tester with a guide for the
procurement and initial check of equipment and supplies. The
activity matrix (Table 1.1) at the end of Section 3.2.1 can be
used as a quick reference, and is a summary of the corresponding
written descriptions.
2. Pretest Preparations
Section 3.2.2 (Calibration of Apparatus) provides a step-by-
step description of the recommended calibration procedure for the
Orsat analyzer and the flow rate meter.
Section 3.2.3 (Presampling Operations) provides the tester
with a guide for supplies and equipment preparation for field
-------
Section No. 3.2
Revision No. 0
Date January 15, 1980
Page 6 of 8
tests. The method for packing and the description of packing
containers should help protect the equipment but are not required.
3. On-site Measurements
Section 3.2.4 (On-site Measurements) contains procedures for
sampling and analysis. Subsection 4.1 outlines the step-by-step
procedure for determination of dry molecular weight. Subsection
4.2 outlines the step-by-step procedure for determination of
excess air and emission rate correction factor. Subsection 4.3
includes a list of precautions that will aid in using the Orsat
analyzer and improve the validity of the results.
4. Posttest Operations
Section 3.2.5 (Postsampling Operations) outlines a data
comparison procedure which will allow detection of gross measure-
ment error. A visual inspection procedure is also included to
detect any change in the sampling and analysis apparatus that
could have adversely affected the measured values.
Section 3.2.6 (Calculations) provides the tester with the
required equations and nomenclature for calculating percent
excess air and dry molecular weight.
Section 3.2.7 (Maintenance) outlines the necessary equipment
maintenance which will help ensure high quality data.
5. Auditing Procedure
Section 3.2.8 (Auditing Procedure) provides a description
of necessary activities for conducting performance and system
audits. The performance audit of the analytical phase can be
conducted using certified gas samples. Auditing procedures for
the analytical, data processing, and systems phases are de-
scribed in this section. A checklist for a systems audit is also
included in this section.
Section 3.2.9 (Recommended Standards for Establishing Trace-
ability) recommends the primary standards for use in assessing
the accuracy of test data.
6. References
Sections 3.2.10 and 3.2.11 contain the Reference Method and
the suggested references.
-------
Section No. 3.2
Revision No. 0
Date January 15,
Page 7 of 8
1980
PRETEST PREPARATIONS
(Method 3, Figure 3.1)
Apparatus check
Probe type:
Borosilicate
glass
Stainless
steel
Other
Filter
In-stack
Out-stack
Glass wool
Other
Pump
One-way
squeeze
Diaphram
Other
Leak
checked*
Condenser
Type
Flexible Bag
Tedlar
Mylar
Teflon
Other
Leak
checked*
Pressure Gauge
Type
Analyzer
Orsat
Fyrite
Other
Leak
checked*
Spare
reagents
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Loaded
and packed
Yes
No
*Most significant items/parameters to be checked.
-------
Section No. 3.2
Revision No. 0
Date January 15, 1980
Page 8 of 8
ON-SITE MEASUREMENTS CHECKLIST
(Method 3, Figure 4.1)
Sampling
Method: single-point grab single-point integrated
multipoint integrated
Is a filter used to remove particulate matter?
*Sampling train leak checked?
*0rsat analyzer leak checked?
All connections tight and leak free?
Sampling port properly sealed?
Sampling rate held constant?
Sampling train purged?
Analysis
Molecular Weight Determination
Analyzer: Orsat Fyrite Other
Fyrite:
Reagent at proper level and zeroed?*
Leak-free connection between analyzer and sample line?
Sampling line purged?*
Orsat:
Reagents at proper level?*
Analyzer level?
Leak checked?*
Sample analyzed within 8 h?*
Sample lines purged?*
Excess Air-Emission Rate Correction
Orsat analyzer leak checked?* Before After
Reagents at proper level?*
Sampling lines purged?*
Analysis repeated by drawing a new sample until the following
criteria are met?
C0_ - any three analyses differ by
a) £0.3% when CO, ^4.0%
b) £0.2% when CO^ £4.0%
O9 - any three analyses differ by
1
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 1 of 15
1.0 PROCUREMENT OF APPARATUS AND SUPPLIES
Diagrams of the sampling trains used in the method are shown
in Figures 1.1 and 1.2. Specifications, criteria, and/or appli-
cable design features are given in this section to aid in the
selection of equipment to assure the collection of good quality
data. Procedures and, where applicable, limits for acceptance
checks are given. During the procurement of equipment and sup-
plies, it is suggested that a procurement log be used to record
the descriptive title of equipment, the identification number (if
applicable), and the results of acceptance checks. An example
procurement log is shown in Figure 1.3; a blank form is given in
Section 3.2.12 for the user. If calibration data are required as
part of the acceptance check, the data should be recorded in a
calibration log. Table 1.1 at the end of this section contains a
summary of the quality assurance activities for procurement and
acceptance of apparatus and supplies.
As alternatives to the sampling systems described herein,
others (e.g., liquid displacement) may be used if they are capa-
ble of obtaining a representative sample, maintaining a constant
sampling rate, and yielding acceptable results. Use of such
systems is subject to the approval of the administrator.
1.1 Grab Sample (Figure 1.1)
1.1.1 Probe - The probe or probe liner should be made of stain-
less steel or borosilicate glass tubing and should be equipped
with an in-stack (preferred) or an out-stack filter to remove
particulate matter. A plug of glass wool is generally a satis-
factory filter. The probe tip should be designed to prevent the
glass-wool filter from being drawn from the probe when sampling a
source that has a substantial negative pressure. Any material
inert to O^, CO-, CO, and N2 and resistant to temperature at the
sampling conditions may be used for the probe; examples of such
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 2 of 15
PROBE
FLEXIBLE TUBING
FILTER (GLASS WOOL)
TO ANALYZER
SQUEEZE BULB
Figure 1.1 Grab sampling train.
RATE METER
PROBE
\
AIR-COOLED
CONDENSER
FILTER •
(GLASS WOOL)
QUICK DISCONNECT
_n
RIGID CONTAINER
Figure 1.2 Integrated gas sampling train.
-------
Item description
*-**
Quantity
i
Purchase
order
number
—j -^ijo | iCi
«X<=»< 1<5 1 "
Vendor
fjccw -loc,.
Date
Ordered
7y^V'^9
Received
^?J/5"/'^9 ?
Cost
Dispo-
sition
Jo Service
Comments
•"d G 5d co
^) Q) (P CD
vQ ft < O
(D H- rt
tn H-
W O H-O
030
Hi C Z
Figure 1.3 Example of a procurement log.
U)
•
N)
VD
CX>
O
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 4 of 15
p
materials are aluminum, steel, glass, PVC plastic, and Teflon .
Since the gases to be sampled are relatively inert, the key
criterion in probe selection is the stack gas temperature.
1.1.2 Pump - A one-way squeeze bulb, or the equivalent, is used
to draw the gas sample into the analyzer.
1.2 Integrated Sample (Figure 1.2)
1.2.1 Probe - A probe equipped in the manner just described in
Subsection 1.1.1 is suitable.
1.2.2 Condenser - An air or water-cooled condenser that will not
remove O2, CO-, CO, and N« should be used to remove excess mois-
ture if the gas stream contains >2% moisture by volume. (This
includes most combustion processes.) The main consideration is
that the condenser volume be kept to the minimum size necessary
to sufficiently cool the sample gas, because the larger the
volume the more difficult it is to completely purge the sampling
train before collecting a sample. A 0.63-cm (0.25-in.) stainless
steel coil or equivalent connected to a water collection chamber
with a capacity of about 40 ml is sufficient.
1.2.3 Valve - Needle valves are needed to adjust the sample gas
flow rate.
1.2.4 Pump - A leak-free diaphragm pump, or the equivalent, is
needed to transport the sample gas to the flexible bag. A small
surge tank should be installed between the pump and the rate
meter to eliminate the pulsation effect of the pump on the rate
meter. Upon receipt, the pump, surge tank, and rate meter (Sub-
section 1.2.5 below) should be checked in the following manner:
1. Assemble the pump, surge tank, and rate meter.
2. Place a needle valve and vacuum gauge at the pump inlet
using a T-connector.
3. Turn on the pump and close the needle valve until a
vacuum of 125 mm (5 in.) Hg is obtained. The pumping rate at
3
this vacuum is suggested to be at least 1 £/min (0.035 ft /min),
Registered trademark.
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 5 of 15
and the rate meter when the flow is adjusted between 0.5 and
1.0 £/min (0.018 and 0.035 ft3/min) should yield steady readings.
If the pump capacity is insufficient, repair, replace, or
return it to the manufacturer. If rotameter readings fluctuate
>2% of the full-scale reading, use a larger surge tank. Be sure
that the rotameter is clean and dry.
1.2.5 Rate Meter - A rotameter or an equivalent rate meter,
capable of measuring flow rates within ±2% of the selected flow
rate should be used.
The calibration curve (Figure 1.4) supplied by the manufac-
turer should be checked by comparing the rotameter readings
against the wet test meter readings. If the rotameter is not
within ±5% of the manufacturer's calibration curve, recalibrate
and construct a new curve.
Changes in sample gas pressure, density, and viscosity will
affect the sampling rate. However, since sampling is performed
at a constant rate and since the total volume sampled need not be
measured accurately, these changes are not significant.
1.2.6 Flexible Bag - Any leak-free inert plastic (e.g., Tedlar ,
R R
Mylar , Teflon ) bag, or the equivalent, having a capacity ade-
quate for the selected flow rate and time length of the test run
may be used. A capacity of 90 £ (3.2 ft ) is usually required.
To leak check the bag (Figure 1.5):
1. Connect it to a manometer and pressurize the bag to
from 5 to 10 cm (2 to 4 in.) H2O.
2. Allow it to stand for 10 min.
Any displacement in the water manometer will indicate a leak
and a need to repair the bag. An alternative leak check is to
pressurize the flexible bag to 5 to 10 cm (2 to 4 in.) H2O and
allow it to stand overnight. A deflated bag indicates a leak.
1.2.7 Pressure Gauge - A water-filled U-tube manometer, or the
equivalent, of about 28 cm (12 in.) is needed for the flexible
Registered trademark.
-------
100
o
<
0.5 1.0
SAMPLING RATE, £/min at 21°C and 760 mm Hg
l~d O pd w
su pj (p fj)
vQ rt < o
ft H- rt
tn H-
o\ ^i H- o
Figure 1.4 Example rotameter calibration curve,
01 *<
CO
oo
o
-------
MANOMETER
TO AIR
PRESSURE
SOURCE
INERT PLASTIC BAG
Q) PJ CD CD
iQ ft < O
0) fD H- rt-
cn H-
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 8 of 15
bag leak check. The gauge should be leak checked upon receipt as
follows:
1. Place a flexible tube on the gauge opening.
2. Apply a positive pressure of from 5 to 10 cm (2 to
4 in. ) IL-jO on the gauge by blowing on and then pinching off the
tube. The pressure reading should remain stable for 10 min.
3. Check each side of the gauge separately.
If a deflection is noted, repair, replace, or return the
gauge to the manufacturer.
1.2.8 Vacuum Gauge - A mercury manometer, or the equivalent, of
at least 760 mm (30 in.) Hg is needed for the sampling train leak
check. If a mercury manometer is used, leak check the system by
pulling a 380 mm (15 in.) Hg vacuum on the gauge and then pinch-
ing off the tube. No deflection should be noted in the reading
over a 10-min period. If another type of gauge is used, compare
the gauge reading with a mercury manometer reading at about 380
mm (15 in.) Hg. The gauge reading should be within ±25 mm
(1 in.) Hg of the mercury manometer reading. If the gauge fails
the leak check or the comparison with the mercury manometer,
repair, replace, or return the manometer to the manufacturer.
1.3 Analyzer
An Orsat or a similar absorption type analyzer is required
for measuring constituents of combustion gases. The latter is
used only for molecular weight determinations, since it is less
accurate than tho Orsat.
f~ r~j
1.3.1 Orsat Gas Analyzer - The Orsat analyzer ' is used to
determine the CO^, 02, and CO stack gas concentrations. A sample
is analyzed by successively passing it through absorbents that
remove specific gaseous components. The difference in gas volume
before and after the absorption represents the amount of the con-
stituent gas in the sample. Constant pressure and temperature
must be maintained throughout the analysis. Results are reported
as dry volume percentages.
The Orsat analyzer illustrated in Figure 1.6 includes a
glass burette to accurately measure the gas volume, a water
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 9 of 15
/THREE-MAY INLET VALVE TO MANIFOLD
/INLET VALVE TO CO PIPETTE
SAMPLE
INLET
SIDE VIEW OF TYPICAL
PIPETTE ABSORBER
INLET VALVE TO 02 PIPETTE
yINLET VALVE TO C02 PIPETTE
MARKS
l>
FMOSPHERE
IENCE— f
si/c ^
J S
r ,.._,
j
^
>
7(
LEVELING
BOTTLE
70 ml
VOLUME
^^•WATER
l-r^ JACKET
•MANIFOLD
VOLUME
-REFERENCE
MARK
CONFINING
FLUID
Figure 1.6 Orsat apparatus.
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 10 of 15
jacket to maintain constant temperature, a manifold to control
the gas flow, three absorption pipettes (CO, 0-, and C02), rubber
expansion bags, and a liquid-filled leveling bottle to move the
gases. The apparatus is usually assembled inside a case that has
front and rear doors and a carrying handle.
For expected C02 readings >4.0%, a standard Orsat analyzer
containing a burette with 0.2-ml divisions and spacings between
divisions of about 1 mm (0.04 in.) is satisfactory. For lower
C02 values or for 0,, values >15%, an analyzer equipped with a
burette having 0.1-ml divisions with spacings of >_1 mm (0.04 in.)
should be used.
Upon receipt of the analyzer, wash and dry all components
and assemble the apparatus according to the manufacturer's in-
structions. Then properly lubricate all glass valves with sili-
cone stopcock lubricant. If the apparatus is to be used prompt-
ly, add the liquid reagents and check for leaks as follows:
1. Allow the apparatus to reach ambient temperature with
the manifold valve open and the three pipette valves closed.
2. Bring the liquid in each absorption pipette up to the
reference mark by opening the pipette valves one at a time and by
slowly lowering the leveling bottle. Pinch off the rubber tube
to the leveling bottle with the heel of the hand to quickly stop
liquid flow. Close the pipette valves.
3. Displace the indicating fluid until a reading is ob-
tained in the narrow part of the burette, and quickly close the
manifold inlet valve.
4. Place the leveling bottle on top of the Orsat case, and
read the meniscus in the burette.
5. Wait at least 4 min; then read the meniscus again. A
change of >_0.2 ml in the reading indicates a leak in the system
which must be repaired. A drop in reagent level to below the
capillary tube over a 4-min period indicates a leak in that
pipette.
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 11 of 15
If leaks are detected, correct them so that the above cri-
teria will be met.
Desirable Design Qualities - There is a variety of Orsat
analyzer designs on the market. Some design features increase
the precision and accuracy. Some of these desirable features are
described below.
Precision and probably accuracy are improved with a glass
burette configuration as shown in Figure 1.6; that is, the
burette column has a large diameter having a volume of about 70
ml joined onto a narrow 30-ml burette graduated in 0.1-ml divi-
sions. Such designs result in less error in reading the gas
volume than with designs having larger graduations and less
spacing between divisions. To further reduce reading error, the
volume line should be scribed completely around the burette at
the reference point. For processes in which CO2 is released from
the product (e.g., in a limestone kiln), the cumulative total of
()„ and C0~ may be >25%. For these processes, the graduated
portion of the burette must be long enough to provide a reading.
(Graduated burettes are available up to 100 ml.) A burette with
a vertical dark line behind the graduations is easier to read.
The volume reference mark should be on the capillary tube at
the top of the glass burette, not on the larger diameter burette.
Having the mark on the small capillary tube increases the preci-
sion from test to test and increases the accuracy of the burette
calibration—both for a more accurate sample volume determina-
tion.
The connecting manifold should have as small a volume as
possible to reduce the possibility of diluting the sample due to
incomplete purging of the manifold. It also minimizes the in-
crease in sample volume; the volume of gas in the manifold be-
tween the reference mark on the burette and that on the pipette
is small.
These burettes are commercially available.
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 12 of 15
The Orsat apparatus and case should be designed so that the
leveling bottle and the glass burette can be viewed side by side
when leveling the liquid. The liquid levels in both the burette
and the bottle must be at the same height when reading the
volumes; otherwise, the sample gas will not be at atmospheric
pressure.
The inlet manifold valve should be three-way to allow purg-
ing of the manifold without causing the sample bag or the inlet
gas to be diluted by ambient air.
Reagents - Four reagents are required by a standard Orsat
apparatus for analyzing flue gas. These are the gas-confining
solution, the C0? absorbent, the O? absorbent, and the CO absorb-
ent. Due to the solubility of CO- in water, a colored aqueous
acidic salt solution is used as the confining solution; it con-
tains sodium sulfate, sulfuric acid, and methyl orange. The CO
absorbent is a solution of potassium or sodium hydroxide, and the
0- absorbent is a solution of alkaline pyrogallic acid or
chromous chloride. The CO absorbent is usually a cuprous
chloride or sulfate solution, but other solutions may be used.
All of these solutions can be purchased from most chemical sup-
pliers. Note the shelf-life requirements, since some reagents
deteriorate with time.
1.3.2 Other Absorption Type Analyzers - Absorption type
analyzers which determine CO? or O_ concentrations are also
available. These devices are simpler and easier to use than an
Orsat, and they are more rugged. However, they provide less
precision and can thus be used only for molecular weight determi-
nations of the gases. These devices operate similarly to the
Orsat by absorbing the gas in a colored solution; then the volume
absorbed is read directly on a scale as percentage by volume. A
commonly used 02 analyzer is shown in Figure 1.7. The use of
continuous monitors for determining 02 content must be approved
by the administrator.
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 13 of 15
ONE-WAY
SQUEEZE BULB
GLASS WOOL
FILTER
GAS ABSORBER
PROBE
Figure 1.7 Absorption type analyzer.
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 14 of 15
Table 1.1 ACTIVITY MATRIX FOR PROCUREMENT OF APPARATUS AND
SUPPLIES
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Grab Sampling
Train
Probe
Stainless steel, boro-
silicate glass, or
equivalent; not damaged
or corroded; no
leakage
Visual observation
upon receipt
Discard or
return defec-
tive equipment
to supplier,
as appropriate
Pump
One-way squeeze bulb
or equivalent; not
damaged or corroded
As above, plus
manual operating
check
As above
Integrated Gas
Sampling Train
Probe
Stainless steel, boro-
silicate glass, or
equivalent; no leakage
As above
As above
Air-cooled
condenser
No leakage; keep the
condenser volume to a
minimum necessary to
cool the sample with
As above
As above
air
Valve
Needle valve
As above
As above
Pump
Diaphragm type, leak
free, and 1 £/min (0.035
ft /min) capacity
Check for leaks and
capacity upon receipt
As above
Rate meter
(rotameter)
Check flow range from
0 to 1 £/min (0 to
0.035 ft /min) must be
accurate to within ±2%
of selected flow rate
Check upon receipt
for damage; calibrate
against WTM
Recalibrate
and construct
new calibration
curve
Flexible bag
Capacity of 55-to 90 SL
(1.9 to 3.2 ft ); leak
test not mandaotry
Check for leaks and
capacity
Return to
supplier
(continued)
-------
Section No. 3.2.1
Revision No. 0
Date January 15, 1980
Page 15 of 15
Table 1.1 (continued)
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Pressure gauge
28-cm (12-in.) water-
filled U-tube or equiv-
alent for flexible bag
leak check
Visually observe and
leak check upon
receipt
As above
Vacuum gauge
At least 760-mm (30-in.)
Hg gauge for the sam-
sampling train leak
check
Check against a mer-
cury U-tube manometer
and leak check
As above
Orsat Analyzer
Glass burette
0.1-ml divisions with
spacings of about 1mm
Visually inspect
upon receipt
Return to
supplier
Pipettes, mani-
folds, etc.
Air tight
Initially and before
tests
Repair or
discard
Leveling bottle
Can be viewed side-by
side with glass burette
Visually check for
damages
As above
Other Analyzers
<0.5% divisions
Visually check for
damage and leaks
As above
-------
Section No. 3.2.2
Revision No. 0
Date January 15, 1980
Page 1 of 4
2.0 CALIBRATION OF APPARATUS
Calibration of sampling apparatus is one of the most
important functions in maintaining data quality. Only limited
initial calibration is required for gas absorption using an
analyzer such as an Orsat. Continued maintenance, reagent
checks, and most importantly, the operator's technique and dili-
gence are required for good quality data. Table 2.1 at the end
of this section summarizes the quality assurance activities for
calibration.
2.1 Analyzers
Calibration is recommended upon receipt, before every third
field test, and before any field test in which the Orsat or other
absorption type analyzer has not been checked during the previous
3 mo.
To check the 0~-absorbing reagent and the operator's techni-
que, the percentage of 02 in air should be determined. The
average of three replicates should be 20.8 ±0.7% when using the
standard Orsat. A measured average value >21.5% generally
indicates poor operator technique, while a value <20.1% generally
indicates leaking valves, spent absorbing reagent (for 02 only),
and/or poor operator technique. (See Section 4.1 of Reference 1
for the derivation of the above limits.) The three replicates
and their averages should be reported on an X and R chart, as
illustrated by Figure 2.1; a blank copy of this form is in Sec-
tion 3.2.12.
A more thorough check, if required equipment is available,
would be to take a sample from a manifold containing a known
mixture of C02 and 02. This is applicable to grab samples or to
the integrated samples. In both cases, the sample is analyzed
for C02 and 02 using the Orsat. The average of three replicates
should be ±0.5% (absolute) of the known concentration of each
gas. Again, high measured values indicate poor operator techni-
que, while low values indicate leaking valves, spent absorbing
reagent, and/or poor operator technique.
-------
(D
NJ
M
X
O
Hi
OJ
XI
0)
O
tr
OJ
H
rt
Comments
(Correct RANGES,
Action,
• tc.)
"77 1 1 *
NBA? J_ J-L_
<9/esa O
— . M
* *
r.
1 cs-
^t-
0
T «j^
0
T °«
[._ , ^>
j. ^ s - 9>
, - ' c 0>
I ^
BJ
^
°»
1 m
1 w^
^
T ^
° ^A
- ?
- *j
i
^*
1<
"
w
_
•*
—
*
. H
**
. '
•
i _
"*
E>
-
/^
-
•*
AVERAGED
t
k
<»i
K
Co
•<>
^
i.-.
1
^
£
t
VI
c
c.
-o
»;
"\
S":
«\
?^
1
1
s
5:
L-
1-
6
1
MEASUREMENT
RESULT
w
J
^>
G"
^
~0
Si-.
Cv>
1
b
1
^
i
1
^
»
VB
^
«^>
Sb
k
io
^>
"*•
^
1'
«v
le
1
t^
->si
O
**»
(V
•<
'A
^
^
\
CB
£
Sc
^
^
CODE
w
\
Kl
\
t-
H
V
^i
t
^
J\
^
^_
^
O
9
o\
\
"I
H
s
(f\
5s
r
^
&>
J^
1
•o
PI
1
1
i
H
Ift
>
rv
^
I!!
>:
0861 '<
jo
0 'ON UOTSTASH
*e 'ON
-------
Section No. 3.2.2
Revision No. 0
Date January 15, 1980
Page 3 of 4
If the above limits are exceeded, corrective action should
be equipment maintenance and/or operator training.
2.2 Rate Meter
Clean and calibrate the rate meter in the integrated gas
sampling train every 6 mo and at any sign of erratic behavior.
Calibrate using either a wet test meter or a volume meter which
has been recently calibrated against a primary standard.
1. Place the calibrated volume meter or wet test meter in
series with the rate meter.
3
2. Adjust the flow rate to 1 £/min (0.035 ft /min) on the
rate meter.
3. Take readings with the wet test meter and stopwatch.
3
If the flow rate is not near the desired 1 £/min (0.035 ft /min)
on the rate meter, adjust the valve and repeat the reading with
the wet test meter and stopwatch; repeat until the desired flow
rate is obtained for the rate meter setting.
4. Take readings at 0.5, 0.75, and 1.0 £/min (0.18, 0.027,
and 0.035 ft /min) on the rate meter. Record the readings from
the calibrated meter and the rate meter in the calibration log.
5. Construct a calibration curve of rate meter reading
versus flow rate for the meter using corrected wet test meter
stopwatch readings.
6. Number each rate meter and include the number and the
date of calibration on the calibration curve.
-------
Section No. 3.2.2
Revision No. 0
Date January 15, 1980
Page 4 of 4
Table 2.1 ACTIVITY MATRIX FOR THE CALIBRATION OF APPARATUS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Orsat analyzer
Average of three repli-
cates should be 20.8
±0.5% (absolute) or
known concentration
±0.5 (absolute)
Upon receipt and
before any test in
which the analyzer
has not been checked
during the previous 3
mo; determine % 0 in
ambient air, or use
a calibration gas
with known CO, CCL,
CL concentrations
Check Orsat
analyzer for
leaking valves,
spent absorbing
reagent, and/or
operator tech-
niques; take
corrective
action
Rotameter or
rate meter
Smooth curve of rotame-
ter actual flow rates
with no evidence of
error
Check with wet test
meter or volume
meter at 6-mo inter-
vals or at indica-
tion of erratic
behavior
Repeat cali-
bration steps
until limits
are attained
-------
Section No. 3.2.3
Revision No. 0
Date January 15, 1980
Page 1 of 6
3.0 PRESAMPLING OPERATIONS
The quality assurance activities for presampling operations
are summarized in Table 3.1 at the end of this section. See Sec-
tion 3.0 of this Handbook for details on site selection.
3. 1 Apparatus and Calibration Checks
Figure 3.1 or a similar form is recommended to aid the
tester in preparing an equipment checklist, status report form,
and packing list.
3.1.1 Grab Sample Train - The grab sample train (Figure 1.1)
should be checked before each field test as follows:
1. Clean the probe with soap and water, rinse it with
water, and allow it to dry. Check it visually for leaks indi-
cated by cracks or corrosion. Cap both ends of the probe tightly
to prevent contaminants from entering while it is not in use. If
particulates are expected, insert a plug of glass wool into the
sampling end of the probe.
2. Check the pump—either a one-way squeeze bulb or a
leak-free diaphragm type pump—to see if it is operating prop-
erly. Check all connectors and tubes for leaks; do this by
slightly pressurizing the system and by applying soap to the
connections and joints and watching for bubbles.
3.1.2 Integrated Sample Train - The integrated gas sampling
train (Figure 1.2) should be checked before each field test as
follows:
1. Clean the probe with soap and water, rinse it with
water, and allow it to dry. Visually check it for leaks indi-
cated by cracks or corrosion. Cap both ends of the probe tightly
to prevent contaminants from entering it while it is not in use.
If particulates are expected, insert a plug of glass wool into
the sampling end of the probe.
2. Clean the air-cooled condenser, or equivalent, and leak
check it by slightly pressurizing the unit, applying soap to
joints and connections, and watching for bubbles.
-------
Section No. 3.2.3
Revision No. 0
Date January 15, 1980
Page 2 of 6
Apparatus check
Probe type:
Borosilicate
glass
Stainless ,
steel i/
Other
Filter
In-stack /
Out-stack
Glass wool
Other
Pump
One-way
squeeze
Diaphram x/"
Other
Leak
checked*
Condenser
Type OUL GOO&C*
Flexible Bag
Tedlar
Mylar ^
Teflon
Other
Leak
checked* ^^p
X7~
Pressure Gauge
Type uJL JiJis-*-
Analyzer
Orsat y
Fyrite ^
Other
Leak
checked* ^o>o
Spare Q
. reagents ,/
Acceptable
Yes
/
/
/
y
s
s
s
^
v~
No
Quantity
required
2
2
2
2
6
2
2
1
Ready
Yes
/
/
u/
v/
/
I/
^
^
s
No
Loaded
and packed
Yes
/
/
S
S
S
^
i/
i/
No
'
*Most significant items/parameters to be checked.
Figure 3.1 Pretest preparation.
-------
Section No. 3.2.3
Revision No. 0
Date January 15, 1980
Page 3 of 6
3. Disassemble, clean, and reassemble the needle valve and
rate meter at any sign of foreign matter in the rotameter or
erratic behavior of the rotameter.
4. Leak check the flexible bag by pressurizing and by
observing for any loss in pressure as described in Section 3.2.1.
3.1.3 Orsat Gas Analyzer - The Orsat apparatus should be checked
and serviced before each field test in the following manner:
1. Check the confining fluid levels in the leveling bottle
and the burette. Be sure the approximately 300 ml of fluid in
the leveling bottle is clear, orange, and sufficient to fill the
burette. Be sure the solution in the leveling bottle is distil-
led water containing approximately 5% by volume of concentrated
sulfuric acid and 2 to 3 ml of methyl orange acidic indicator;
then saturate the solution with a salt, usually sodium sulfite or
sodium chloride, at the temperature at which the Orsat is
expected to operate. (The sulfuric acid acts as a drying agent
to remove any moisture from the sample, and the saturated salt
solution prevents the absorption of sample gases by the leveling
solution.) This leveling bottle solution should be prepared as a
stock solution and taken to the field in case it is needed.
2. Remove and clean the stopcocks. Carefully apply stop-
cock grease to prevent system leaks, and do it without plugging
the air passages. Stopcocks are generally not interchangeable,
so replace each one in the same port from which it was originally
taken.
3. Change the absorbing solutions if >10 passes are needed
to obtain a constant reading for any gas component. If in doubt,
change the solution (following the manufacturer's instructions)
by emptying the absorber and adding fresh absorbing reagents.
Add new reagents when required, 6 to 8 h prior to field use.
Prior to adding the 0~ reagent, flush the absorbing pipette and
the expansion bag with N~, and pass N~ over the reagent while
adding it to the pipette.
-------
Section No. 3.2.3
Revision No. 0
Date January 15, 1980
Page 4 of 6
4. Leak check the Orsat analyzer thoroughly on site before
using it, since moving an Orsat to the site may have caused it to
leak. (Use the procedure in Section 3.2.1) If there are leaks,
check all connections and stopcocks until the cause of the leak
is identified. Leaking stopcocks must be disassembled, cleaned,
and regreased; leaking rubber connections must be replaced.
After the analyzer is reassembled, the leak-check procedure must
be repeated.
3.1.4 Fyrite Gas Analyzer - Check the absorption analyzer
visually for leaking of reagents prior to each test.
3.2 Equipment Packaging
Logistics of the method, time of sampling, and quality of
data are dependent on the packing of the sampling and analytical
equipment for (1) accessibility in the field, (2) ease of move-
ment on site, and (3) optimum functioning in the field. Equip-
ment should be packed to withstand severe treatment during ship-
ment and field operations.
1. Pack probes, pumps, and condenser in cases or wooden
boxes filled with packing material or lined with styrofoam. The
cases should have handles or hooks that can withstand hoisting
and should be rigid enough to prevent bending or twisting during
shipping and handling.
2. Pack rate meters, needle valves, and all small glass-
ware individually in shipping containers.
3. Use the rigid container with the integrated sampling
bag for its shipping container.
4. Disassemble the Orsat and pack each item individually
in suitable packing material and rigid containers for long trips
or for shipping as freight. Ship the spare parts and the absorb-
ent solutions in separate containers.
-------
Section No. 3.2.3
Revision No. 0
Date January 15, 1980
Page 5 of 6
Table 3.1 ACTIVITY MATRIX FOR PRESAMPLING OPERATIONS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Grab Sample
Train
No visual sign of
breakage
Visual observation
before each field
test
Replace as
necessary
Probe
As above
As above
As above
Pump
As above
As above
As above
Integrated Gas
Sampling Train
Probe
As above
As above
As above
Air-cooled con-
denser
As above
As above
Clean and re-
place as
necessary
Needle valve
and rotam-
eter
No foreign matter or
erratic behavior
As above
Clean and reas-
semble as
necessary
Flexible bag
No visual indication of
leakage
As above
Replace as
necessary
Pump
According to manufac-
turer's criteria
Before each field
test, use manufac-
turer's directions
Service or re-
turn to sup-
plier as
necessary
Gas Analyzer
Orsat
Leveling solu-
tion
Distilled water con-
taining approximately
5% by volume of concen-
trated H?SO, and satu-
rated with a salt
Prepare fresh
solution
Absorbing solu-
tion
<10 passes needed for
constant readings with
any component gas
Performance check
using any component
gas
Use fresh
reagent
(continued)
-------
Section No. 3.2.3
Revision No. 0
Date January 15, 1980
Page 6 of 6
Table 3.1 (continued)
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Stopcocks
No leakage
Visual observation
Remove, clean,
regrease as
necessary
Assembly
No leaks present
See text
Eliminate leaks
before test
Gas Analyzer
(Fyrite)
Fill with reagents;
no leaks
Visual observation
Add fresh
reagent; re-
pair as neces-
sary
Package Equip-
ment for Ship-
ment
Not applicable
See packing instruc-
tions
Not applicable
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 1 of 12
4.0 ON-SITE MEASUREMENTS
The choice of procedure to be used at the sampling site
depends on whether an emission rate factor (F-factor), an excess
air determination, or a molecular weight determination is re-
quired. The applicable measurement is specified in the emission
standard, and the quality assurance activities are summarized in
Table 4.1 in this section. In any case, the equipment is un-
packed at the sampling site and visually inspected for damage
during shipment from the laboratory; the Orsat analyzer, espe-
cially, is carefully checked for reagent levels and leaks as
described in Section 3.2.1. Figure 4.1 (On-site Measurement
Checklist) can be used as a guide for sampling and analysis of
molecular weight, excess air, and emission rate determination.
4.1 Determination of CCs and 02 for Dry Molecular Weight
Calculations
Three methods are described in the Federal Register for
measuring a gas stream's dry molecular weight. These are dis-
cussed in order of increasing complexity, and their uses are de-
termined by the applicable standards or by expected variations in
gas composition.
4.1.1 Single-Point Grab Sampling and Analysis - Set up the grab
sampling train as depicted in Figure 1.1. Visually check each
connection for leaks.
1. Be sure the sampling point in the duct is either at the
centroid of the cross section or at a point >^1 m (3.28 ft) from
the walls of larger ducts, unless otherwise specified by the
administrator.
2. Place the probe securely in the stack at the sampling
point.
3. Seal the sampling port as well as possible with a
sponge or rag to prevent dilution of the stack gas by ambient air
if the stack pressure is negative.
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 2 of 12
Sampling
Method: single-point grab /^ single-point integrated
multipoint integrated
Is a filter used to remove particulate matter?
*Sampling train leak checked?
*0rsat analyzer leak checked?
All connections tight and leak free?
Sampling port properly sealed?
Sampling rate held constant?
Sampling train purged?
Analysis
Molecular Weight Determination
Analyzer: Orsat yX Fyrite Other
Fyrite:
Reagent at proper level and zeroed?*
Leak-free connection between analyzer and sample line?
Sampling line purged?*
Orsat:
Reagents at proper level?* ^ yj^v-o
Analyzer level?
Leak checked?* __^__^
Sample analyzed within 8 h?*
Sample lines purged?*
Excess Air-Emission Rate Correction tO/ f^-
Orsat analyzer leak checked?* Before After
Reagents at proper level?*
Sampling lines purged?*
Analysis repeated by drawing a new sample until the following
criteria are met?
CO- - any three analyses differ by
a) £0.3% when CO- >_4."0/
b) <0.2% when CO^ <4.
%
%
09 - any three analyses differ by
^ a) £0.3% when 07 <15.0%
b) £0.2% when 0^ >15.0%
CO - any three analyses differ by £0.3%
All readings averaged and reported to nearest 0.1%
*Most significant items/parameters to be checked.
Figure 4.1 On-site measurement checklist.
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 3 of 12
4. Check the Orsat analyzer for leaks as described in
Section 3.2.1. (Though this step is not mandatory, it is highly
recommended.) If another gas absorption device is used, it must
be zeroed before use.
5. Purge the sampling line several times by squeezing the
one-way squeeze bulb and then attaching the gas analyzer (either
the Orsat or another gas absorption device).
6. Draw a gas sample into the analyzer and immediately
analyze it for CO- and 02. Record the data on data form shown in
Figure 4.2 or on a similar form.
7. Calculate the molecular weights as described in Sec-
tion 3.2.6.
8. Repeat steps 5 through 7 until the calculated molecular
weights of any three samples differ from their mean by
£0.3 g/mole.
4.1.2 Single-Point Integrated Sampling and Analysis - Set up the
sampling train as shown in Figure 1.2. Visually check for leaks.
1. Be sure the sampling point in the duct is either at the
centroid of the cross section or at a point >_1 m (3.28 ft) from
the walls of larger ducts, unless otherwise specified by the
administrator.
2. Place the probe securely in the stack at the sampling
point.
3. Seal the sampling port as well as possible with a
sponge or rag to prevent dilution of the stack gas by ambient air
if the stack pressure is negative.
4. Leak check the flexible bags as described in Section
3.2.1, and then evacuate the selected bag. Leak check the
sampling system by attaching a vacuum gauge to the condenser
inlet, drawing a vacuum of 250 mm (10 in.) Hg, and plugging the
outlet fitting where the bag is usually attached. Turn off the
pump and observe the vacuum reading for 30 s; it should remain
stable. If the vacuum drops, check the system for leaks, then
repair if necessary, and finally recheck. (These leak checks are
optional, but highly recommended.)
-------
PLANT.
DATE_
8-/- 7?
COMMENTS:
SAMPLING TIME (24-hr CLOCK).
SAMPLING LOCATION
_TEST N0_
/33S~-/^5V
SAMPLE TYPE (BAG, INTEGRATED, CONTINUOUS).
ANALYTICAL METHOD $J
^.S
MULTIPLIER
44/100
32/100
^/lOO
^/lOO
MOLECULAR WEIGHT OF
STACK GAS (DRY BASIS)
%
j.6'1'
J. 5~^
O
li. (,i~
TOTAL -** ^•-i
n^ \j Juj tO
Oj f^ fft ft\
vQ ft < O
0) (D H- rt
03 H-
H-O
O S § 3
Figure 4.2 Gas analysis data form.
CJ
M O •
en to
IO
00
O
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 5 of 12
5. Connect the probe, open the quick disconnect at the bag
connection, and purge the sampling system with stack gas by
running the pump for about 1 min at a high rate. Make sure that
the condenser drain valve is closed tightly.
6. Connect the evacuated flexible bag, and begin the
sampling. Record the time, flow rate, and other appropriate data
on a form like the one shown in Figure 4.3.
7. Sample at a constant rate so that about 30 to 90 I (1
q
to 3 ft ) of gas are collected simultaneously with the pollutant
emission rate test.
8. Disconnect, seal, and remove the flexible sampling bag
to a suitable area for performing the analysis. Allow the col-
lected sample to sit for about 30 min to ensure thorough mixing
and temperature equilibrium. It is recommended that the analysis
be performed as soon as practical after the 30-min waiting
period, but not more than 8 h after sampling. If an Orsat
analyzer is used, leak check it as described in Section 3.2.1.
(Though not mandatory, this step is highly recommended.) If a
gas absorption device is used, zero it before use.
9. Calculate the molecular weights as described in Sec-
tion 3.2.6. A data form similar to the one shown in Figure 4.2
can be used for recording the results of the calculations.
10. Repeat steps 8 and 9 until the calculated molecular
weights of any three analyses differ from their mean by
^0.3 g/mole.
4.1.3 Multipoint Integrated Sampling and Analysis - This proce-
dure is similar to the single-point integrated sampling proce-
dure, but it is used when the stack cross section is traversed.
1. Locate the sampling points according to the procedures
described in Method 1. Determine the minimum number of traverse
points, as follows:
a. 8 points for a round stack with <0.61 m (24 in.)
diameter,
b. 9 points for a rectangular stack with an equiva-
lent diameter of <0.61 m (24 in.), or
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 6 of 12
Date
Sampling location
9
Run number Q- /
Plant j)nV
P
Barometric pressure
Ambient temp. °C
Operator
- Cf.
Stack temp. °C
% Dev. =
Q - Q
Time
A3: 00
/ 'S-t>jr
/ ?> /D
y S.'/.'T
;^'2O
/ 3 -^
;3: v5"
/3 i.'Sft
/J-^-5"
/^ rtfi
yv-^-r
; yv o
Traverse
point
,^- /
D
3
s/
.•^T
6
K;- )
i
^
V
5"
^>
Rate meter flow
rate (Q),
cm3/min
500
.5750
.f/5D
.*J/0(0
O^C1
,^D
•^OO
.^-5/?O
5""°^
.«r/or>
v5Z>n
v-50O
Avg = .5i)n
% Dev.a
n
n>
n)
0
0
o>
0
d>
r)
c?
o
o
(^
Q
100; must be £10%.
avg
Figure 4.3 Integrated bag sampling field data.
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 7 of 12
c. 12 points for a larger stack.
2. Leak check and purge the bag and the sampling train as
described in Subsection 4.1.2.
3. Sample each point at the same rate and for the same
time increment. Record the sampling data as shown in Figure 4.3.
Collect from 30 to 90 S, (1 to 3 ft ) of gas simultaneously with
the pollutant emission rate test.
4. Disconnect, seal, and remove the bag to a suitable area
for performing the analysis within 8 h, as described in Subsec-
tion 4.1.2.
5. Calculate the molecular weight, and repeat the analysis
until the results from any three analyses differ from their mean
by <_0.3 g/mole.
4.2 Determination of Gas Composition for Emission Rate
Factor or Excess Air Calculations
The same three sampling procedures may be used as previously
described (Subsections 4.1.1, 4.1.2, and 4.1.3), but in all cases
the Orsat analyzer must be used for analysis, and it must be leak
checked before and after analysis. In addition, the integrated
sampling train (when used) and the flexible bags must be leak
checked prior to sampling. Care in using the Orsat and in assur-
ing the accuracy of the results is also required, as described in
this section.
4.2.1 Single-Point Grab Sampling and Analysis - Set up, check,
and purge the system as described in Subsection 4.1.1. Perform
the Orsat analysis immediately according to the manufacturer's
instructions and as follows:
1. Draw sample gas into the Orsat and flush (i.e., allow
to bubble through the burette) at least three times to saturate
the liquid in the burette with the gas being analyzed and to
ensure that the air remaining in the manifold is of the same
composition as the sample to be analyzed. Caution; Once the
flushing has begun, ambient air must not be allowed to enter the
manifold.
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 8 of 12
2. Draw in a fixed volume (usually 100 ml) of the sample
gas, following the manufacturer's instructions. Allow a minimum
of 5 min for the sample gas to come to temperature equilibrium
with the water jacket around the burette (unless the sample and
the analyzer have both been at the same temperature for at least
5 min).
3. Proceed with the sequential determinations of CO*, Cu,
and CO as directed by the instructions supplied by the manufac-
turer of the gas analyzer. Make repeated analyses of each compo-
nent until two consecutive readings are identical. Always make
two or three passes through the absorbing solution between read-
ings. Note: If more than three readings of two or three passes
are required to reach a constant reading for any component gas,
replace the absorbing reagent and repeat the entire sampling
sequence.
4. Record the readings on the data form (Figure 4.1), and
determine the average value for each component of interest.
5. Leak check the Orsat after analysis. If it does not
pass the leak test, repair it and repeat the analysis.
4.2.2 Integrated Single-Point and Multipoint Sampling and
Analysis - The sampling procedures are identical to those de-
scribed in Subsections 4.1.2 and 4.1.3. The flexible bag and the
sampling train must be checked for leaks prior to sampling, and
the Orsat must be leak checked before and after analysis.
After taking the sample, remove the flexible bag to the
analysis area and let it remain there for at least 30 min before
analyzing with the Orsat. Analysis must be completed within 4 h
of sampling. Perform the analysis according to the manufac-
turer's instructions and as outlined in Subsection 4.2.1. Repeat
the analyses by drawing in new samples of C02/ O2/ or CO from the
bag until the following criteria are met:
For CO,, - Repeat until any three analyses differ by
£0.3% (absolute) when C02 is >4.0%, or by £0.2% (absolute) when
CO? is £4.0%. Average the three acceptable readings, and report
to the nearest 0.1%.
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 9 of 12
For 02 - Repeat until any three analyses differ by £0.3%
when the 02 is <15.0%, or by £0.2% when the C>2 is >15.0%.
Average the three acceptable readings and repeat to the nearest
0.1%.
For CO, if required - Repeat until any three results differ
by £0.3%.
4.3 Special Precautions
The Orsat analyzer is a simple instrument, but the validity
of results depends on operator technique, care, and patience.
Special precautions for using an Orsat analyzer include:
1. Do not allow ambient air to enter the Orsat analyzer
during testing.
2. Always perform the analysis in the following sequence:
absorber No. 1 - CO2, absorber No. 2 - O2, and absorber No. 3 -
CO. This sequence is necessary because absorber No. 2 will also
absorb CO2, and absorber No. 3 will absorb O2 and possibly C02 ;
double absorption will yield erroneous data.
3. Be sure to saturate the indicating solution in the
burette with salt at the operating temperature to prevent absorp-
tion of sample gases prior to analysis. Be sure the solution is
acidic (as indicated by methyl orange) to enable it to absorb any
moisture in the sample gas.
4. Keep the absorber solution from entering the capillary
column manifold. Void the test if any absorber solution enters
the manifold, and clean the sample manifold with acetone.
5. Allow a minimum of 5 min for gas samples to come to
temperature equilibrium with the water jacket before the
analysis.
6. Operate the Orsat analyzer under constant temperature
and pressure. Be sure that the levels of solutions in the
burette and the leveling bottle are the same to ensure equal
pressures before taking a reading from the Orsat. The water
jacket acts as a buffer for temperature changes.
7. Measure SO2 concentrations quantitatively (Method 6) if
the source being tested is known to have or is suspected of
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 10 of 12
having high S02 concentrations, and subtract the value from that
of the C02 determination. Measure and correct the values when
the SO2 concentration is suspected to be >_3% (relative) of the
C02 concentration and when the data are to be used to correct
emission rates or to calculate gas flows. If the data are to be
used for calculating just the molecular weight (M,), then S02 in-
terferences as high as 0.5% (absolute) or 5000 ppm are accept-
able; this level of interference will result in an error of only
about 0.1 g/g-mole (0.1 Ib/lb-mole) in M-
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 11 of 12
Table 4.1 ACTIVITY MATRIX FOR ON-SITE MEASUREMENTS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Grab Sampling
Sampling train
No leaks
Visually check before
each field test
Eliminate
leaks before
proceeding with
test
Sampling points
At the centroid of the
cross section or at a
point >1 m (3.28 ft)
from the walls
Not applicable
Not applicable
Integrated
Sampling
Locate sampling
points
8-12 points; see Sub-
sec 4.1.3
Not applicable
Not applicable
Flexible bag
No leaks
Check before each
field test; see
Sec 3.2.1
Replace as
necessary
Train
No leaks; vacuum
stable for >30 s
Pull vacuum of at
least 250 mm
(10 in.) Hg
Check all
connections,
replace items
as necessary
Sampling rate
Constant rate
Check using Fig 4.2
Repeat sampling
to meet 10%
deviation limit
Orsat Analyzer
Leak check
No leaks for 4 min
Varies with test
method; mandatory
for emission rate
factor and excess
air calculations;
Sec 3.2.1
Check rubber
connections and
stopcocks
until cause
of leak is
identified; leak
check after re-
pair and
reassembly
(continued)
-------
Section No. 3.2.4
Revision No. 0
Date January 15, 1980
Page 12 of 12
Table 4.1 (continued)
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Test Results
For M
M, from each of three
grab samples and anal-
yses differ from their
mean by <0.3 g/g mole
(0.3 Ib/Ib mole)
For each field test,
compare calculated
M
Repeat analysis,
perhaps by
another operator
For emission
rate factor
or excess
air calcu-
tions
1. Make repeated passes
thru the absorbing solu-
tion until two consecu-
tive readings are the
same; compare three
readings
2. Make repeated ana-
lyses; see Subsec 4.2.2
for criteria
Compare readings
1. Replace ab-
sorbing solution
2. Compare analyses
of component gases
2. Repeat analy-
ses by another
operator; check
the apparatus
and technique
-------
Section No. 3.2.5
Revision No. 0
Date January 15, 1980
Page 1 of 2
5.0 POSTSAMPLING OPERATIONS
Table 5.1 at the end of this section summarizes the quality
assurance activities for the postsampling operations.
5.1 Compare Measured Values Against Theoretical Values
After the analyses have been performed and before the appa-
ratus is disassembled, the measured and the theoretical results
(if available) should be compared as a quick check for gross
measurement errors.
Combustion nomographs are available for estimating the per-
centages by volumes of C09 and 09 when the fuel composition is
89
known. ' Also the nomograph can be used to calculate the mole-
cular weight of the stack gas.
Perform the calculations on the measured data as directed in
Section 3.2.6 and perform the following comparison:
n = °/rn - °/m
DC02 /oC02(m) /oL02(e)
where
DCQ = difference in measured and estimated values, %,
%CO2, . = measured C02 (average of r replicates), %, and
%c°2(e) = estimated or theoretical C02, %.
Accept the measured value if Drn is <2% (absolute); otherwise,
VxC/Q
check the apparatus, the technique, and the estimating procedures
before collecting and analyzing more samples.
Record the estimated or theoretical values on a form similar
to Figure 4.1. (Theoretical values may have been calculated and
recorded before the field test if sufficient knowledge of the
process was available.)
A second method to help eliminate gross errors is the use of
the Fyrite sampler at several points during the test. This will
indicate whether a problem does exist, but will not reveal which
value is indeed correct.
-------
Section No. 3.2.5
Revision No. 0
Date January 15, 1980
Page 2 of 2
5.2 Disassemble and Inspect Apparatus
When disassembling the apparatus, visually inspect the
sampling train components and the Orsat analyzer for damages that
could have adversely affected the measured values. Any identi-
fied damage that was not detected during the test should be
documented on the field data form and thoroughly evaluated by the
appropriate apparatus check in the laboratory. After checking if
it is concluded that the damage could have biased the measure-
ments, a description of potential bias in the data should be
included in the field test report. If possible, repeat the field
test.
5.3 Pack Apparatus for Shipment to Laboratory
Pack the apparatus for shipment to the laboratory as de-
scribed in Section 3.2.3. Return the data forms, prepared in
duplicate, to the laboratory--one copy should be sent by mail,
and one copy handcarried.
Table 5.1 ACTIVITY MATRIX FOR POSTSAMPLING OPERATIONS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Compare mea-
sured vs.
estimated
values of
%co2(m) - %co2(e)
<2% (absolute) sug
gested
As suggested by ad-
ministrator; e.g.,
for each incinerator
test when an estimate
of %C02 is to be
used to correct parti-
culate emission levels
Repeat the
analysis for
additional
samples
Disassemble and
inspect ap-
paratus
No damage that could
have adversely affected
the measurement
Visual inspection
Report damage
and its pos-
sible bias on
measurements to
the administra-
tor; use Fig 4.1
Pack apparatus
for shipment
Follow specified pack-
ing instructions
After each field test
Not applicable
-------
Section No. 3.2.6
Revision No. 0
Date January 15, 1980
Page 1 of 3
6.0 CALCULATIONS
Table 6.1 at the end of this section summarizes the quality
assurance checks pertaining to calculations.
6.1 Excess Air
Use Equation 6-1 to calculate the percentage of excess air.
Use the average value for each of the component gases, as fol-
lows :
where
%EA =
%00 - 0.5 %CO
0.264 %N2 (%02 - 0.5 %CO)
100
Equation 6-1
%EA = percent excess air, %,
%09 = percent 09 by volume (dry basis)
£* £*
02 values, %,
%CO = percent CO by volume (dry basis)
CO values, %,
%N2 = percent N2 by volume (dry basis)
average of three
average of three
average of three
N2 values, %, and
0.264 = ratio of 02 to N2 in air, v/v.
The average value for each of the gases is computed from the
Orsat analyses satisfying the criteria in Section 3.2.4. Round
each average to the nearest 0.1%. In many cases, %CO will be
close to zero and can be dropped to simplify Equation 6-1. Equa-
tion 6-1 is applicable whenever most of the N~ in the flue gas
comes from N~ in the combustion air, as is the case with most
fuel and refuse combustion processes. If the fuel contains
appreciable amounts of N2 or if 02 enrichment is used, Equation
6-1 cannot be used; alternate methods, subject to the approval by
the administrator, are required.
-------
Section No. 3.2.6
Revision No. 0
Date January 15, 1980
Page 2 of 3
6.2 Dry Molecular Weight
Use Equation 6-2 to calculate the dry molecular weight from
data in Figure 4.1--i.e., the average values of the component
gases reported to the nearest 0.1%.
M, = 0.44 (%C09) +0.32 (%09) +0.28 (%N9 + %CO) Equation 6-2
'-I £*£*£*
where
Mo = dry molecular weight, g/g-mole (Ib/lb-mole),
%C02 = percent CO, by volume (dry basis), average of three
analyses, and
%02, %N2, and %CO are previously defined.
Round M, to the nearest 0.1, and record the value Figure 4.1.
6.3 Data Reporting
A copy of Figure 4.1 or an equivalent form should be filed
in the laboratory log, and the original should be forwarded
either to the home laboratory for further internal review or to
the user. An independent check of the calculations should be
performed, and the corrected values should be indicated on the
form if the differences are more than the acceptable roundoff
error. The checking analyst should initial the data form.
-------
Section No. 3.2.6
Revision No. 0
Date January 15, 1980
Page 3 of 3
Table 6.1 ACTIVITY MATRIX FOR CALCULATIONS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Calculations
1. Data form Fig 4.1
contains all data
required for calcula-
tions of %EA, M,, and
emission rate factor
2. Average concentra-
tions calculated to the
nearest 0.1%; final
calculations rounded
to nearest 0.1%
3. Independent calcu-
lation agrees to the
nearest 0.1%
1. Visual observa-
tion at each field
test
2. For each field
test, compute the
average concentration
of three analyses
that meet test re-
quirements
3. For each field
test, repeat calcu-
lations starting
with raw data
4. Visual check
1. Obtain neces-
sary data to com-
plete the form
2. Recalculate
all results for
which computa-
tions not con-
sistent with pro-
cedure
3. Report cor-
rected values of
the calculations
in Fig 4.1
4. Correct
calculations
Data reporting
Data report complete
with indication of
calculation check
Visual observation
of each field test
Perform
necessary cal-
culation checks
-------
Section No. 3.2.7
Revision No. 0
Date January 15, 1980
Page 1 of 1
7.0 MAINTENANCE
Little periodic maintenance is required for the Orsat
apparatus—other than visual checks of the glassware, tubes, and
expansion bulbs. Keep the valves closed during storage, and
avoid freezing temperatures. If the Orsat is to be stored over
an extended period, it is generally better to remove all of the
absorbing reagents. The flexible bags are generally subjected to
extensive wear, and require repair or replacement when leaks
occur. The pump and rotameter should be kept clean and should be
maintained in accordance with manufacturers' instructions.
Table 7.1 ACTIVITY MATRIX FOR MAINTENANCE
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Glassware, con
necting tub-
ing, expan-
sion bulbs
No damage
Visually check before
each use
Replace if
damaged
bags
AC;
As above
Repair or re-
place as re-
quired
Pump and
rotameter
Clean and maintained
in accordance with
manufacturer's in-
structions
According to manu-
facturer's instruc-
tions
Adjust/repair
or request
assistance of
supplier
-------
Section No. 3.2.8
Revision No. 0
Date January 15, 1980
Page 1 of 5
8.0 AUDITING PROCEDURE
An audit is an independent assessment of data quality. It
is independent because it is conducted by personnel other than
the field crew and by using apparatus and measurement standards
that are different from those used by the regular field crew. In
the field, routine quality assurance checks are necessary for
obtaining good quality data from a series of test runs at one
source, but they are not part of the auditing procedure.
Table 8.1 at the end of this section summarizes the quality
assurance activities for auditing. Based on the results of col-
laborative tests, three performance audits and a systems audit
are recommended in Subsections 8.1 and 8.2. Both types are to
be conducted by auditors.
8 .1 Performance Audits
Performance audits are quantitative evaluations of the
quality of the data produced and recorded by the total measure-
ment system (sample collection, sample analysis, and data proces-
sing). These audits should be conducted by the responsible con-
trol agency once during every enforcement source test, regardless
of whether the test is conducted by a control agency or by a
private company personnel. A source test for enforcement com-
prises a series of runs at one source.
8.1.1 Audit of M, - Because the maximum relative error in M-, is
d d
approximately 4%, it is not practical to audit M, unless directed
by the administrator.
8.1.2 Audit of Analytical Phase Using Certified Gas Mixtures for
Emission Rate Correction Factor and Excess Air Determination
Analyzer operation and operator technique can be checked by pro-
viding audit samples of certified gas mixtures to be analyzed
prior to or along with field samples. One sample should contain
concentrations of 2-4% 02 and 14-18% C02, and another sample
should contain concentrations of 2-4% C02 and about 15% 02.
-------
Section No. 3.2.8
Revision No. 0
Date January 15, 1980
Page 2 of 5
These gas samples can be transferred from their pressurized
storage containers to flexible bags and delivered to the test
team on site by the auditor. Replicate samples of the audit gas
containing 0_ and CC- concentrations similiar to the concentra-
tions expected during the test and one sample of the other audit
gas should be sufficient for audit of the analytical phase.
The error of the analytical phase can be calculated using
Equation 8-1, and should be £1.0% for CO- and O .
D = %V - %V Equation 8-1
ci O
where
D = difference in the field test results and the certi-
fied audit value, %,
%V = field team's value as the average of r replicates,
%, and
%V = certified value of audit gas, %.
v*
The emission rate correction factor is not directly proportional
to the Orsat analyzer error. Therefore, the standard calculation
of %D is not applicable. The results of the calculated %D should
be included in the enforcement source test report as an assess-
ment of accuracy of the analytical phase of Method 3 during the
actual enforcement source test.
8.1.3 Audit of Data Processing - Data processing errors c?n be
detected by auditing the data recorded on the field and the
laboratory forms. The original and the field check calculations
should agree; if not, all of the remaining data should be re-
checked by the auditor, and any errors should be clearly
explained to the team to prevent or minimize reoccurrence. The
data processing errors may also be detected in copies of data
sets compiled and filed in the field and in copies of manual data
reductions (or computer printouts, if used) forwarded to the
evaluator for audit. Calculation errors are prevalent among
users of Method 3.
-------
Section No. 3.2.8
Revision No. 0
Date January 15, 1980
Page 3 of 5
8.2 Systems Audit
A systems audit is an on-site qualitative inspection and
review of the quality assurance checks used by the team for the
total measurement system (sample collection, sample analysis,
data processing, etc.). Initially, a systems audit specified by
a quality assurance coordinator should be conducted for each
enforcement source test, which by definition comprises three
runs at one source. After the team gains experience with the
procedure, the frequency of audit may be reduced, for example, to
once for every four tests. The auditor should have extensive
experience in source sampling—more specifically, with the
characterization technique being audited.
The functions of the auditor are summarized as follows:
1. Observe procedures and techniques of the field team
during sample collection.
2. Check/verify the records of apparatus calibration and
the quality control charts used in the laboratory analysis.
3. Record the results of the audit and forward them with
comments on source team management to the quality assurance
coordinator so that any needed corrective actions may be imple-
mented.
8.2.1 Collecting On-Site Information - While on-site, the
auditor should observe the field team's overall performance of
the source test. Specific operations to observe should include,
but not be limited to:
1. Setting up and leak testing the sampling train.
2. Purging the sampling train with stack gas prior to
collecting the sample.
3. Proportional sampling.
4. Transferring of the sample from the collapsible bag to
the Orsat analyzer.
Table 8.1 is a suggested form for use by the auditor.
8.2.2 Collecting Laboratory Information - When visiting the
field team's home laboratory, the auditor should check the re-
cords to verify that the performance criteria in Table 4.3 (Sec-
tion 3.2.4) have been met since the last audit was performed.
-------
Section No. 3.2.8
Revision No. 0
Date January 15, 1980
Page 4 of 5
Yes
No
OPERATION
Presampling Operation
1. Availability of theoretical value
2. Use of modified Orsat analyzer (0.1-ml
divisions)
On-Site Measurements
3. Setting up and leak testing the samp-
ling train
4. Purging the sampling train with stack
gas prior to collecting the sample
5. Constant rate sampling
6. Transfer of sample from collapsible
bag to the Orsat analyzer
7. Maintaining constant pressure throughout
the test
8. Exposing the sample to ambient air
9. Spent absorbing reagent
Postsampling Measurements
10. Perform independent calculations using
data from audit
11. Compare the audit value with the field
team's test value
12. Make sufficient passes for complete
absorption of a component gas
13. Minimize volumetric reading error
14. Check/verify applicable records of
apparatus calibration checks and quality
control charts in the field team's home
laboratory
General Comments
Figure 8.1 Checklist for Method 3 for use by the auditor.
-------
Section No. 3.2.8
Revision No. 0
Date January 15, 1980
Page 5 of 5
Table 8.1 ACTIVITY MATRIX FOR AUDITING PROCEDURES
Audit
Analytical
audit
Data processing
audit
Systems audit
Acceptance limits
D - %Va - %Vc
%V = mean value of
measurements
by field team
%V - certified value
of audit gas
Agreement of original
and check calculations
Technique described in
this section
Frequency and method
of measurement
As designated by the
administrator
Once during each
enforcement source
test; independent
calculations starting
with raw data
Once during each
enforcement test
until experience
gained, then every
fourth test; observe
techniques; use audit
checklist Fig 8.1
Action if
requirements
are not met
Advise team of
sources of
errors , and re-
quest they seek
additional train-
ing; rerun test
if necessary for
determination of
compliance
Check and correct
all data
Explain to
team the de-
viations from
recommended
techniques, and
note deviations
on Fig 8.1
-------
Section No. 3.2.9
Revision No. 0
Date January 15, 1980
Page 1 of 1
9.0 RECOMMENDED STANDARDS FOR ESTABLISHING TRACEABILITY
To acquire data of good quality, two considerations are
essential: (1) the measurement process must be in a state of
statistical control at the time of the measurement, and (2) the
systematic errors combined with the random variations (errors of
measurement) must result in an acceptable level of uncertainty.
As evidence of good quality, it is necessary to perform quality
control checks and independent audits of the measurement process,
to use materials and measurement procedures which can be traced
to an appropriate reference standard, and to document data from
the checks and audits (e.g., by means of a quality control
chart).
Data must be routinely obtained by repeat measurements of
standard reference samples, primary, secondary, and/or working
standards. The working calibration standards should be traceable
to either primary or higher order standards.
In the case of absorption type gas analyzers, operator
techniques and analyzer operations can be checked by sampling two
certified mixtures of bottled gas containing 2-4% 02 and 14-18%
C02/ or 2-4% C02 and about 15% 02. Bottled gases used for audit
purposes should be traceable to NBS standards.
-------
Section No. 3.2.10
Revision No. 0
Date January 15, 1980
Page 1 of 3
10.0 REFERENCE METHOD
METHOD 3— QAS ANALTSIS FOR CARBON DIOXIDE,
OXYGEN, EXCESS AIR, AND DRY MOLECULAR WIIOHT
1. Principle and Applicability
1.1 Principle. A gas sample is extracted from a stack,
by one of Hi.-- following munods. (1) single-point, grab
sampling; (2j single-point, in''if>ralcd sampling; or (3)
multi-point, intcj-nited sampling. The gas sample is
analyzed fur percent carbon dioxide (062), percent oxy-
gen (O?). and, if necessary, percent carbon monoxide
(CO). If a ry molecular wei:;ht determination is to be
made, either an Orsat or a FyiHe ' analyzer may be used
for the analysis, for excess air or emission rate correction
factor deU" mination, an Orsat analyzer must bo used.
1.2 App u'L.bility. This mi thod is applicable for de-
termining Ul>2 and O, coi.ccn-ralions, excess air, and
dry molecular weight oi a simple from a gas stream of a
fossil-fuel combustion procc.vs. The method may also be
applicable, U> other processes nhereit has been determined
that compt^rai^ other tnan C't-j. Oi, CO, and nitrogen
(Ni) are n>;t present in concentrations sufficient to
affect I he results,.
Other methods, as well as modificolions to the proce-
dure doscnhi'u herein, are al.sc, applicable for some or all
of thoubovi -1 aerminatioith. K\umples of specific meth-
ods and mo- n ,\\\ !0i,s include' (1) a niuiti-[)oint samp-
ling method i,-me an Or^at .iimiw.cr to analyze indi-
vidual grab s.nnpli'.- obtained at each point. (2) a method
using C(>2 fir O- ami sluu'lii, n p.- calc u'.alions to deter-
mine dry 1.10 • ul.ii vu tghl ai , \. ess air: (3) assigning a
value of 30.0 iOi dry molecular weight, in lieu of actual
measurements, for processes butning natural gas, coal, or
oil. These methods and modifications mav be used, but
are subject to the approval of the Administrator.
2. Apparatus
As an altenialivo to the sampling appatatus and sys-
tems descti'K 1 herein, other sampling systems (e.g.,
liquid displ:vce(! , nt) m,iy bo used provided such systems
are capable o, obtaining a representative sample and
maintaining a constant sampling rate, and arc otherwise
capable of yielding acceptable results. Use of such
systems is subject to the approval of the Administrator.
2.1 Griib .Sampling (Figure 3 I).
2.1.1 Prooe The probe shoiud be made of stainless
steel or borosilicate glass tubing and should be equipped
with an in-slack or ont-staclt Iil' • to remove paniculate
matter (a pi; „ jf glass .vi, il ii . .usfaclory for this pur-
pose). Any cvin r maten,. uicr i,> 02, COi, CO, and Nt
and resistant u- temperature at sampling conditions may
be used for the probe: ex unple*, of such material are
aluminum, copper, quartz glass iud Tollon.
2.U Pump \ one-way .-...eez" bulb, or e(|Uivalont,
Is used to i.ni..rt tho f*\ sample to the analyzer.
2.2 In'cgraied 8,impLng (Figure 3-2).
2.2.1 I'robe. A probe such as that described in Section
2.1.1 Is suitable.
' Mention of trade names or specific products does not
constitute endorsement by the Environmental Protec-
tion Agency.
2.2.2 Condenser. An air-cooled or water-cooled eon-
denser, or other condenser that will not remove Ot,
("Oi, CO, and Ni, may be used to remove excess molston
which would Interfere with the operation of the pump
and flow meter.
2 2.3 Valve. A needle valve is used to adjust sample
pas flow rate.
2 2.4 Pump. A leak-free, diaphragm-type pump, or
f qulvalent, Is used to transport sample gas to the flexible
baR. Install a small surge tank between the pump and
rate meter to eliminate the pulsation effect of the dia-
phragm pump on the rotameler.
2.2.8 Rate Meter. The rolameter, or equivalent rate
meter, used should be capable of measuring Mow rale
to within ±2 percent of tho selected flow rate. A flow
rate range of 600 to 1000 cm'/min is suggested.
2.2.8 Flexible Bag Any Icak-fiec plaslic (e.g., Tedlar,
JV.ylar, Teflon) or plastic-coated aluminum (e g., alumi-
nized Mylar) bag, or equivalent, having a capacity
consistent with the selected flow rate and time length
r.f the test run, may be used. A capacity m the range of
6.1 to 90 liters is suggested.
To leak-check the bag, connect it to a water manometer
and pressurize the bag to 6 to 10cm HiO (2 to 1 in. HiO).
Allow to stand for 10 minutes. Any displacement in the
water manometer indicates a leak. An alternative leak-
check method is to pressuroo the bag to 6 to 10 cm HtO
(2 to 4 In. HiO) and allow to scand overnight. A deflated
bag Indicates a teak
23.7 Pressure Gauge A water-nllcd U-tube manom-
eter, or equivalent, of about 28 cm (12 in.) is used tor
the flexible bag leak-check.
2.2.8 Vacuum Gauge. A mercury manometer, or
equivalent, of at least 700 mm Ilg (30 in. Hg) i» used for
the sampling train leak-cheek.
2.3 Analysis. For Orsat and Fyritc analyzer main-
tenance and operation procedures, follow the instructions
recommended, by the manufacturer, unless otherwise
specified herein.
2 3.1 Dry Molecular Weight Determination. An Orsat
-.nalyzer or Fyrlte typo combustion gas analyzer may bo
awd.
2.3.2 Emission Rate Correction Factor or Excess Air
Determination An Orsat analyzer must be used. For
low COi (less than 4 0 percent) or high Oj (greater than
15.0 percent) concentrations, the measuring burette of
the Orsat must have at least 0 1 percent subdivisions.
8. Dry Moltcular Weight Determination
Any of the three sampling and analytical procedures
described below may be used for determining the dry
molecular weight.
3.1 Single-Point, Grab Sampling and Analytical
Procedure.
3.1.1 The sampling point in the duct shall either be
at the centroid of the cross section or at a point no closer
to the walls than 1.00 m (3.3 ft), unless otherwise specified
by the Administrator.
3.1.2 Bet up the equipment as shown In Figure J-l,
makinc sura all connections ahead of the anslyier are
tight and leak-free. If an Orsat analyzer Is used, It is
recommended that the analyzer be leaked-chorksd by
following the procedure in Section 5; however, the leak-
cheek It optional.
J.I.3 Place the probe In the stack, with the tip of the
probe positioned at the sampling point; purge the sampl-
ing line. Draw a sample into the analyzer and imme-
diately analyze it for percent COi and percent Oi. Deter-
mine the perci-nlage of the gas that is Ni and CO by
subtracting the sum of the percent COi and percent Oi
from 100 percent. Calculate the dry molecular Welcht ai
Indicated in Section 6.3.
3.1.4 Repeat the sampling, analysis, and calculation
procedures, until the dry molecular weights of any throe
fcrab samples differ from their mean by no more than
0.3 (/(-male (0.3 IbAb-mole). Average these three molec-
ular weights, and report the results to the Dearest
U.I g/g-molf (Ib/lb-mole).
3.2 Sinjlo-Pomt, Integrand Sampling and Analytical
Procedure.
3.2.1 The sampling point in tho duct shall be located
as specified In Section 1.1.1.
8.2.2 Leak-check (optional) tho flexible bag as In
faction 2.2.6. Set up the rqiiipmem as shown in Figure
3-2. Just prior to sampLiipr. leak-check (optional) the
train by placing a vacuum f,auge at the condenser inlet,
pulling a vacuum of at least "••« mm Ilg (10 In. Hg),
plugging the outlet at 11 if ijaick disconnect, _and then
turning off tho pump. The \ aci.um should remain stable
for at least 0.5 minute. Evacuate the flexible bag. Connect
the probe and place it in tin' stack, with the tip of the
probe positioned at the sami .ling point: purge the sampl-
ing line. Next, connect the K'i and make sure that all
connections are tight and l<*aV Hoc.
3.2.3 Sample at a coi.sun. rate. The sampling run
should be simultaneous »im, and for the same total
Irngth of lime as, the pollu .ni e'nisM,,n rale determina-
tion. CoUecliMi of at least .1 > i.ters tl w ft') of sample gas
is reeommondid: howevi , biuallor volumes may be
collected, if desired.
3.2.4 Obtain one integiated flue gas sample during
Tach pollutant emission ial» dclmninalimi. Within 8
hoiirs after the sample is tal '
-------
Section No. 3.2.10
Revision No. 0
Date January 15, 1980
Page 2 of 3
RATE METER
AIR COOLED
CONDENSER
PROBE
V
FILTER
(GLASS WOOL)
PUMP
QUICK DISCONNECT
VALVE
RIGID CONTAINER
Figure 3-2. Integrated gas-sampling train.
TIME
TRAVERSE
PT.
AVERAGE
Q
1pm
54 DEV.»
%DEV.( 5
V
Qavg
(MUST BE < 10%)
Figure 33. Sampling rate data.
-------
Section No. 3.2.10
Revision No. 0
Date January 15, 1980
Page 3 of 3
from KM) percent. Calculate the dry molecular weight ai
Indicated In Section (1.3.
3.2J> Repeat the analysis and calculation procedures
nntil the Individual dry molecular weights for any three
analyses differ from their moan by no more than 0.3
g/g-mole (0 3 Ib/lb-mole). Average these three molecular
weights, and report tho results to the nearest 0.1 g/g-mole
(0.1 Ib/lb-mole).
3 3 Multi-Point, Integrated Sampling and Analytical
Procedure
3.3 1 Unless otherwise specified by the Adminis-
trator, a minimum of i-ight traverse points shall be used
for circular stacks having diameters less then 0.81 m
(24 in ), a minimum of nine shall be used for rectangular
stacks having equivalent diameters less than 0.61 m
(24 in.), and a minimum of twelve traverse points shall
be used for all other cases. The traverse points shall be
located according to Method 1. The use of fewer points
is subject to approval of the Administrator.
3.3.2 Follow the procedures outlined in Sections 3.2.2
through 3.2.5, except for the following: traverse all sam-
pling points and sample at each point for an equal length
of time. Record sampling data as shown in Figure 3-3.
t. Kniition Hate Correction Factor or Exceu Air Dtter-
mination
NOTE.—A Fyritc-lypo combustion gas analyzer is not
acceptable for excess MT or emission rate correction factor
determination, unl.ss approved by the Administrator. ,
If both percent CO.- and percent Oi are measi cd the
analytical results of • ,v of the three procedures given
below may also be ui. J for calculating the dry molecular
weight.
Each of the three j.r -edures beiow shall be used only
when specified in a: ui.nlicablesubpart of the standards.
The use of these procedures for other purposes must have
specific prior approval of the Administrator.
4.1 Single-Point Grub Sampling and Analytical
Procedure.
4.1.1 The samphr ,.imt in the duct sh.il! cither be
at tho crntroid uf l -'-section or at a point no closer
to the, walls than l.i ;.3 ft), unless otherwise specified
by the Administrator
4 1.2 Set up tho equipment as shown in Figure 3-1,
making sure all conneciions ahead of the analyzer are
tight and leak-free. Leak-check the Orsat analyzer ac-
cording to the procedure described In Section 4. This
leak-check is mandatory.
4 1 3 rince the probe In tho stack, v. ith the tip of tiie
prob. positioned at the sampling point, purge the sam-
pling line. Draw a sample into the analyzer. For emission
rate correction factor determination, immediately ana-
lyze the sample, as outlined in Sections 4.1.4 and 4.1 5,
f.V percent COi or percent O;. If excess an' is desired,
pronod as follows' (1) immediately analyze, tho sample,
as in ^ectiuns 4.1.4 and 4.1.5. for percent COi, Oi, and
CO. (2) determine tho percentage of the gas that Is Ni
by subtracting the sum of the peieent CO:, percent Oi,
an' i>ercent CO from 1X> percent, a,id (J) calculate
pel cent evcebS air as outlined in Section G 2.
4.1.4 To ensure ooi..;ilele absorption of the, COi, Oi,
or if applicable, CO, maiwe repeated passes thr ugh each
absorbing solution u I'-il UN o consecutive readings are
l'ii- same. Several pas^-s 'three or four^ should be made
b.tneen readings, (i. cmslant nut. ,f^ "unnot be
oininned after three consecutive raiding-, replace the
ol.-,.>rl'liiR solulion.)
4.1 5 Af'er the anal1 sis Is completed, leak-check
(mandaloi v) tin1 Oisat .walyzer once .1^:11:., fid descubed
n> ^ec1lon o (''or tiie n uit.* of the ant-iyf-is lo be valid,
tin- Orsat analyzer nii.'.t pass this leak tei-t before and
hlUT the anal\si<;. Noli..- Since tins sni[!: '-puint, grab
sampling and an;U5lical procedure i:, notnmiiy conducted
in comtincuon \utli a si igle-point, giab sampling and
analytical pinccduic for a pollutant, only i.ne analysis
is onh'.ianly C",iuiuc1fd. i'li<;re(ure, irrca' o:t;e must bo
takrn to obtain a vali 1 Sample and jnaij.-i- Althougii
in most cases onlv COj or O: is reau red, it is recom-
mended that hotii COt anil O: be in, asurod, And that
Citation 5 in the Bibliography be use,! to validate tho
analytical data.
4.2 Single-Point, InUviaU'd Sainplln? .ilnl Analytical
rrocednio
4 2 1 Tnc sampling poll- m the duel -.1 all be located
as specified m Section 4 1 I
4.2,2 Leak-check (mandatory) tho fleAible Imp as in
Section 2.2.6. Set up the equipment as shown m Figure
3-2 Just prior to sampling, leak-check (mandatory) tho
train by placing a vacuum gauge at the condenser inlet,
pulling a vacuum of at least 250 mm Ilg (10 in. Kg),
plugging the outlet at the quick disconnect, and tboa
turning off the pun i, Tho vacuum shall rcma,- .hie
for at least 0.5 minute. Evacuate the flexible bag. Con-
nect the probe and place it in the stark, with the tip of the
probe positioned at the sampling point; purge the sam-
pling line. Next, connect the bag and make sure that
all connections aro tight and leak froe.
4.2.3 Sample at a constant rate, or as specified by the
Administrator. The sampling run must bo simultaneous
with, and for the same total length of time as, tho pollut-
ant omission rate determination. Collect at least 30
liters (1.00 ft1) of sample gas. Smaller vohimos may be
collected, subject to approval of th a.dnunistrsitor.
4.2.4 Obtain one integrated duo gas sample during
each pollutant emission rate determination. For emission
rate coirection factor determination, analyze the sample
within 4 hours after it is taken for percent COi or percent
Oi (as outlined in Sections 4.2.5 through 42.7). The
Orsiit analyzer must bo leak-checked (soe Section 5)
before the analysis If o\cess air is desired, proceed as
follows. (1) within 4 hours alter the sample is taken,
analyze it (as in Sections 4.2.5 through 4.2.7) for percent
CO), Oj, and CO, (2) determine tho percentage of the
gas that is Nj bv subtracting the sum of the percent COi,
pcrce.nt Oi, and jieicent CO from 100 percent; (3) cal-
culate percent excess air, as outlined in Section 6.2.
4.2.5 To ensure coiipletc absorption of tho COi, Oi,
or if applicable, CO, ma.;e repealed passes through each
absorbing solution until two consecutive readings are the
s.ime. Several passes i throe or four) should bo made be-
tween readings. (If constant readings .-annot be obtained
after three consecutive readings, replace tho absorbing
solution.)
4.2 6 Kepeat the analysis until the following criteria
are met-
4.2.61 For percent CO:, repeat the analytical pro-
cedure until the results if any three analyses dilTer by no
more than (a) 0.3 percent by volume when COi Is greater
than 4.0 percent or (b) 0.2 percent by volume when COi
Is less than or equal to 4.0 percent. Average the three ac-
ceptable values of percent COi and report the results to
the nearest 0.1 percent.
4.2.6.2 For percent Oi, repeat the analytical procedure
until the results of any three analyses differ by no more
than (a) 0.3 percent by volume when Oi Is less than 15.0
percent or (b) 0.2 percent by volume when Oi is greater*
than 15.0 percent. Average the three acceptable 'values of
percent Oj and report tho results to the nearest 0.1
iwrcent.
4.2.8.3 For percent CO, repeat the, analytical proce-
dure until the results of any three analyses differ by no
more than 0.3 percent Avi'iapc the three acceptable
values of poront (JO and i"!'uit 'h,. icsnltslotlie neanat
0.1 percent.
42.7 After t'i, analysis is completed. Kik-ehcck
(mandatory) the Orsal anal.v. ei once .igam, as described
InbectionS. Fortln' restills of the analysis to be valid the
Orsat analyzer must pass tins '"'ik test befoie mid after
the analysis. Note Although in nost instances only COi
or Oi IS rc<|lihc', l is icconnncndca that both ''(Ijand
OibcmoaMird1.,!!. 'I that t iutmn 5 in the Dihhoffiauhy
be used to validate the anal\ heal data.
4.3 Multi-Point, Integral".! Sunphng and Analytical
Procedine.
4.3.1 Both the Minimum number of s.inipl'iiK no'nts
and the sampling point loca'ion ;1m!t he ,is spfi Hied in
Section a.3.1 of this method. The use of fewei points than
specified ;s subject to the nppi -iy.i if the Administrator.
4.3.2 Follow \ •• proeedmes 0111 lined in Sections 42''
tlnough 42.7, eicepl for llie following Tr.ivuse all
sampling points and sample ,-.' each point f'ir . -i e.mal
length of time. liecold sampln • data ns sln.vn "• '• iL'iirn
5. Leak-Check Fi-t.-nlurt for 0-s,'l .•liialn:irs
Moving an Ovsat nralyZT 'iwnicntly e.ui-r-. p o leak
Therefore, an Orsat analy/n should be tliriuupthiv leak-
checked on site bi fore the line gas sample is unreduced
into it. The pnx I'u-vfoi look ;h«'king,in '.vrs .t ": il\, r
is. • '
5.1.1 Biing the liiinid Uvel ni each pnieUe tin ',' 'Me
r.-fcienccnia-lton the capillr.ly tnlmi!; and tl en cl"<. 'ho
pipette Mopi oek.
S 1.2 U.nsetn levelin™ bulb sulbcienllj' to In •« lie
condnniR Injuid inemscns onto ''iy (ii'aduaieti H,I> , ,, ,,f
inn bnreite and ttiui close • he i ':'.,nfuld stnj). K
5 1 3 Iti'iwl l'-e menisei -• p,.-. lion.
5.1.4 Obscrv tiie mu'ls' 'S in the bllre't^ or ' the
lliinid level in tl :>ipclle f.n •nov.'ment over tin ncil 4
ninntes.
5.1.5 For the Orsat analyzer to pass tho leak-check
two conditions must be met.
5.1 5.1 The liqu'd level In each pipette must not fall
below the bottom of the capillary tubing dining this
4-imnilteinterval.
5.1.5.2 The meniscus In tbe burette must not change
by more than 0.2 ml during this 4-ffll nute InK-rval.
5.1.« If the analywr falls the leak-check procedure, all
rubber connections and stopcocks should be cheeked
until the cause of the leak is Identified. Leaking stopcocks
must be disassembled, cleaned, and regreased. Leaking
rubber connections muet be rcpliwcd. After tbe analyzer
Is reassemble'", the leak-rb"ck procedure nttst be
repeated.
J. Ctlnilatimt
t.l Nomenclature.
n ¥i= n ry molecul«r weight, g/g-mole (Ib/lb-mole).
%EA-Percent excess air.
%COi=Percent COi by volume (dry basis).
%Oi= Percent Oi by volume (dry basis).
/oCO = Percont CO by volume (dry basis)
%N,=Percent Njby volume (dry basis).
0.264= Hntio of O. to N. in air, v,v.
0.2SO=.Moleculur woigl,' of N- or CO divided by \00
IS"}!"'1''-'"1'11' weight ,( o» divided by 100.
0.440=Molecular weight • f CO. divided by 100.
.0.2 Percent Kxr-ess Air fileulnte Ibe pcinnt exer*s
air (if appluahlei, by ;ul.stiluting the appropntc.
values of pei-cnt ();, CO,and N; (ob! nneu',,'-!, Scit:o,i
4,l,i> Or 4 _ 1 ;ji 1 j'jijUJlIlO' •>- ]
?04 %Xj; "•' V "0.5 %0()) J 10°
Kqiia' 't>n 3-1
NoTE.-Tlie .'.niation iibove assumes ibal ambient
air is used >s the source of i .. and thai t'ic fuel docs not
contain appreciable amour'- of N, ias do cok.. oven or
blast furnace gases) For t ose cases when -ipprcclfble
amounts of \, are piesen (coal, oil, anil nsiuial gas
do not contain appreciable emounts of N.) or when
oxygen ei-iichinent is uwd niternate methods subject
to approval of 'he Admn li.i'or, aie raniiin d
0.3 Dry Mol.'eular v\e"'ii Use Fnuiii. n i •> fr,
calculate H,e drj molecn' • A-clght of' !b. vaik gas
NOTE.- I he above e<|tui<.on c'oes not consuler arcon
In air (about 0 •• percent, molecular weight of 37 7)
AiwgaiivB enuc ot about t)4 pwccnt is indoduced.'
1 he tester may opt to mcliid • iru-on in Hie au<.' ;is us M
procedures subject to approval of the Adi.-.n blriitor.
7. Ribliogrnpky
Plasti^'f "-'"'in'. ''' S!'?'""!1> ot l1 for,,',:i^ Analysts. Scve-l i e.hiion.
'. J. and M. n. Midgett. Field Reliability
'of Air Pollution Control
.
Val'ldl1?!?,???"' ?iT'\ R- H- Neuu»ht. "n
-------
Section No. 3.2.11
Revision No. 0
Date January 15, 1980
Page 1 of 1
11.0 REFERENCES
1. Smith, Franklin, and D. E. Wagoner. Guidelines for
Development of a Quality Assurance Program: Volume II -
Gas Analysis for Carbon Dioxide, Excess Air, and Dry
Molecular Weight. EPA-650/4-74-005-6, February 1974.
2. Mitchell, William J. On-Site Collaborative Test of
Method 3 of the New Source Performance Standards Using
Modified Orsat Apparatus. Environmental Protection
Agency, Research Triangle Park, N.C., November 1973.
3. Mitchell, William J. On-Site Collaborative Test of
Method 3 of the New Source Performance Standards at a
Municipal Incinerator. Environmental Protection
Agency, Research Triangle Park, N.C., August 1973.
4. Hamil, H. F. and R. E. Thomas, Collaborative Study of
Method for Stack Gas Analysis and Determination of
Moisture Fraction with Use of Method 5. Southwest
Research Institute. EPA-650/4-74-026, June 1974.
5. Hamil, H. F. and R. E. Thomas, Collaborative Study of
Particulate Emissions Measurements by EPA Methods 2, 3,
and 5 Using Paired Particulate Sampling Trains. South-
west Research Institute. EPA-600/4-76-014, March 1976.
6. Flue and Exhaust Gas Analyses. PTC 19.10-1968.
American Society of Mechanical Engineers, New York,
N.Y., 1968.
7. Burrell Manual for Gas Analysts. 7th Ed. Burrell Corp.
Pittsburgh, Penn., 1951.
8. Shigehara, R. T., et al. Validating Orsat Analysis
Data from Fossil Fuel-Fired Units. Stack Sampling News
4(2):21-26, August 1976.
9. Steam Its Generation and Use. 37th Ed. Babcock &
Wilcox Co., N.Y. 1963. pp. 4-11 and 4-12.
10. Quality Assurance Handbook for Air Pollution Measure-
ment Systems, Volume I, Principles. EPA-600/9-76-005,
Environmental Protection Agency, Research Triangle
Park, N. C. March 1976.
-------
Section No. 3.2.12
Revision No. 0
Date January 15, 1980
Page 1 of 6
12.0 DATA FORMS
Blank data forms are provided on the following pages for the
convenience of the Handbook user. Each blank form has the cus-
tomary descriptive title centered at the top of the page. How-
ever, the section-page documentation in the top right-hand corner
of each page of other sections has been replaced with a number in
the lower right-hand corner that will enable the user to identify
and refer to a similar filled-in form in a text section. For
example, Form M3-1.3 indicates that the form is Figure 1.3 in
Section 3.2.1 of the Method 3 Handbook. Future revisions of
these forms, if any, can be documented by 1.3A, 1.3B, etc. Five
of the blank forms listed below are included in this section.
Two are in the Methods Highlights Section as shown by the MH
following the form number.
Form Title
1.3 Procurement Log
2.1 X and R Chart
3.1 (MH) Pretest Preparations
4.1 (MH) On-Site Measurements Checklist
4.2 Gas Analysis Data Form
4.3 Integrated Bag Sampling Data Form
8.1 Checklist for Method 3 for Use by the
Auditor
-------
PROCUREMENT LOG
Item description
Quantity
Purchase
order
number
Vendor
Date
Ordered
Received
Cost
Dispo-
sition
Comments
Quality Assurance Handbook M3-1.3
-------
X AND R CHART
PROJECT
NAME
MEASUREMENT.
_ PERFORMED-
MEASUREMENT
UNITS
DATE
SUM
AVERAGES
RANGE.R
11 II 11 1« IS It I/ II H 30 11 'I >>
IX
tn
u)
u
>
m^
in
u
O
.
c JJc-,
* o •
— o
o
Quality Assurance Handbook M3-2.1
-------
GAS ANALYSIS DATA FORM
PLANT.
DATE_
COMMENTS:
.TEST NO.
SAMPLING TIME (24-hr CLOCK).
SAMPLING LOCATION
SAMPLE TYPE (BAG, INTEGRATED, CONTINUOUS).
ANALYTICAL METHOD
AMBIENT TEMPERATURE
OPERATOR
\^ RUN
GAS ^^\
C02
02 (NET IS ACTUAL 02
READING MINUS ACTUAL
C02 READING)
CO(NET IS ACTUAL CO
READING MINUS ACTUAL
02 READING)
N 2 (NET IS 100 MINUS
ACTUAL CO READING)
1
ACTUAL
READING
NET
2
ACTUAL
READING
NET
3
ACTUAL
READING
NET
AVERAGE
NET
VOLUME
MULTIPLIER
«/100
32/100
^/lOO
28 '100
MOLECULAR WEIGHT OF
STACK GAS (DRY BASIS)
Md-
TOTAL
Quality Assurance Handbook M3-4.2
-------
Date
INTEGRATED BAG SAMPLING DATA FORM
Run number
Plant
Sampling location
Barometric pressure
Ambient temp. °C
Operator
Stack temp. °C
Time
Traverse
point
Rate meter flow,
rate (Q),
cm3/min
Avg =
i
% Dev.a
% Dev. =
Q
100; must be <10%.
avg
Quality Assurance Handbook M3-4.3
-------
CHECKLIST FOR METHOD 3 FOR USE BY THE AUDITOR
Yes
No
OPERATION
Presampling Operation
1. Availability of theoretical value
2. Use of modified Orsat analyzer (0.1-ml
divisions)
On-Site Measurements
3. Setting up and leak testing the samp-
ling train
4. Purging the sampling train with stack
gas prior to collecting the sample
5. Constant rate sampling
6. Transfer of sample from collapsible
bag to the Orsat analyzer
7. Maintaining constant pressure throughout
the test
8. Exposuring the sample to ambient air
9. Spent absorbing reagent
Postsampling Measurements
10. Perform independent calculations using
data from audit
11. Compare the audit value with the field
team's test value
12. Make sufficient passes for complete
absorption of a component gas
13. Minimize volumetric reading error
14. Check/verify applicable records of
apparatus calibration checks and quality
control charts in the field team's home
laboratory
General Comments
Quality Assurance Handbook M3-8.1
-------
t
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 1 of 11
Section 3.3
METHOD 4--DETERMINATION OF MOISTURE IN STACK GASES
OUTLINE
Number of
Section Documentation Pages
SUMMARY 313 2
METHOD HIGHLIGHTS 3.3 g
METHOD DESCRIPTION
1. PROCUREMENT OF APPARATUS
AND SUPPLIES 3.3.1 9
2. CALIBRATION OF APPARATUS 3.3.2 19
3. PRESAMPLING OPERATIONS 3.3.3 7
4. ON-SITE MEASUREMENTS 3.3.4 10
5. POSTSAMPLING OPERATIONS 3.3.5 4
6. CALCULATIONS 3.3.6 8
7. MAINTENANCE 3.3.7 3
8. AUDITING PROCEDURE 3.3.8 4
9. RECOMMENDED STANDARDS FOR
ESTABLISHING TRACEABILITY 3.3.9 1
10. REFERENCE METHOD 3.3.10 5
11. REFERENCES 3.3.11 1
12. DATA FORMS 3.3.12 14
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 2 of 11
SUMMARY
A gas sample is extracted at a constant rate from the
source; moisture is removed from the sample stream and determined
either volumetrically or gravimetrically.
This Reference Method is used for the accurate determination
of moisture content (as needed to calculate emission data) of
stack gas. The Reference Method is often conducted simultane-
ously with a pollutant emission measurement run; when it is,
calculation of percent isokinetic, pollutant emission rate, etc.,
for the run shall be based upon the results of the Reference
Method or its equivalent. Alternative methods capable of yield-
ing results within 1% water of the Reference Method may be used,
subject to the approval of the administrator.
Note: The Reference Method may yield questionable results
when applied to saturated gas streams or to gas streams that
contain water droplets. Therefore, when these conditions exist
or are suspected, a second method for determining the moisture
content shall be used simultaneously with the Reference Method,
as follows. Assume that the gas stream is saturated. Attach a
temperature sensor capable of measuring to ±1°C (2°F) to the
Reference Method probe. Measure the stack gas temperature at
each traverse point during the Reference Method traverse; calcu-
late the average stack gas temperature. Next, determine the
moisture percentage either by using a psychrometric chart and
making appropriate corrections if stack pressure is different
from that of the chart or by using saturation vapor pressure
tables. In cases where the psychrometric chart or the saturation
vapor pressure tables are not applicable (based on evaluation of
the process), alternate methods, subject to the approval of the
administrator, shall be used.
The procedure described in Method 5 for determining
moisture content is acceptable as a Reference Method.
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 3 of 11
The Method Description which follows is based on the method
promulgated in the Federal Register, Vol. 42, No. 160, August 18,
1977.
A complete copy of the Reference Method is contained in
Section 3.3.10. References 1 and 2 in Section 3.3.11 were used
in the subsections concerning the description, calibration, and
maintenance of the sampling train. Data forms are provided in
Section 3.3.12 for the convenience of the Handbook user.
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 4 of 11
METHOD HIGHLIGHTS
Method 4 is a gaseous sampling method for the determination
of water vapor content of stack gas. This method requires fewer
quality control activities than the other methods in this Hand-
book. Since moisture is collected as a gas, the analysis is not
easily biased; furthermore, water vapor is not a regulated pol-
lutant. However, an accurate determination of moisture content
is usually needed to set and determine the isokinetic sampling
rate and also to perform emission data calculations. The accu-
3
racy and precision of the method have been demonstrated to be
acceptable except when applied to saturated gas streams or to
streams that contain water droplets.
The blank data forms at the end of this section may be re-
moved from the Handbook and used as checklists during the pre-
test, field sampling, and posttest operations. Each form has a
subtitle (e.g., Method 4, Figure 2.5) to aid the user in locating
a similar filled-in form in the Method Description. Items/param-
eters that can cause significant error are designated with an
asterisk on each form.
1. Procurement of Equipment - Section 3.3.1 (Procurement
of Apparatus and Supplies) gives the specifications, criteria,
and design features for equipment and materials required for per-
forming Method 4 tests. The sampling apparatus has the same
design criteria as Method 5 with the exception that a pitot tube
system and sample nozzle are not required for collecting the
sample. This section is designed as a guide in the procurement
and initial check of equipment and supplies. The activity matrix
(Table 1.1) at the end of Section 3.3.1 can be used as a quick
reference, and follows the same order as the written descriptions
in the main text.
2. Pretest Preparations - Section 3.3.2 (Calibration of
Apparatus) provides a step-by-step description of the required
calibration procedures. The calibration of the Method 4
equipment is similar to that of Method 5 with the exception that
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 5 of 11
Method 4 sampling is performed at a constant rate not in excess
of 0.021 m3/min (0.75 ft3/min). The calibration section can be
removed and compiled, along with calibration sections for all
other methods, into a separate quality assurance reference manual
for use by calibration personnel. A pretest checklist (Figure
2.5) or similar form should be used to summarize the calibration
data.
Section 3.3.3 (Presampling Operations) provides the tester
with a guide for supplies and equipment preparation for field
tests. Sample impingers may be charged in the base laboratory as
long as the water-filled impinger section and silica gel impinger
are each tightly capped. The pretest preparation form (Figure
3.1) can be used as an equipment checkout and packing list. An
important item in the pretest preparation is the determination of
stack gas saturation or water droplet content. Under these con-
ditions, a specially calibrated stack gas temperature sensor is
required for moisture determination. The methods for packing
and the descriptions of packing containers should help protect
the equipment, but are not required.
3. On-Site Measurements - Section 3.3.4 (On-Site Measure-
ments) contains a step-by-step procedure for performing sampling
and sample recovery. Testing is performed at a constant rate not
to exceed 0.02 m3/min (0.75 ft3/min). When the stack gas is sus-
pected of being saturated or having water droplets, the addition-
=>i nT-~r-<=.Hnr-o for pr-r-nratelv measurnncr the stf-k temperature to
determine the moisture content with the saturated vapor pressure
--^ ^solute stack temperature must be performed and compared
with the Reference Method. The on-site measurement checklist
(Figure 4.4) is provided to assist the tester with a quick method
for checking requirements.
4. Posttest Operations - Section 3.3.5 (Postsampling Oper-
ations) gives the posttest equipment check procedures. Fig-
ure 5.1 or a similar form should be used to provide a summary
of the posttest calibration checks, and should be included in
the emission test report. No control samples are required for
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 6 of 11
analysis since the analysis is only a gravimetric or volumetric
determination of a sample which is large enough to provide an
easy determination.
Section 3.3.6 (Calculations) provides the tester with the
required equations, nomenclature, and suggested number of
significant digits. It is suggested that a programmable calcu-
lator be used if available to reduce the chance of calculation
error.
Section 3.3.7 (Maintenance) provides the tester with a guide
for a routine maintenance program. This program is not required,
but if performed, should reduce malfunctions.
5. Auditing Procedure - Section 3.3.8 (Auditing Proce-
dure) provides a description of necessary activities for con-
ducting performance and system audits. A performance audit of
the data processing and a systems audit of the on-site measure-
ments should provide independent assessments of the quality
of data needed to allow the collaborative test results to be
used in the final data evaluation.
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 7 of 11
PRETEST SAMPLING CHECKS
(Method 4, Figure 2.5)
Date Calibrated by
Meter box number AH@
Dry Gas Meter*
Pretest calibration factor (within 2% of the average
factor for each calibration run)
Impinger Thermometer
Was a pretest temperature correction used? ^ yes no
If yes, temperature correction (within 2°C (4°F) of
reference value)
Dry Gas Meter Thermometer
Was a pretest temperature correction made? ^ yes no
If yes, temperature correction (within 6°C (10.8°F) of
reference value)
Barometer
Was the pretest field barometer reading correct? yes no
Stack Gas Temperature Sensor (if required)*
Was a temperature sensor required for moisture determination pur-
poses? yes no
Was a pretest temperature correction used? _ yes no
If yes, temperature correction (within ±1°C (2°F) over
the entire range)
Did the temperature sensor agree with the reference thermometer
(within ±1°C (2°F) over the range of 10° to 82°C (50° to
180°F»? yes no
*Most significant items/parameters to be checked.
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 8 of 11
PRETEST PREPARATION CHECKLIST
(Method 4, Figure 3.1)
Apparatus check
Probe type
Borosilicate
glass
Quartz
glass
Other
Heater and leak
checked*
Filter
In-stack
Out-stack
Glass wool
Other
Condenser
Impingers
Other
Cooling System
Ice bath
Other
Metering System
Vacuum gauge
Checked*
Pump
Leak
checked*
Thermometers
Calibrated*
Dry gas
meter
Calibrated*
Other
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Packed and
loaded
Yes
No
*Most significant items/parameters to be checked.
(continued)
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 9 of 11
Figure 3.1 (continued)
Apparatus check
Barometer
Mercury
Aneroid
Other
Calibrated*
Quantitative
Instrument
Graduated
cylinder
Trip
balance
Calibrated*
Stack Temperature
Sensor*
Type
Calibrated
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Packed and
loaded
Yes
No
*Most significant items/parameters to be checked.
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 10 of 11
ON-SITE MEASUREMENT CHECKLIST
(Method 4, Figure 4.1)
Procedure used; Reference Approximate
Reference Method
Conducted simultaneously with pollutant emission test?
Impingers properly placed?*
Impinger content: 1st 2nd 3rd
4th Modifications
Cooling System: Crushed ice Other
Sampling time per point
Probe heater (if applicable) on? Temp
Crushed ice in ice bath?
Leak check? (optional) Leakage rate
Sampling rate constant (within 10%)?*
All data properly recorded?*
Posttest leak check?* (mandatory)
Leakage rate*
Analysis - Impinger Content
Method: Volumetric Gravimetric
Measurement of volume of water condensed:
Graduated cylinder Other
Measurement of silica gel: Balance Other
Color of silica gel? Condition
All analytical data properly recorded?
*Most significant items/parameters to be checked.
-------
Section No. 3.3
Revision No. 0
Date January 15, 1980
Page 11 of 11
POSTTEST EQUIPMENT CHECKS
(Method 4, Figure 5.1)
Dry Gas Meter
Pretest calibration factor Y (must be within ±2%)*
Posttest checks, Y.. Y7 (must be within ±5% of
pretest)
Recalibration required? yes no
If yes, recalibration factor Y (must be within ±2%)*
Lower calibration factor Y for calculations (pretest
or posttest)*
Dry Gas Thermometer
Was a pretest meter temperature correcton used? yes no
If yes, temperature correction (within ±3°C (5.4°F)
over range)*
Posttest comparison with mercury-in-glass thermometer
(within +6°C (10.8°F) at room temperature)
Recalibration required? ^_ yes no
Recalibration temperature correction,if used (within
±3°C (5.4°F) over range)*
If yes, no correction is necessary for calculations when meter
thermometer temperature is higher
If recalibration temperature is higher, add correction to aver-
age meter temperature for calculations
Barometer
Was pretest field barometer reading correct? yes no
Posttest comparison mm (in.) Hg [within ±2.5 mm
(0.1 in.) Hg of mercury-in-glass barometer reading]
Was recalibration required? yes __^ no
If yes, no correction is necessary for calculations when the
field barometer has the lower reading
If the mercury-in-glass reading is lower, then subtract the
difference from the field data readings for the calculation
Stack Gas Temperature Sensor (if required)
Posttest comparison [within ±2°C (4°F) of reference
values]*
Was recalibration required? yes no
*Most significant items/parameters to be checked.
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 1 of 9
1.0 PROCUREMENT OF APPARATUS AND SUPPLIES
A schematic of the sampling train used in Method 4 is shown
in Figure 1.1. Commercial models of this train are available.
For those who desire to build their own, construction details
are published in APTD-0581. Allowable modifications are de-
scribed in the following sections.
The operating, maintenance, and calibrating procedures for
2
the sampling train are in APTD-0576. Since correct usage is
important to obtaining valid results, all users should read the
document and adopt the procedures unless alternatives are out-
lined herein.
Applicable specifications, criteria, and/or design features
are in this section to aid in the selection of equipment which
assures collection of data of good quality. Procedures and
limits (where applicable) for acceptance checks are given. The
descriptive title, the identification number (if applicable), and
the results of the acceptance check are recorded in the procure-
ment log, which is dated and signed by the individual performing
the check. An example of a procurement log is shown in
Figure 1.2, and a blank copy of the log is in Section 3.3.12 for
the convenience of the Handbook user. If calibration is required
as part of the acceptance check, the data are to be recorded in a
calibration log. Table 1.1 at the end of this section is a sum-
mary of the quality assurance activities for the procurement and
acceptance of apparatus and supplies.
1.1 Sampling Apparatus
1.1.1 Probe - The sampling probe should be a borosilicate
(Pyrex), quartz glass, or stainless steel tubing with an outside
diameter (OD) of about 16 mm (0.625 in.), and it should be en-
cased in a stainless steel sheath with an OD of 25.4 mm (1 in.).
Alternatively, other metals or plastic tubing may be used if
approved by the administrator.
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 2 of 9
O
X!
-P
OJ
O
c
QJ
^
Q)
m
cu
-H
(0
M
C
•H
e
n3
U)
0)
M
•H
O
S
-------
Item description
He\ex~ ^x>X
\
Quantity
<3
Purchase
order
number
1 1 / O^ /""*N
1 t"5O 1 V^h'
Vendor
Perre^tv;
Eop \wieriV
r
Date
Ordered
(^Q\~tS
Received
Q.\>^-\ "~]O
Cost
?c^5"00/-€A
Dispo-
sition
Oo\ \V5flxW?
-* PxSQ^Lj1
Comments
CxlA\V)XCkVQ
A \a
%^«>\ n
^TJ D 50 w
0) (U (D CO
vQ r+ < O
fl> fl> H- ft
CQ H-
CO C| H. o
0 3 §
Hi d 525
D) tZj O
to 1^ O *
CO
Figure 1.2 Example of a procurement log. ui0co
VD
CO
O
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 4 of 9
Either borosilicate or quartz glass liners may be used for
stack temperatures up to about 480°C (900°F), but quartz glass
liners should be used from 480° to 900°C (900° to 1650°F).
Either type of liner may be used at the higher temperatures for
short periods of time with administrator approval. However, the
absolute upper limits—the softening temperatures of 820°C
(1508°F) and 1500°C (2732°F)--for borosilicate and quartz respec-
tively must be observed.
A heating system is required which will maintain an exit gas
temperature of 120° ±14°C (248° ±25°F) during sampling. Other
temperatures may be specified by a subpart of the regulations and
must be approved by the administrator for a particular applica-
tion. Since the actual probe outlet temperature is not usually
monitored during the sampling, probes constructed in accordance
to APTD-0581 and utilizing the calibration procedures in
APTD-05762 will be acceptable.
Upon receiving a new probe, the user should visually check
it for specifications: that is, is it the length and composition
ordered? The probe should be visually checked for breaks or
cracks, and it should be checked for leaks on a sampling train
(Figure 1.1). The probe heating system should be checked as
follows:
1. Connect the probe with a nozzle attached to the inlet
of the pump.
2. Electrically connect and turn on the probe heater for 2
or 3 min. The probe should become warm to the touch.
3. Start the pump and adjust the needle valve until a flow
o q
rate of about 0.02 m /min (0.75 ft /min) is achieved.
4. Be sure the probe remains warm to the touch. The
heater should be capable of maintaining the exit air temperature
at a minimum of 100°C (212°F) under these conditions. If it can-
not, the probe should be repaired, returned to the supplier, or
rejected.
1.1.2 Condenser - Four impingers should be connected in series
with leak-free ground-glass fittings or any similarly leak-free
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 5 of 9
noncontaminating fittings. The first, third, and fourth imping-
ers must be the Greenburg-Smith design modified by replacing the
inserts with an unconstricted 13 mm (0.5 in.) ID glass tube
extending to within 13 mm (0.5 in.) of the flask bottom. The
second impinger must be a Greenburg-Smith with the standard tip
and plate. Modifications—for example, using flexible connec-
tions between impingers, using materials other than glass, or
using a flexible vacuum hose to connect the filter holder to the
condenser—may be used if approved by the administrator. The
fourth impinger outlet connection must allow insertion of a
thermometer capable of measuring ±1°C (2°F) of true value in the
range of 0° to 25°C (32° to 77°F).
Alternatively, any system that cools the gas stream and
allows measurement of the condensed water and the water vapor
leaving the condenser, each to within 1 ml or 1 g, may be used
with approval of the administrator.
Upon receipt of a standard Greenburg -Smith impinger, the
user should fill the inner tube with water. If the water does
not drain through the orifice in <6 to 8 s, the impinger tip
should be replaced or enlarged to prevent an excessive pres-
sure drop in the sampling system. Each impinger should be
checked visually for damage—breaks, or cracks, or manufacturing
flaws such as poorly shaped connections.
1.1.3 Temperature Gauge - A thermometer capable of measuring
within 1°C (2°F) is located at the outlet of the fourth impinger.
The thermometer should be checked upon receipt for damage—for
example, dents, bent stem, broken face.
1.1.4 Cooling System - An ice bath container and crushed ice (or
equivalent) are needed for condensing the moisture.
1.1.5 Metering System - The metering system should consist of a
vacuum gauge; a leak-free vacuum pump; thermometers capable of
measuring ±3°C (5.4°F) of true value in the range of 0° to 90°C
(32° to 194°F); a dry gas meter with 2% accuracy at the required
sampling rate; and related equipment as shown in Figure 1.1.
Other metering systems capable of maintaining sampling rates
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 6 of 9
within 10% of constant rate and capable of determining sample
volumes to within 2% may be used if approved by the administra-
tor. Sampling trains with metering systems designed for sampling
1 7
rates higher than that described in APTD-0581 and APTD-0576 may
be used if the above specifications can be met.
Upon receipt or after construction of the equipment, the
user should perform both positive and negative pressure leak
checks before beginning the system calibration procedure de-
scribed in Section 3.3.2. Any leakage requires repair or re-
placement of the malfunctioning item.
1.1.6 Differential Pressure Gauge - The differential pressure
gauge should be an inclined manometer or the equivalent to
measure the orifice pressure differential.
Initially, check the gauge against a gauge-oil manometer at
a minimum of three points: 0.64 mm (0.025 in.); 12.7 mm (0.5
in.); and 25.4 mm (1.0 in.) EUO. The gauge should agree within
5% of the gauge-oil manometer. Repair or return to the supplier
any gauge which does not meet these requirements.
1.1.7 Barometer - A mercury, aneroid, or other barometer capable
of measuring atmospheric pressure to within 2.5 mm (0.1 in.) Hg
is required.
A preliminary check of a new barometer should be made
against a mercury-in-glass barometer or the equivalent. In lieu
of this, the absolute barometric pressure may be obtained from a
nearby weather service station and adjusted for the elevation
difference between the station and the sampling point. Either
subtract 2.5 mm Hg/30 m (0.1 in. Hg/100 ft) for an elevation in-
crease or add the same for an elevation decrease from the station
value. If the barometer cannot be adjusted to agree within
2.5 mm (0.1 in.) Hg of the reference barometric pressure, it
should be returned to the manufacturer.
1.1.8 Graduated Cylinder and/or Triple Beam Balance - A gradu-
ated cylinder or triple beam balance may be used to measure the
water condensed in the impingers during sampling. Additionally,
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 7 of 9
the graduated cylinder may be used to measure the water initially
placed in the first and second impingers. In either case, the
required accuracy is 1 ml or 1 g; therefore, the cylinder must
have subdivisions <2 ml, and the triple beam balance is usually
capable of weighing to the nearest 0.5 g.
1.1.9 Stack Gas Temperature Sensor - A thermocouple, thermom-
eter, or equivalent, for measuring the stack gas temperature
within ±1°C (2°F) is required when the gas stream is suspected of
being saturated or containing water droplets. This accuracy
should be in the range of about 10° to 82°C (50° to 180°F). Upon
receipt check the specifications and calibrate as described in
Section 3.3.2.
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 8 of 9
Table 1.1 ACTIVITY MATRIX FOR PROCUREMENT AND
ACCEPTANCE OF EQUIPMENT
Apparatus
and
supplies
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Sampling probe
liner
Specified material of
construction; equipped
with heating system
capable of maintaining
120° ±14°C (248° ±25°F)
Visually check, and
run heating system
Repair, re-
turn to sup-
plier, or re-
ject
Differential
pressure
gauge
(manometer)
Meet criteria (Method 2,
Sec 3.1.2); agree
within 5% of gauge-oil
manometer
Check against gauge-
oil manometer at a
minimum of 3 points:
0.64(0.025); 12.7
(0.5); 25.4(1.0) mm
(in.) HO
Repair or
return to sup-
plier
Vacuum gauge
Range 0-760 mm (0-30
in.) ±2.5 mm (0.1 in.)
Hg at 380 mm (15 in.)
Hg
Check against a mer-
cury U-tube manometer
upon receipt
Adjust or re-
turn to sup-
plier
Vacuum pump
Leak free and capable
of maintaining a flow
rate of 0.02-0.03 m /
min (0.66-1.0 ft /min)
for pump inlet vacuum
of 380 mm (15 in.) Hg
Check upon receipt
for leaks and capaci-
ty
Repair or re-
turn to sup-
plier
Orifice meter
AH@ of 46.74 ±6.35 mm
(1.84 ±0.25 in.) H20;
not mandatory
Upon receipt, visual-
ly check for damage,
and calibrate against
wet test meter
Repair if
possible; other-
wise return to
supplier
Impingers
Standard stock glass;
pressure drop across
impingers not excessive
(Subsec 1.1.6)
Visually check upon
receipt; check pres-
sure drop (Subsec
1.1.6)
Return to
supplier
(continued)
-------
Section No. 3.3.1
Revision No. 0
Date January 15, 1980
Page 9 of 9
Table 1.1 (continued)
Apparatus
and
supplies
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Dry gas meter
Capable of measuring
total volume within ±2%
at a flow rate of 0.02
m /min (0.75 ft /min)
Check for damage upon
receipt; calibrate
against wet test
meter (Sec 3.3.2)
Reject if
damaged, behaves
erratically,
or cannot be
properly adjusted
Thermometers
Should read within
±1°C of true value
in the range of 0°C to
25°C for impinger
thermometer, and ±3°C
of true value in the
range of 0° to 90°C
for dry gas meter
thermometers
Check upon receipt
for dents or bent
stem; calibrate
against mercury-in-
glass thermometer
(Sec 3.3.2)
Reject if unable
to calibrate
Barometer
Capable of measuring
atmospheric pressure
within ±2.5 mm (0.1
in.) Hg
Check against a mer-
cury-in-glass barom-
eter or equivalent;
calibrate ( Sec
3.1.2)
Determine cor-
rection factor
or reject if
difference is
more than ±2.5
mm (0.1 in.) Hg
Graduated
cylinder
Glass, Class-A, 250 ml,
subdivisions <2 ml
Upon receipt, check
stock number, cracks,
breaks, and manufac-
turer flaws
Replace or re-
turn to sup-
plier
Trip balance
500-g capacity; capable
of measuring within
±0.5 g
Check with standard
weights upon receipt
As above
Stack gas
temperature
sensor
Within ±1°C (2°F) in
range of 10° to 82°C
(50° to 180°F)
Upon receipt check
specifications; then
calibrate (Sec 3.3.2)
As above
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 1 of 19
2.0 CALIBRATION OF APPARATUS
Calibration of the apparatus is one of the most important
functions in maintaining data quality. The detailed calibration
procedures included in this section are designed for the equip-
ment specified by Method 4 and described in the previous section.
A laboratory log book of all calibrations must be maintained.
Table 2.1 at the end of this section summarizes the quality
assurance activities for calibration.
2.1 Metering System
2.1.1 Wet Test Meter - Wet test meters are calibrated by the
manufacturer to an accuracy of +0.5%. The calibration of the
wet test meter must be checked initially upon receipt and yearly
thereafter. A wet test meter with a capacity of 3.4 m /h
(120 ft3/h) will be necessary to calibrate the dry gas meter.
For large wet test meters (>3£/rev), there is no convenient
method to check the calibration. For this reason, several
methods are suggested, and other methods may be approved by the
administrator. The initial calibration may be checked by any of
the following methods:
1. Certification from the manufacturer that the wet test
meter is within +1% of true value at the wet test meter dis-
charge, so that only a leak check of the system is then required.
2. Calibration by any primary air or liquid displacement
method that displaces at least one complete revolution of the wet
test meter.
3. Comparison against a smaller wet test meter that has
previously been calibrated against a primary air or liquid dis-
placement method, as described in Section 3.5.2.
4. Comparison against a dry gas meter that has previ-
ously been calibrated against a primary air or liquid displace-
ment method.
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 2 of 19
The calibration of the test meter should be checked annu-
ally. The calibration check can be made by the same method as
that of the original calibration, with the exception that the
comparison method need not be recalibrated if the calibration
check is within +1% of the true value. When this agreement is
not obtained, then the comparison method or wet test meter must
be recalibrated against a primary air or liquid displacement
method.
2.1.2 Sample Meter System - The sample meter system—consist-
ing of the pump, vacuum gauge, valves, orifice meter, and dry gas
meter—is initially calibrated by stringent laboratory methods
before it is used in the field. After the initial acceptance,
the calibration is rechecked after each field test series. This
recheck is designed to provide the tester with a method that can
be used more often and with less effort to ensure that the cali-
bration has not changed. When the quick check indicates that the
calibration factor has changed, the tester must again use the
complete laboratory procedure to obtain the new calibration
factor. After recalibration, the metered sample volume must be
multiplied by either the initial or the recalibrated calibration
factor that yields the lowest gas volume for each test run.
Before initial calibration of the metering system, a leak
check should be conducted. The meter system should be leak free.
Both positive (pressure) and negative (vacuum) leak checks should
be performed. Following is a pressure leak-check procedure that
will check the metering system from the quick disconnect inlet
to the orifice outlet and will check the orifice-inclined manom-
eter for leaks:
1. Disconnect the orifice meter line from the downstream
orifice pressure tap (the one closest to the exhaust of the
orifice), and plug this tap.
2. Vent the negative side of the inclined manometer to the
atmosphere. If the inclined manometer is equipped with a three-
way valve, this step can be performed by merely turning the
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 3 of 19
three-way valve that is on the negative side of the orifice-
inclined manometer to the vent position.
3. Place a one-hole rubber stopper with a tube through its
one hole in the exit of the orifice, and connect a piece of
rubber or plastic tubing to the tube, as shown in Figure 2.1.
4. Open the positive side of the orifice-inclined manom-
eter to the "reading" position. If the inclined manometer is
equipped with a three-way valve, this will be the line position.
5. Plug the inlet to the vacuum pump. If a quick discon-
nect with a leak-free check valve is used on the control module,
the inlet will not have to be plugged.
6. Open the main valve and the bypass valve.
7. Blow into the tubing connected to the end of the
orifice until a pressure of 127 to 178 mm (5 to 7 in.) H20 has
built up in the system.
8. Plug or crimp the tubing to maintain this pressure.
9. Observe the pressure reading for a 1-min period. No
noticeable movement in the manometer fluid level should occur.
If the meter box has a leak, a bubbling-type leak-check solution
may aid in locating the leak(s).
After the metering system is determined to be leak free by
the positive leak-check procedure, the vacuum system to and in-
cluding the pump should be checked by plugging the air inlet to
the meter box. If a quick disconnect with a leak-free stopper
system is presently on the meter box, then the inlet will not
have to be plugged. Turn the pump on, pull a vacuum within
75 mm (3 in.) Hg of absolute zero, and observe the dry gas
meter. If the leakage exceeds 1.5 x 10~4 m /min (0.005 ft /min),
the leak(s) must be found and minimized until the above specifi-
cations are satisfied.
Leak checking the meter system before initial calibration
is not mandatory, but is recommended.
Note; For metering systems having diaphragm pumps, the
normal leak-check procedure described above will not detect
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 4 of 19
e
0)
cn
tn
G
-rH
M
-H
4->
•H
CO
O
CN
o;
-H
CM
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 5 of 19
leakages within the pump. For these cases, the following
leak-check procedure is suggested: make a 10-min calibration
3 3
run at 0.00057 m /min (0.02 ft /min); at the end of the run,
take the difference of the measured wet test meter and dry gas
meter volumes; divide the difference by 10 to get the leak
3
rate. The leak rate should not exceed 0.00057 m /mm
(0.02 ft3/min).
Initial calibration - The dry gas meter and orifice meter
can be calibrated simultaneously and should be calibrated when
first purchased and any time the posttest check yields a Y
outside the range of the calibration factor Y +0.05Y. A
calibrated wet test meter (properly sized, with +1% accuracy)
should be used to calibrate the dry gas meter and the orifice
meter.
The dry gas meter and the orifice meter should be
calibrated in the following manner:
1. Before its initial use in the field, leak check the
metering system, as described in Subsection 2.1.2. Leaks, if
present, must be eliminated before proceeding.
2. Assemble the apparatus, as shown in Figure 2.2, with
the wet test meter replacing the probe and impingers—that is,
with the outlet of the wet test meter connected to a needle
valve that is connected to the inlet side of the meter box.
3. Run the pump for 15 min with the orifice meter
differential (AH) set at 12.7 mm (0.5 in.) H2O to allow the
pump to warm up and to permit the interior surface of the wet
test meter to be wetted.
4. Adjust the needle valve so that the vacuum gauge on
the meter box will read between 50 and 100 mm (2 to 4 in. ) Hg
during calibration.
5. Collect the information required in the forms
provided (Figure 2.3A or 2.3B). Sample volumes, as shown,
should be used.
-------
AIR INLET
MET TEST METER
AIR OUTLET >v\~. ^^j<( WATER OUT
ORIFICE
MANOMETER
Figure 2.2 Sample meter system calibration setup.
WATER
LEVEL
GAUGE
h^ O £0 C/3
0) B> (t> (D
id ft < O
(D (D H- rt
, CO H-
cn^ H-0
3 ° 3
HiC 2J
0* *? n
" O ?
OJ
M o •
U1 u
10
00
O
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 7 of 19
Date
Meter box number
Barometric pressure, ?b = cD9-OC) in- Hg Calibrated by N^JGcVj
Orifice
manometer
setting
(AH),
in. H20
0.5
1.0
1.5
2.0
3.0
4.0
Gas volume
Wet test
meter
(V )
fl3
5
5
10
10
10
10
Dry gap
meter
(vd),
ft3
363--SV&
£/(,.
Time
(6),
min
^9-!
Avg
Y.
i
1.995
AH@±
in. H«(
A 3V
AH,
in.
H20
.5
1.0
1.5
2.0
3.0
4.0
AH
13.6
0.0368
0.0737
0.110
0.147
0.221
0.294
V P,(t, + 460)
w bv d
*i ~ AH
u ft> + ^^ ^ ft- + /ifin i
" jl-l-V T i^ /-y \*- T tOU^
d b Ij.o
l~ $•&&• o cS'2*-(*>~>
^\f-- f) -jC^ ")^" -54^ /-54/N/ •Slb'5~ ^
"
ffl 0.0317 AH w
^i - P (t + 460) _ V
c^.^/vco.^r^) ^3^3"^ /^ "^"^ ^^> •^5" •- ^
If there is only one thermometer on the dry gas meter, record the temperature
under t,.
d
Figure 2.3A Dry gas meter calibration data form (English units)
(front side)
-------
Nomenclature:
Vw = Gas volume passing through the wet test meter, ft .
Vd = Gas volume passing through the dry gas meter, ft .
tw = Temperature of the gas in the wet test meter, °F.
td = Temperature of the inlet gas of the dry gas meter, °F.
td = Temperature of the outlet gas of the dry gas meter, °F.
o
td = Average temperature of the gas in the dry gas meter, obtained by the average t, ;
t, , °F. i
o
AH = Pressure differential across orifice, in. H~0.
Y. = Ratio of accuracy of wet test meter to dry gas meter for each run; tolerance Y- =
Y ±0.02Y. 1
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs;
tolerance Y = Y ±0.01Y.
AH(5K = Orifice pressure-differential at each flow rate that gives 0.75 ft3/min of air at
standard conditions for each calibration run, in. H^O; tolerance = AH@ ±0.15
(recommended).
_ hi O pd w
AH@ = Average orifice pressure differential that gives 0.75 ft /min of air at standard vq ?t <; o
conditions for all six runs, in. H20; tolerance = 1.84 ±0.25 (recommended). ® "> £"
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 9 of 19
Date
Meter box number \— is/] —
Barometric pressure, P. = 13L, mm Hg Calibrated by
V\!
Orifice
manometer
setting
(AH),
mm HO
10
25
40
50
75
100
Gas volume
Wet test
meter
.
V ., (P , "^ -1 W > J (t «~ 2.IJ)
d d 13.6 w
£0. i^^)C 73 4^? £ <=5 9 / J
—771-5— 7^^^ f *7.3 1^) Co> *5 7~) ~
c
_ 0.00117 AH [(tw+273> 9]2
^1Li P (t + 273) V
L&. oo/ 1 "7 ) c j&2_ rr-i>y/yc /Qk^s
C~73 L,^) C^^ f "^ ] £? • ^
If there is only one thermometer on the dry gas meter, record the temperature
under t,.
d ,
Figure 2.3B Dry gas meter calibration data form (metric units).
(front side)
-------
and
Nomenclature :
Vw = Gas volume passing through the wet test meter, m .
V^ = Gas volume passing through the dry gas meter, m .
t = Temperature of the gas in the wet test meter, °C.
W
td = Temperature of the inlet gas of the dry gas meter, °C.
td = Temperature of the outlet gas of the dry gas meter, °C.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average of t,
U 4- Op U •
M ' 1
o
AH = Pressure differential across orifice, mm H«0.
Y. = Ratio of accuracy of wet test meter to dry gas meter for each run; tolerance Y- =
Y +0.02Y. 1
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs;
tolerance Y = Y +0.01Y.
AH@^ = Orifice pressure differential at each flow rate that gives 0.021 m3 of air at standard
conditions for each calibration run, mm H?0; tolerance AH@. = AH@ +3.8 mm H^O
(recommended). 1
_ V O W en
AH@ = Average orifice pressure differential that gives 0.021 m of air at standard con- ^ ft < o
ditions for all six runs, mm H2O; tolerance AH@ = 46.74 +6.3 mm H20 (recommended). n n £g.
h- ' ^ H- O
0 = Time of each calibration run, min. ° 3 § 0
o g !z;
P, = Barometric pressure, mm Hg. "** o .°
JJ (— !*"< .
Figure 2.3B. Dry gas meter calibration data (metric units). (backside)
M O •
<-n Co
CO
o
-------
Yl -
" Y2 '
h Y3 -
> Y4 ^
h Y5 -
h Y6
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 11 of 19
6. Calculate Y. for each of the six runs, using the equa-
tion in Figure 2.3A or B under the Y^ column, and record the
results on the form in the space provided.
7. Calculate the average Y for the six runs using the
following equation:
„ _
JL ~"~
Record the average on Figure 2.3A or B in the space provided.
8. The dry gas meter should be cleaned, adjusted, and
recalibrated, or rejected if one or more values of Y fall outside
the interval Y +0.02Y. Otherwise, the average Y (calibration
factor) is acceptable and will be used for future checks and
subsequent test runs .
9. Calculate AH@. for each of the six runs using the
equation in Figure 2. 3 A or B under the AH@. column, and record
on the form in the space provided.
10. Calculate the average AH@ for the six runs using the
following equation:
AH@, + AH@0 + ABSL + AH@, + AH®,- + AH®,-
AH@ = - 1 - 2 - 3 - 4 - 5 - 6
Record the average on Figure 2.3A or B in the space provided.
11. Adjust the orifice meter or reject it if AH@. varies
by more than +3.9 mm (0.15 in.) H~0 over the range of 10 to
100 mm (0.4 to 4.0 in.) H20. Otherwise, the average AH@ is
acceptable and will be used for subsequent test runs.
Posttest calibration check - After each field test series,
conduct a calibration check of the metering system, as in Sub-
section 2.1.2, except for the following variations:
1. Three calibration runs at a single intermediate orifice
meter setting may be used with the vacuum set at the maximum
value reached during the test series. The single intermediate
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 12 of 19
orifice meter setting should be based on the previous field test.
A valve must be inserted between the wet test meter and the inlet
of the metering system to adjust the vacuum.
2. If a temperature-compensating dry gas meter was used,
the calibration temperature for the dry gas meter must be within
+6°C (10.8°F) of the average meter temperature during the test
series.
3. Use Figure 2.4A or 2.4B, and record the required
information.
If the calibration factor Y deviates by <5% from the
initial calibration factor Y (determined in Subsection 2.1.2),
then the dry gas meter volumes obtained during the test series
are acceptable. If Y deviates by >5%, recalibrate the metering
system (as in Subsection 2.1.2), and use whichever meter
coefficient (initial or recalibrated) that yields the lowest gas
volume for each test run.
Alternate procedures—for example, using the orifice meter
coefficients—may be used, subject to the approval of the
administrator.
2.2 Temperature Gauges
2.2.1 Impinger Thermometer - The thermometer used to measure the
temperature of the gas stream exiting the impinger train should
initially be compared with a mercury-in-glass thermometer which
meets ASTM E-l No. 63C or 63F specifications. The procedure is
as follows:
1. Place both the reference thermometer and the test
thermometer in an ice bath. Compare readings after they both
stabilize.
2. Remove the thermometers from the bath and allow both
to come to room temperature. Again, compare readings after
they both stabilize.
3. Accept the test thermometer if its reading agrees
within ±1°C (2°F) of the reference thermometer reading at both
temperatures. If the difference is greater than ±1°C (2°F),
-------
"T*
c
j£
P>-
V
1
§
f> \-
£
\
' i 1
c_i *•*
^•- to
4-1 01
d 4J
efl 01
rH M
CM CM
IN
i
t
^-
U
,
5~
u.
S-l
vw
01 e
^a a
3
fl ^
01
X 4-1
O 01
43 S
S-l to
01 efl
4-1 60
Ol
}-l
Os
C^
"^s
IS^i
«x t
-»s.
cr
Q
ttO
""«
•
d
--H
.
(•v^i
Ol " .
4_) ,\f.
(3 Q|
II
rO
*
---^
CO
^jT
^
CM
^
01
S-l
a
to
co
OJ
S-l
PH
S-l
u u
& -H
a 4-j
d 01
4-1 O
10 S-l
01 efl
H pq
•H
o
3
ID
4-1
,0
PH
O
5
4-
^^
3
^ —
— ^.
VO
co
rH
2
T)
•H
g
S
u
«
01
»s
60
d
•rl
4-1
4-1
OJ
S **^
•H
Q
H ^
01
S-l
a
4-1
efl
01
ft
E
01
H
01
rH
O
CO
efl
O
IH
01
4-1
01
B
to
efl
60
r^>
S-l
a
4-1
CO
01
01
to
tfl
60
S-l
Q
4-1
to
01
4-1
4J
01
^
SH
0)
01 4-J
U it
•H E
4H O
•H d
S-4 efl
0 S
01 (0
60
efl /-
S-l
01 4-1
^
e v-
S-i •
eu / — •
4_>
01 >
E ^-
n
60
d •
•H >~^
4-1 >32
4-1 ^
(U ^^
to
t
< P
•0 0
/
\
0
T3
t
•^
\
•H
•Q
t
•*
\
O
CO
O 4
H
CO
3 4.
4.
O
C1
W
•
d
•rt
60
d
•rH
d
•H
S
•-i
PM
o
ta
o
1-1
-1
J
-1
g
i ' ^
Ok"
vj r_\
Jjj
w
0^
C"**
Q^
j|~
^j'*'
/-»
%J
K)
tr>
CVj
Cv'
_,
^=»a.
ON
r.
*
•O
^Sr^
^
hA
^.
OQ
/*"/
L
>** -MI
^* OR
•O f\,
3*+
fe ^*^
**\ A
<*-> W
o
rH
~""V
— -
-X*
«—
O
rH
O
rH
•o
l)
+^
S-l
01
II T3
tH 3
OJ
S-l
a
4-1
efl
S-l
OJ
01
01
XI
4-1
•o
o
u
01
S-l
*
S-l
01
4-1
-OJ '
e
to
efl
60
^
S-l
•o
01
XI
d
o
S-l
01
±J
01
s
0
|
01
XI
4-1
01
d
o
>»
rH
d
o
to
•H
01
S-l
01
XI
4-1
4H
M
efl
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 13 of 19
T3
4J
"S
*
w
co co
4-1 4-1
4-1 4H
S-l S-l
0) OJ
4-1 4-1
1 i
4-1
CO CO
oi a)
4-> bo
4-> >>
01 M
S -o
01 01
X) XI
4-1 4->
XI XI
60 60
3 3
0 O
S-l S-l
X! X!
01
S-l
01
XI
3
4-1
60
d
•H
to
10
efl
ft
01
rH
O
^
to
efl
C3
II
5
^
4-1
60
d
•H
M
to
efl
ft
01
Q
a
rH
O
^
to
efl
O
II
T3
^
O
si
Ol
4-1
01
4-1
to
01
4-1
01
OJ
d
•H
to
efl
60
.S
4-1
4H
O
01
S-l
a
efl
01
B1
01
H
II
*
4->
O
S-l
01
1
CO
tfl
00
S-l
01
XI
4-1
MH
o
to
efl
60
01
rH
d
•H
Ol
XI
4->
4H
O
01
S-l
a
efl
S-l
01
&
01
H
II
•H
TJ
4->
0
si
01
4-1
=
CO
n>
00
£
13
OJ
XI
4-1
4H
0
to
60
4-1
01
rH
a
o
01
4-1
H-4
O
0)
a
4-1
efl
S-i
01
81
01
EH
II
O
^
I i
01
60
efl
01
efl
01
XI
4-1
•o
01
•rH
43
O
*N
01
4-)
CO
rt
00
•0
OJ
XI
4-1
d
•H
to
efl
60
01
XI
4-1
4-1
0
01
S-l
3
4-1
efl
SH
01
ft
S
01
01
60
efl
S-l
01
<
II
T3
4_>
1 across orifice, in. HLO.
efl
•H
4-1
d
01
^
01
4-t
•H
OJ
S-l
to
10
01
CM
II
M
•g
XI
u
OJ
S-l
o
4H
S-l
0)
4-1
01
s
3
1 M
0
4-1
1-1
01
4-1
01
4-1
to
Ol
4-1
01
4H
O
U
tfl
M
a
u
u
4H
O
0
•H
4-1
efl
II
• H
^4
OJ
S-l
4-1
rH
rH
03
SH
O
4H
IH
CO
00
t
o
OJ
4-1
OJ
4-1
to
OJ
4-1
4-1
OJ
4H
o
S-l
3
u
u
efl
4H
O
o
•H
4->
S-l
01
60
SH
0)
S
M
>H
>H
m
0
4-1
to
01
4-1
-------
1
-/-
c
r£
^
i-
>
>
^
s
e— "f-
fC
• .
0^
O«N
C
>-l
^ 4-1
4-J CO
d oi
CO 4->
rH 01
CM s-i
Oi
rv
^v
,
s^
*v
^
£x
1
Vi.
t 1
M
U 01
01 X>
§3
d
d
i-i
X 01
0 4->
X> 01
M
01 to
4-1 CO
01 00
J3
J7
O>
^
— •»
5
0
Q
00
.1
O
sq
Q
II
^
t
•"^
.^
li
_*
^4
n
PL.
•«
01
M
I CO
' w
0)
ft
01 U
Xl -H
§ £
H 4)
4, §
CO M
01 <0
H m
>rJ
/— \
CO
&4
>
CO
Csl
+
4-1
j—
<
^.
CM
^
i
^
CO
,- 1
a
D
•H
~
00
d
3 -ri
01
f^
rj
4J
<0
M
01
H
01
j3
i-H
0
^
CO
(0
01
4-1
i
CO
CO
00
b*^
Q
•P
CO
01
4-1
CO
CO
00
e?
a
4-1
M
01
4J
4->
01
2t
l-l
01
0) 4-1
U 01
«H O
•H fl
l-l CO
o a
U
CO
>
0
.f
H
01 CO
00 •
eo r^
l-l '
01 4-1
**
1 \ ,
+• "
0) /—•
rH
4.) '
3 4->
O *-
•
4J /~
01
4-)
4J
01
CO
^
©"
C.
T3 0
O
O
•H
rH T3
rt ^j
HH ^
^
0) ^
i
M •
01 /->
4J '
01 >
a v-
M •
OI -->
4J
a ^"^
M
00
w
d
•H
a
3
CJ
O
CJ
O
£ CJ
O
CO
o e
co
3
3
d -o
•rt ^^
4J ^
^
~; ^
C( r~
^c ^
j /
5 ;
X"
ro ^
C
Vj"*'
Vs"
o
t
H_
-^
1^
'o
-.
1 ^
vC
n
r
\f
-^
n
(
.
iy
^
— -
'IS
/
*^», ^
|T
V1*
• °°
x^ V"
*\. *>*
9 '
10
•
•>JS
or
5
CO
•
ro
•
II
n the dry gas meter, record the temperature under t.
o
M
01
4-1
i
§
B
4-1
0)
d
0
^>
rH
d
o
CO
•H
01
01
XI
01
4-1 ^4
M 01
xl
CO CO
a a
*k #S
01 01
4-) 4-1
01 01
a a
4_)
co 2
{U w,
4J 00
9 -o
01 01
XI XI
4-1
•a
a
o
xl
4-1
d0
•H
CO
to
ft
01
rH
O
^
CO
18
O
II
u
^
P
•a
3
O
XI
P
00
d
•H
CO
CO
CO
ft
OI
rH
O
^
CO
CO
O
II
T)
>
CJ
o
M"
01
4-1
01
P
CO
01
4-1
4-1
01
01
XI
P
d
•H
CO
CO
00
JS
P
4H
O
01
1-4
rj
P
10
M
01
p4
Q
OI
H
II
S
P
CJ
o
01
P
i
CO
a
£
P
o
to
CO
00
4-1
01
rH
d
• H
1
4-1
0
OI
^4
3
+J
10
V4
01
Qj
g
01
H
II
•H
•0
P
o
l-l
01
4-1
01
a
0)
CO
00
1-1
•o
01
XI
4->
4-1
O
ca
CO
00
01
1— 1
3
O
01
4.)
4-1
O
0)
^4
3
ca
l-l
01
O*
Q
H
II
O
•O
4-1
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 14 of 19
CJ
0
o
T3
P
d
CO
•H
T3
P •— .
•" W
4-1 CO jj
o d tj
3 "d
QJ M M
oo 3
co 01
i-i oi n
0) l-l
> xi •£
« " ^
S
d CO 01 ^
•H 01 P
10 oi rd
4.1 V4 a 4->
0 ^ co T3
*• I-i "S
| a ^ TJ
» o 2
w . rt 2 S
R) o M ^ -fj
M °CM ^4 -H
W >. 0) '-j
>> H P t!
O i.
0) « P P „.
XI 0) w V
P U M OI -P
•H OI P CD
.3 3 t! P s
* S s S +J
10 P • • W
00
4->
4-1
O
OI
3
4-1
0)
81
01
4J
OI
00
CO
l-l
01
II
T3
4-1
ID
M
O
V4
U
CO
1— 1
CO
•H
d
01
M
01
4-1
•r-t
•o
01
M
3
ca
0)
II
J-J-j
*g
ca
OI
P
P
01
*
o
u
CO
14
3
u
CO
4-1
O
0
•H
P
II
•H
4-1 >H
O lO
o
o d
CO + I
u
U P
ce ca
OI
4-1 4-1
O 01
l-l
0 ft
•H
4-1 II
CO
U 01
U
oi d
00 CO
CO M
l-l OI
01 i-l
> 0
< 4-1
II
>-*
00
s
s
ft
OI
3
01
U
U
• H
l-l
P
01
a
o
u
CO
II
_
P j
g2
•H
B
„
d
3
d
o
• H
p
l-l
Xl
•H
rH
10
O
4-1
O
OI
a
•H
n
CD
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 15 of 19
the thermometer should be adjusted and recalibrated until the
criteria are met, or it should be rejected.
4. Prior to each field trip compare the room temperature
with the meter thermometer and the mercury-in-glass thermometer.
If the readings are not within ±2°C (4°F), the meter thermometer
should be replaced or recalibrated.
2.2.2 Dry Gas Thermometers - The thermometers used to measure
the metered gas sample temperature should initially be compared
with a mercury-in-glass thermometer as above, using a similar
procedure.
1. Place the reference and the test thermometers in a hot
water bath maintained at 40° to 50°C (104° to 122°F). Compare
the readings after both stabilize.
2. Allow both thermometers to come to room temperature.
Compare readings after the thermometers stabilize.
3. Accept the test thermometer if its reading agrees
within 3°C (5.4°F) of the reference thermometer reading at both
temperatures. If not, either the thermometer should be adjusted
and recalibrated or a temperature correction factor should be
marked on the thermometer where it is readily visible to the
operator. When the factor is used, it must be noted on the pre-
test sampling check form (Figure 2.5) and in the calibration log.
4. Compare the temperatures prior to each field trip at
room temperature with the thermometer as part of the meter
svstem. If the readings or corrected values are not within ±6°C
(10.8°F) of the mercury-in-glass thermometer value, the meter
thermometer should be replaced or recalibrated.
2.3 Barometer
The field barometer should be adjusted initially and before
each test series to agree within ±2.5 mm (0.1 in.) Hg of the
mercury-in-glass barometer or with the pressure reported by a
nearby National Weather Service Station. Correction for eleva-
tion difference between the station and the sampling point should
be applied at a rate of -2.5 mm Hg/30 m (0.1 in. Hg/100 ft).
Record results on the pretest sampling check form (Figure 2.1).
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 16 of 19
Date (jtisM*****^ /A, /9$b Calibrated by
^/ ff T~
Meter box number r/fi-/ AH@
Dry Gas Meter*
Pretest calibration factor 0. J%(t (within 2% of the average
factor for each calibration run)
Impinger Thermometer
Was a pretest temperature correction used? _ yes ^ no
If yes, temperature correction (within 2°C (4°F) of
reference value)
Dry Gas Meter Thermometer
Was a pretest temperature correction made? _ yes v no
If yes, temperature correction (within 6°C (10.8°F) of
reference value)
Barometer
Was the pretest field barometer reading correct? I/ yes no
Stack Gas Temperature Sensor (if required)*
Was a temperature sensor required for moisture determination pur-
poses? yes \/ no
Was a pretest temperature correction used? yes is no
If yes, temperature correction -—— (within ±1°C over
the entire range)
Did the temperature sensor agree with the reference thermometer
(within ±1°C (2°F) over the range of 10° to 82°C (50° to
180°F))? _\..:s'_j^z no
*Most significant items/parameters to be checked.
Figure 2.5 Pretest sampling checks.
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 17 of 19
2.4 Trip Balance
The trip balance should be calibrated initially by using
Class-S standard weights and should be within ±0.5 g of the
standard weight. Adjust or return the balance to the manufac-
turer if limits are not met.
2.5 Stack Gas Temperature Sensor
The stack gas temperature must be accurately determined when
the stack is suspected of being saturated or having water drop-
lets. Therefore proper calibration of the stack gas temperature
sensor is important for this method. Upon receipt, the sensor
should be calibrated over the entire range. An ASTM E-l No. 3C
or 3F thermometer should be used as the reference temperature.
The initial and, as required, recalibration procedure is as
follows:
1. Place both the temperature sensor and the reference
thermometer in water or in a controlled-temperature atmosphere.
2. Record both temperatures after each has stabilized for
30 s. Increase the temperature in increments of about 6°C
(10°F), taking readings over the entire range (10-82°C (50-
180°F)).
3. Both values should agree within ±1°C (2°F). If not,
the temperature sensor should be adjusted if possible. However,
if the values are off by a constant factor over the entire range,
a correction factor may be used.
After each field use, the temperature sensor calibration
should be checked. The procedure for the check is as follows:
1. Check the temperature sensor with the reference ther-
mometer at a temperature within ±5°C (10°F) of the average stack
temperature. If the values agree within ±2°C (4°F), then the
pretest calibration is acceptable.
2. When the above agreement is not met, the temperature
sensor should be recalibrated at a temperature within ±2°C (4°F)
of the average stack temperature, and a correction factor should
be determined with the reference thermometer. The difference
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 18 of 19
between the temperature sensor and the reference thermometer
should be used to correct the average stack temperature for cal-
culation purposes. Also, a complete recalibration of the temper-
ature sensor is suggested.
-------
Section No. 3.3.2
Revision No. 0
Date January 15, 1980
Page 19 of 19
Table 2.1 ACTIVITY MATRIX FOR EQUIPMENT CALIBRATION
REQUIREMENTS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Wet test meter
Capacity of at least
3.4 rn /h (120 ftj/h)
and accuracy within
±1%
Calibrate initially
and then yearly by
the liquid displace-
ment technique; see
Subsec 2.1.1
Adjust until
specifications
are met, or re-
turn to manu-
facturer
Dry gas meter
Y. = Y ±0.02Y at a flow
rate of 0.02-0.033
m /min (0.66-1 ft /min)
Calibrate vs. wet
test meter initially
to agree, and when
the posttest check is
not within Y ±0.05Y
Repair or re-
place, and then
recalibrate
Thermometers
Impinger thermometer
±1°C (2°F); dry gas
meter thermometer
±3°C (5.4°F) over
range
Calibrate each ini-
tially as a separate
component against a
mercury-in-glass
thermometer; before
each field trip,
compare each as part
of the train with
the mercury-in-glass
thermometer
Adjust, deter-
mine a constant
correction fac-
tor, or reject
Barometer
±2.5 mm (0.1 in.) Hg
of the mercury-in-glass
barometer
Calibrate initially
using mercury-in-
glass barometer;
check before and after
each field test
Adjust to agree
with certified
barometer
Stack gas
temperature
sensor for
moisture de-
termination
Pretest calibration
±1°C (2°F) over range;
posttest check ±2°C
(4°F)
Calibrate initially
over the range with
an ASTM reference
thermometer; after
each field test, make
a single-point cali-
bration check
Adjust to
agree with re-
ference ther-
mometer; use a
constant cor-
rection factor,
or reject;
posttest data
corrected for
calculation
purposes
-------
Section No. 3.3.3
Revision No. 0
Date January 15, 1980
Page 1 of 7
3.0 PRESAMPLING OPERATIONS
The quality assurance activities for presampling operations
are summarized in Table 3.1 at the end of this section. See
Section 3.0, the introduction to this Handbook, for details on
preliminary site visits.
3.1 Apparatus Check and Calibration
A pretest check will have to be made on most of the sampling
apparatus. Figure 3.1 should be used as a pretest operations and
packing list. An inquiry must be made as to whether the stack
gas is saturated or has water droplets.
3.1.1 Sampling Train - The specifications of the Method 4 sam-
pling train used by the EPA are given in Figure 1.1. Commercial
models of this system are available. Each individual or fabri-
cated train must be in compliance with the specifications of the
Reference Method, Section 3.3.10.
3.1.2 Probe - Clean the probe internally by brushing first with
tap water, then with deionized distilled water, and finally with
acetone; allow it to dry in the air. In extreme cases, the probe
liner can be cleaned with stronger reagents. In either case, the
objective is to leave the probe liner free from contaminants.
The probe's heating system should be checked to see that it is
operating properly. The probe should be sealed at the inlet or
tip and checked for leaks at a vacuum of 380 mm (15 in.) Hg, and
the probe must be leak free under these conditions.
3.1.3 Impinger and Glass Connections - All glassware should be
cleaned first with detergent and thoroughly rinsed with tap water
and then with deionized distilled water. All glassware should be
visually inspected for cracks or breakage and then repaired or
discarded if defective.
3.1.4 Pump - The vacuum pump should be serviced as recommended
by the manufacturer, or every 3 mo, or upon erratic behavior
(nonuniform or insufficient pumping action). Check oiler jars,
if used, every 10 tests.
-------
Section No. 3.3.3
Revision No. 0
Date January 15, 1980
Page 2 of 7
Apparatus check
Probe type
Borosilicate s
glass v/
Quartz
glass
Other
Heater and leak
r:hf»rked* •><
Filter
In-stack ^/
Out-stack ^
Glass wool
Other
Condenser
Impingers yX^
Other
Cooling System
Ice bath ^/
Other
Metering System
Vacuum gauge iX
Checked* \^
Pump \^"
Leak .
checked* __\^_
Thermometers S
Calibrated* ^
Dry gas /
meter vX
Calibrated* J^"
Other
Acceptable
Yes
v/
v/
S
S
S
•/
^
v/
No
Quantity
required
3
I Box
5- OS
ID HOji
-7
O
^5
^}
3
(.Q-JOtft)
<=3
Ready
Yes
/
vX
v^
/x
^
y
No
Packed and
loaded
Yes
vX
v/
^
y
^
/
s
y
No
*Most significant items/parameters to be checked.
Figure 3.1 Pretest preparation checklist, (continued)
-------
Section No. 3.3.3
Revision No. 0
Date January 15, 1980
Page 3 of 7
Figure 3.1 (continued)
Apparatus check
Barometer
Mercury ,/
Aneroid
Other
Calibrated* S
Quantitative
Instrument
Graduated
cylinder ,x
Trip
balance ,/
Calibrated* yt5_
Stack Temperature
Sensor*
Type ff&jfMpMjpLL.
Calibrated yzs
Acceptable
Yes
-
IX
IX
-
NO
Quantity
required
'
Z-
2-
Ready
Yes
-
-
-
No
Packed and
loaded
Yes
^
"
~-
No
*Most significant items/parameters to be checked.
-------
Section No. 3.3.3
Revision No. 0
Date January 15, 1980
Page 4 of 7
3.1.5 Dry Gas Meter - A dry gas meter calibration check should
be made using the procedure in Section 3.3.2.
3.1.6 Silica Gel - Either dry the used silica gel at 175°C
(350°F) or use fresh silica gel and weigh several 200- to 300-g
portions in airtight containers to the nearest 0.5 g. Record the
total weight (silica gel plus container) on each container.
3.1.7 Thermometers - The thermometers should be compared to the
mercury -in -glass reference thermometer at ambient temperature
(Subsection 2.2.1 of Section 3.3.2).
3.1.8 Barometer - The field barometer should be compared with
the mercury -in -glass barometer or the weather station reading
prior to each field trip (Section 3.3.2).
3.1.9 Stack Gas Temperature Sensor - A specially calibrated
temperature sensor is required if the stack gas is saturated or
has water droplets present. The sensor should be calibrated
against a reference thermometer (Section 3.3.2).
3.1.10 Water - It is recommended, but not required, that 100 ml
of deionized distilled water conforming to ASTM D1193-74 type 3
be used in each of the first two impingers.
3.2 Equipment Packing
The accessibility, condition, and functioning of measurement
devices in the field depend on careful packing and on the care of
movement on site. Equipment should be packed to withstand severe
treatment during shipping and field handling operations. One
major consideration in shipping cases is the construction
materials. The following containers are suggested, but are not
mandatory.
3.2.1 Probe - Seal the inlet and outlet of the probe and then
wrap with polyethylene or other suitable material to protect the
probe from breakage. An ideal container is a wooden case (or
equivalent) lined with foam material and with separate compart-
ments to hold individual probes. The case should have handles or
eye-hooks that can withstand hoisting and that will be rigid
enough to prevent bending or twisting during shipping and han-
dling.
-------
Section No. 3.3.3
Revision No. 0
Date January 15, 1980
Page 5 of 7
3.2.2 Impingers, Connectors, and Assorted Glassware - All im-
pingers and glassware should be packed in rigid containers and
protected by polyethylene packing material or other suitable
material. Individual compartments for glassware will help to
organize and protect each piece and simplify inventorying.
3.2.3 Volumetric Glassware - A sturdy case lined with foam
material can contain drying tubes and assorted volumetric glass-
ware.
3.2.4 Meter Box - The meter box—which contains the manometers,
orifice meter, vacuum gauge, pump, dry gas meter, and thermom-
eters—should be packed in a shipping container unless its
housing is sufficient to protect components during travel.
Pump oil sump and oiler jars should be drained to prevent fouling
of the components during shipment. Additional pump oil should be
packed if oil is required. It is advisable to carry a spare
meter box in case of failure.
3.2.5 Wash Bottles and Storage Containers - Storage containers
and miscellaneous glassware should be packed in a rigid foam-
lined container.
-------
Section No. 3.3.3
Revision No. 0
Date January 15, 1980
Page 6 of 7
Table 3.1 ACTIVITY MATRIX FOR PRESAMPLING PREPARATIONS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Probe
1. Probe liner free of
contaminants and con-
structed of borosili-
cate glass, quartz, or
equivalent; metal
liners must be approved
by administrator
2. Probe leak free
at 380 mm (15 in.) Hg
3. Probe that prevents
moisture condensation
1. Clean probe in-
ternally by brushing
using tap water, then
deionized distilled
water, and finally
acetone; air dry
before test
2. Visually check be-
fore test
3. Check heating
system initially and
when moisture cannot
be prevented during
testing
1. Repeat
cleaning pro-
cedure, and
reassemble
2. Replace
3. Repair or
replace
Impingers,
filter
holders, and
glass con-
tainers
Clean and free of
breaks, cracks, leaks,
etc.
Clean with detergent
and tap water, then
deionized distilled
water
Repair or
discard
Pump
Sampling rate of about
O.Q2-.03 m /min (0.66-1
ft /min) up to 380 mm
(15 in.) Hg vacuum at
pump inlet
Service every 3 mo
or upon erratic be-
havior; check oiler
jars every 10 tests
Repair or re-
turn to manu-
facturer
Dry gas meter
Readings within ±2%
average calibration
factor; clean
Calibrate according
to Sec 3.3.2
check for excess oil
As above
Thermometers
Readings within ±2°C
(4°F) of mercury-in-
glass thermometer
Compare with mercury-
in-glass thermometer
at room temperature
prior to each field
test
Replace or re-
calibrate
Barometer
Readings within 2.5 mm
(0.1 in.) Hg
Compare with mercury-
in-glass barometer
or value reported by
nearby National Wea-
ther Station corrected
for elevation prior to
each field test
As above
(continued)
-------
Section No. 3.3.3
Revision No. 0
Date January 15, 1980
Page 7 of 7
Table 3.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Stack gas
temperature
sensor for
moisture
determination
*1°C (2°F) over range
of 10 to 80°C (50° to
Compare against ASTM
reference thermometer
As above
180°F)
Water
Deionized distilled;
ASTM-D1193-74 type 3
Run blank evapora-
tions prior to field
use to eliminate high
solids (only required
if impinger contents
to be analyzed)
Redistill or
replace
Silica gel
Indicating type, size
6 to 16 mesh; dry
used gel at 175°C
(350°F) for at least
2 h; weigh 200 g por-
tion to nearest 0.5 g;
record the weight
Prior to each field
test, observe drying
time if appropriate;
check weighings
Repeat proce-
dure
Package Equip-
ment for
Shipment
Probe
Packed in rigid con-
tainer and protected
by polyethylene foam
Prior to each ship-
ment, check packing
of equipment
Repack
Impingers, con-
tainers, and
assorted
glassware
Packed in rigid con-
tainer and protected
by polyethylene foam
As above
As above
Meter box
Meter box case and/or
additional material to
protect train compon-
ents; pack spare meter
box
As above
As above
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 1 of 10
4.0 ON-SITE MEASUREMENTS
The on-site activities include transporting the equipment to
the test site, unpacking and assembling the equipment, making
duct measurements, determining whether the stack gas is saturated
or has water droplets, charging the impingers, obtaining a sam-
ple, and recording data. Table 4.1 at the end of this section
summarizes the on-site quality assurance activities and Figure
4.1 is an on-site measurement checklist. Blank data forms are in
Section 3.3.12 for the convenience of the Handbook user.
4.1 Handling Equipment
The most efficient means of transporting or moving the
equipment from ground level to the sampling site should be
decided during the preliminary site visit or through prior cor-
respondence to minimize damage to the test equipment or injury to
test personnel. A "laboratory" area should be designated for
assembling the sampling train, placing the filter in the filter
holder, charging the impingers, recovering the sample, and docu-
menting the results; this area should be clean and should be free
of excessive drafts.
4.2 Sampling
The on-site sampling includes addition of the water and
silica gel to the impingers; setup of the sampling train; con-
nection to the electrical service; preparation of the probe (leak
check of entire sampling train and addition of particulate fil-
ter); insertion of the probe into stack; sealing of the port;
check of the probe temperature; and sampling and recording the
data (Figure 4.2). A final leak check of the train is mandatory
after sampling. l
4.2.1 Preliminary Measurements and Setup - The sampling site
should be selected in accordance with Method 1. If this is
impossible due to duct configuration or other reasons, the
site should be approved by the administrator. A 115 V, 30-A
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 2 of 10
Procedure used; Reference \s Approximate
Reference Method
Conducted simultaneously with pollutant emission test?
Impingers properly placed?*
Impinger content: 1st
4th 20fa $i'Jt£4ty£l Modifications
Cooling System: Crushed ice i/ Other
Sampling time per point «5XT?//I/
Probe heater (if applicable) on? ^4*^ Temp £5*0*?
Crushed ice in ice bath?
Leak check? (optional) _ ^^^ _ Leakage rate 0. O
Sampling rate constant (within 10%)?*
All data properly recorded?*
Posttest leak check?* (mandatory)
Leakage rate* _ Q. Q
Analysis - Impinger Content
Method: Volumetric iS Gravimetric
Measurement of volume of water condensed:
Graduated cylinder _ cds _ Other
Measurement of silica gel: Balance _ iX" Other
Color of silica gel? j@r£^\o^ _ Condition
All analytical data properly recorded?
*Most significant items/parameters to be checked.
Figure 4.1 On-site measurement checklist
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 3 of 10
60 4-1
cQ 00 00
U -H
•rl 41
r-l *
CO
41 41
•H r-l
M
i
^
^
1
y,
P
a
i
i
IL
0
•
V
X,
r
J>
^
T—l
CO
d
•H
PM
-^«
•f-
•4
VJ
41 M
,£> OJ
r-l B £>
•rl d 3
i-i a
^
Q
V]
%
^
^^
^
c
0
^
1-1
CO
•H
+J
•H
d
r-l
c
§^
\c
••^ Aj
U
CO 41
41 .a
41 r-l S
P CO 60 d
^^-^ M 0
•H i-l
V X • • M H 41
4-iox
tO ^ o ffl *0 4) 'O 4)
S ,0 < CJ r-l B
41 B O
01 i-l h I-l t-4 i— 138
JQ pi 4) 4) 4) CO 3 I-l
OS4-l4-J4-ldU41
j-iajujcjaj-Hiflpd
PLiCOSSSPH^E"!
It
d
!*.
i
1^
0
1
<3
r/-j
JJ
•o
C
t.
Q
.*-
2
f
c£
*
,2
i
5-
r-
•^J
•— «•
(C
.3 rl
0 0
•H 4-1
!
C
>
1
fX
fr-
CT
™
•^
-IK!
^"\
-P r-l
3 d dj
4-) 4J flj d 41 S 41
d <0 ^1 41 -H O ,£
cOU4!4->d^ll-lO
i-HOftcOSScO^
CM i-J O O ff! < P3 Oi
41 O
M
3 60 I-l
4-> to d 4)
(0 CO -rl M
M 60 > d
41 co 41
ft^-l 4) t3
S 0 r-< d
41 O
H U
M CO
60
i— 1 I-l
CO 41
(U -H 4->
M 4-> W 0)
3 d w B
tfl 41 O
tfl I-l U 41
41 41 U U
M <4-l CO -H
O-l M-l M-l
•H -i-l
13 14
0
r4 M
U 4>
CO 41
4-1
60
•H
r— 1
1
CO
CO
41
(fl
S-l
41
CO
I-l
H
41
60
Q /l~^
0)0^
4J 0\
ta
co
iH
Q
4-IXJ
41 OX
^H /" *N
4-1 4-1
3 3
° S°
H_
^^
o
s^. /
4J-0
41 O\
1— 1 /— v
d d
M 'H
B
H
CO
4-1
= %
/ — \
(O
^
o
CN
«W
i7
>— ' -H
^^
v
g
i
*• /^S
OJ pq
M O
« "(U
0\
CD"
•H
a e
•H
4-1
^
4-1 41
d r?
•H S
O 3
1
1
1
1
1
s
is
h
i
i
i
/)
i
**.
rc
r
*
-.
%^j
V i
0
ro
ro
V-
o
C)Q
f\^
"^
s
-o
.-*"
.jj
^
rr
^J*
'0
rO
'0
*^x
s
^
r
^
fe
60
or
'd
cC
3
^
^
>
"^Ji
^
|
»(
Q
*v
^
CT
r-
<)c
r
cr
n
^ol
^
0
IX)
•o
5
s
™" *
•§
0
^s
^-
^
on
Xj
CJ
n
"
5
o
"**
c
V
o
oc
^
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 4 of 10
electrical supply is necessary to operate the standard sampling
train. A minimum of eight traverse points should be used for
rectangular stacks having equivalent diameters <0.61 m (<24 in.),
and a minimum of 12 should be used for all other stacks unless
otherwise specified by the administrator. Record all data on the
traverse point location form shown in Section 3.0 (introduction
to this volume). These measurements will be used to locate the
sampling probe during preliminary measurements and actual sam-
pling.
Select a suitable probe liner and probe length so that all
traverse points can be sampled. For large stacks, consider
sampling from opposite sides of the stack to reduce the length of
the probe.
Select a total sampling time so that a minimum gas volume of
0.60 sm3 (21 sft3) can be collected at a constant rate of £0.021
3 3
m /min (0.75 ft /m). The rate can be limited by selecting a
pressure drop (AH) which is
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 5 of 10
B = S'p'?' Equation 4-1
ws Fstatic
*bar 13.6
where
B = water vapor in the gas stream, proportion by
WS
volume
S.V.P. = saturated vapor pressure of water at average
stack temperature, mm (in.) Hg
P, = barometric pressure, mm (in.) Hg, and
P . . . = static pressure of the stack, mm (in.) H,O.
SL-cl"ClC ^
If the psychrometric chart or the saturation vapor pressure
tables are not applicable (based on evaluation of the process),
alternate methods approved by the administrator should be used.
The stack gas can be checked for saturation with wet and dry
bulb thermometers. When the stack is saturated, the wet and dry
bulb temperatures are the same. This will not, however, check
for the presence of water droplets.
4.2.2 Condenser Preparation - Place known volumes of water in
the first and second impingers; generally, 100 ml in each im-
pinger is adequate. Immerse the tips of the impinger tubes at
least 13.0 mm (0.5 in.) in the water. The third impinger should
be left dry to trap any entrained water droplets. Place a known
amount of silica gel in the fourth impinger; generally, 200 g is
sufficient. Record the amount of water and silica gel placed in
the impingers. If the stack temperature is high >400°C (752°F),
a lower sampling rate may be necessary to maintain the tempera-
ture leaving the fourth impinger at <20°C (£68°F).
Alternatively, each impinger and its contents can be weighed
to the nearest 0.5 g. Record these weights on the analytical
data form (Figure 4.3) for determining the amount of water con-
densed.
4.2.3 Sampling Train Assembly - Assemble the sampling train as
shown in Figure 1.1, and perform the following:
1. Adjust the probe heater to operating temperature, and
place crushed ice and water around the impingers.
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 6 of 10
Plant
Date
'-•??
Run number
Final
Initial
Liquid collected
Total volume collected
Volume of liquid
water collected
Impinger
volume ,
ml
z-?/
^oo
-?/
Silica gel
weight,
g
^/570
^3.5-
//,5~
g* £2,5^1
* Convert weight of water to volume by dividing total weight
increase by density of water (1 g/ml):
increase g = water vol x
1 g/ml
Figure 4.3 Method 4 analytical data form.
2. Leak check the sampling train just prior to use by
disconnecting the probe from the first impinger or (if appli-
cable, from the filter holder); plug the inlet to the first
impinger (or filter holder); and pull a 380 mm (15 in.) Hg
vacuum. If the leakage rate is >4% of the average sampling rate
or if it is >_0. 00057 m /min (0.02 ft /m), whichever is less, it
is unacceptable. This leak check is recommended but not manda-
tory.
3. Place a loosely packed filter of glass wool in the end
of the probe if an external heated filter is not used, and con-
nect the probe to the sampling train.
4. Attach a stack temperature sensor on the probe when
required.
4.2.4 Sampling Train Operation (Constant Rate) - Sampling is
2
performed at a constant rate of approximately 0.02 m /min (0.75
3
ft /m) or less during the entire period as follows:
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 7 of 10
1. Record the initial dry gas meter readings, barometric
pressures, and other data as indicated in Figure 4.2.
2. Position the tip of the probe at the first sampling
point, and turn on the pump.
3. Adjust the sample flow to the predetermined constant
rate of 0.021 m3/min (0.75 ft3/m) or less.
4. Take other readings required by Figure 4.2 at least
once at each sample point during each time increment.
5. Record the dry gas meter readings at the end of each
time increment.
6. Record the stack gas temperature at each point when the
stack gas is saturated or has water droplets.
7. The static pressure of the stack must also be deter-
mined when the moisture content is to be calculated using the
partial pressure method.
8. Repeat steps 3 through 5 for each sampling point.
9. Turn off the pump, remove probe from the stack, and
record the final readings after each traverse.
10. Leak check (as described in Subsection 4.2.3) after the
last traverse, and record all leakage rates. This leak check is
mandatory.
11. Cap the impingers with serum caps (or equivalent) and
transport to the sample cleanup area if the train passes the leak
check. If it does not, either reject the test results or correct
the sample volume (see Section 3.4.6).
12. Check the sampling rate and the sample volume (AVm) for
each point. The volume for each point should be within ±10% of
the average sample volume for all points. If all are within the
limit, then the sample run is acceptable; otherwise, reject the
results and either repeat the test run or consult the administra-
tor.
4.3 Sample Recovery
Measure the volume of the condensed moisture to the nearest
1 ml. Determine the increase in weight of the silica gel (or gel
plus impinger) to the nearest 0.5 g. Record these data on the
data form shown in Figure 4.3 or on a similar form.
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 8 of 10
4.4 Sample Logistics, Data Collection, and Equipment Packing
Follow the above procedures until the required number of
runs are completed. At the completion of the test:
1. Be sure that all data recorded during the field test
are duplicated by using carbon paper or by using data forms and a
laboratory notebook. Mail one set of data to the base labora-
tory, or give it to another team member or the agency, and have
the other handcarried.
2. Examine all sampling equipment for damage and for
proper packing for shipment. Label all shipping containers
properly to prevent sample or equipment loss.
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 9 of 10
Table 4.1 ACTIVITY MATRIX FOR ON-SITE MEASUREMENT CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Condenser,
addition of
water and
silica gel
to system
100 ml of distilled
water in first two
impingers; approximate-
ly 200 g of silica gel
in fourth impinger
Either use graduated
cylinder to measure
water or weigh each
impinger and its con-
tents to nearest 0.5 g
Correct the
additions
Assembling
sampling
train
1. Assembled to speci-
fications in Fig 1.1
2. Leak rate <4% or
0.^0057 m /min (0.02
ft /min), whichever is
less
1. Assemble before
each sample run
2. Leak check before
sampling by plugging
the nozzle or inlet
to first impinger and
pulling a vacuum of
380 mm (15 in.) Hg
1. Reassemble
2. Correct
leak
Sampling
1. Sampling volume for
each point within ±10%
of average sample volume
for all points
2. Minimum total sam-
ple gas volume of 0.60
sm (21 sft ) at a con-
stant sampling rate
<0.021 in /min (0.75 ft /
min)
3. Minimum number and
location of points
specified by Method 1
1. Calculate for
each test run
2. Make a quick cal-
culation before test-
ing; do an exact cal-
culation after tra-
verse
3. Check before the
first test run by mea-
suring duct and using
Method 1
1. Repeat test
run
2. As above
3. Repeat the
procedure to
comply with
specifications
of Method 1
(continued)
-------
Section No. 3.3.4
Revision No. 0
Date January 15, 1980
Page 10 of 10
Table 4.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Samp1ing (cont.)
4. Leakage rate <4%
of the average sampling
volume or <0.00057 m3/
min (0.02 fts/min),
whichever is less
4. Leak check after
each test run or be-
fore equipment re-
placement during test
at the maximum vacuum
during the test (man-
datory)
4. Correct the
sample volume, or
repeat the sample
run
Sample recovery
Volume of moisture
condensed to nearest
1 ml; weight increase
of silica gel to
nearest 0.5 g
Use volumetric/
gravimetric measure-
ment
Repeat the
measurement
Sample logis-
tics, data
collection,
and packing
of equipment
1. All data recorded
correctly
2. All equipment exam-
ined for damage and
labeled for shipment
3. All sample contain-
ers and blanks properly
labeled and packaged
1. After completion
of each test and be-
fore packing
2. As above
1. Complete
the data
3. Visually check
upon completion of
each sample
2. Repeat the
sampling if
damage occurred
during test
3. Correct when
possible
-------
Section No. 3.3.5
Revision No. 0
Date January 15, 1980
Page 1 of 4
5.0 POSTSAMPLING OPERATIONS
Table 5.1 at the end of this section summarizes the quality
assurance activities for postsampling operations.
Posttest checks will have to be made on most of the sampling
apparatus. The checks will include three calibration runs at a
single orifice meter setting; cleaning; and/or routine main-
tenance. The cleaning and maintenance are discussed in
2
APTD-0576 . Figure 5.1 should be used to record the posttest
checks.
5.1.1 Metering System - The metering system has two components
that must be checked—the dry gas meter and the dry gas meter
thermometer(s).
The dry gas meter thermometer(s) should be compared with the
ASTM mercury-in-glass thermometer at room temperature. If the
two readings agree within 6°C (10.8°F), they are acceptable; if
not, the thermometer must be recalibrated according to Section
3.3.2 after the posttest check of the dry gas meter. For calcu-
lations, use the dry gas meter thermometer readings (field or
recalibration values) that would give the higher temperatures—
that is, if the field readings are higher, no correction is
necessary, but if the recalibration value is higher, add the
difference in the two readings to the average dry gas meter
temperature reading.
The dry gas meter must be posttested (Section 3.3.2). The
metering system should not have any of the leaks that were cor-
rected prior to the posttest check. If the dry gas meter cali-
bration factor (Y) does not deviate by >5% from the initial
calibration factor, the dry gas meter volumes obtained during the
test series are acceptable. If Y deviates by >5%, recalibrate
the metering system (Section 3.3.2).
-------
Section No. 3.3.5
Revision No. 0
Date January 15, 1980
Page 2 of 4
Date ; / , ^ ,- £(\ Calibrated by
1 '
Meter box number -~ A-
Dry Gas Meter
Pretest calibration factor Y Q. 7%(^ (must be within ±2%)*
Posttest checks, Y, /-, c; cvV Y9 (must be within ±5% of
pretest) ~^' * z
Recalibration required? yes \^ no
If yes, recalibration factor Y (must be within ±2%)*
Lower calibration factor, Y c. ^9-G~- f°r calculations (pretest
or posttest)*
Dry Gas Thermometer
Was a pretest meter temperature correcton used? _____ Yes ^ n°
If yes, temperature correction (within ±3°C (5.4°F)
over range)*
Post test comparison with mercury-in-glass thermometer (r, jt.
_ (within +6°C (10.8°F) at room temperature)
Recalibration required? | ^ yes \^ no
Recalibration temperature correction, if used —-- (within
±3°C (5.4°F) over range)*
If yes; no correction is necessary for calculations when meter
thermometer temperature is higher.
If recalibration temperature is higher, add correction to average
meter temperature for calculations
Barometer
Was pretest field barometer reading correct ^ yes ______ n°
Posttest comparison __^ mm (in.) Hg +2.5 mm (0.1 in.) Hg
Was recalibration required? yes ^ no
If yes; no correction is necessary for calculations when the
field barometer has the lower reading
If the mercury-in-glass reading is lower, then subtract the dif-
ference from the field data readings for the calculation
Stack Gas Temperature Sensor (if required)
Average stack temperature /.3j" °C (>F)
Posttest comparison / ^^-° [within ±2°C (4°F)]*
Was recalibration required? yes ^ no
*Most significant items/parameters to be checked.
Figure 5.1 Posttest equipment checks.
-------
Section No. 3.3.5
Revision No. 0
Date January 15, 1980
Page 3 of 4
For the calculations, use the calibration factor (initial or
recalibration) that yields the lower gas volume for each test
run.
5.1.2 Barometer - The field barometer should be compared to the
mercury-in-glass barometer. If the readings agree within ±5 mm
(0.2 in.) Hg, the field readings are acceptable; if not, use the
lesser calibration value for the calculations. If the field
barometer reads lower than the mercury-in-glass barometer, the
field data are acceptable. If the mercury-in-glass barometer
gives the lower reading, use the difference in the two readings
(the adjusted barometric value) in the calculations.
5.1.3 Stack Gas Temperature Sensor - The stack gas temperature
sensor should be compared with an ASTM mercury-in-glass refer-
ence thermometer. Place both the stack sensor and reference
thermometer in an atmosphere (air or water) that is within ±5°C
(10°F) of the average stack temperature. If both values agree
within ±2°C (4°F) then the pretest calibration is acceptable.
If not, then calculate the moisture content using both the pre-
test calibration and the posttest corrected values. If either or
both calculated values are greater than the measured moisture,
then either or both may be eliminated from any final emissions
calculations.
-------
Section No. 3.3.5
Revision No. 0
Date January 15, 1980
Page 4 of 4
Table 5.1 ACTIVITY MATRIX FOR POSTTEST OPERATIONS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Dry gas meter
Within ±5% of the ini-
tial calibration fac-
tor
Make three runs at a
single, intermediate
orifice setting and
at highest vacuum
occurring during
test (Sec 3.3.2)
Recalibrate;
use calibration
factor that
gives lesser
sample volume
Dry gas meter
thermometer
Within ±6°C (10.8°F)
at room temperature
Compare with ASTM
mercury-in-glass
thermometer after
each field test
Recalibrate;
use higher
temperature
for calcula-
tions
Barometer
Within ±5 mm (0.2 in.)
Hg at ambient pressure
Compare with mercury-
in-glass barometer
after each field
test
Recalibrate;
use lower
barometric
values for
calculations
Stack tempera-
ture sensor
Within ±2°C (4°F) of
the reference check
temperature
After each run, com-
pare with reference
temperature
Recalibrate;
perform calcu-
lations with
and without
temperature
correction
-------
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 1 of 8
6.0 CALCULATIONS
Calculation errors due to mathematical mistakes can be a
large part of total system error. Therefore, each set of calcu-
lations should be repeated or spot-checked by a team member other
than the one who performed them originally. If a difference
greater than a typical roundoff error is detected, the calcula-
tions should be checked step by step until the source of error is
found and corrected. A computer program can be advantageous in
reducing calculation errors. If a standardized computer program
is used, the original data entry should be checked; if differ-
ences are observed, a new computer run should be made. Table 6.2
at the end of this section summarizes the quality assurance
activities for calculations.
Carryout calculations, retaining at least one significant
digit beyond that of the acquired data. Roundoff after final
calculations to two significant digits for each run or sample in
accordance with the ASTM 380-76 procedures. Record the results
on Figure 6.1A, 6.IB, or 6.1C.
6.1 Nomenclature
The terms defined and listed alphabetically herein are to be
used in calculating dry gas and water vapor volumes and moisture
contents, and in verifying constant sampling rate.
B = Water vapor in the gas stream, proportion by volume
W o
AH = Average pressure differential across the orifice
meter, mm (in.) H^O
AH@. = Measurement of pressure differential across the
1 orifice meter, mm (in.) H2O
L = Maximum acceptable leakage rate for either a pretest
a leak check or a leak check,, following a component
change; equal to 0.00057 m /min (0.01995 ft /min)
M = Molecular weight of water, 18.0 g/g-mole
w (18.0 Ib/lb-mole)
-------
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 2 of 8
p
bar = Barometric pressure, mm (in.) Hg
P = Absolute pressure at the dry gas meter (for this
method, same as barometric pressure), mm (in.) Hg
P = Absolute stack pressure, mm (in.) Hg
Astatic = static pressure of the stack, mm (in. ) H~0
Pstd = standard absolute pressure, 760 mm (29.92 in.) Hg
Pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml)
R = Ideal gas constant, 0.06236 (mm Hg) (m3V(g-mole) (K)
for metric units and 21.85 (in. Hg) (ft )/(lb-mole)
(°R) for English units
S.V.P. = Saturated vapor pressure of water at average stack
temperature, mm (in.) Hg
T = Absolute average dry gas meter temperature, K (°R)
Tstd = standard absolute temperature, 298K (528°R)
V-r = Final volume of condenser water, ml
V- = Initial volume of condenser water, ml
V = Volume of gas sample measured by dry gas meter, dcm
m (dcf)
AV = Incremental volume-measured by dry gas meter at each
traverse point, dm (dcf)
V x . ,. = Volume of gas sample measured by the dry gas meter,
* ' corrected to standard conditions, dsm (dscf)
v = Stack gas velocity, calculated by Method 2, using
data from Method 5, m/s (ft/s)
Vwc(std) = Volume of condensed water vapor, corrected to
* standard conditions, sm (scf)
V fstdl = Volume of water vapor collected in silica gel,
"^ ' corrected to standard conditions, sm (scf)
Wf = Final weight of silica gel or silica gel plus
impinger, g
W- = Initial weight of silica gel or silica gel plus
impinger, g
Y = Dry gas meter calibration factor
-------
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 3 of 8
6.2 Condensed Water Vapor Volume
V
wc(std>
where
•3
K, = 0.001333 m /ml for metric units, or
= 0.04707 ft3 /ml for English units.
6.3 Water Vapor Volume Collected in Silica Gel
(Wf - W.) RT d
wsg(std)
Mw
= VWf - V
where
Cation 6-
K2 = 0.001335 m/g for metric units, or
= 0.04715 ft3/g for English units.
6.4 Dry Gas Volume, Corrected to Standard Conditions
Correct the sample volume measured by the dry gas meter to
standard conditions (20°C and 760 mm Hg or 68°F and 29.92 in. Hg)
by using Equation 6-3 .
T P
std m
K V Y P
3mm
where
K3 = 0.3858 K/mm Hg for metric units, or
= 17.64 °R/in. Hg for English units.
Note; If the leak rate observed during any mandatory leak checks
exceeds the specified acceptable rate (L ), either the value of
a
V in Equation 6-3 may be corrected (as described in Section
3.4.6 of Method 5) or the test run may be invalidated.
-------
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 4 of 8
VOLUME OF WATER VAPOR CONDENSED IN IMPINGERS
Vf = ..2 2 / • ml/ vi = a? jo o • ml
Vwc(std) = °-04707
V Y P
Vm(std) = 17-64 -^ = -? Q. • ± 'L 4. ft3 Equation 6-3
MOISTURE CONTENT
Vwc(std) = ^ * • -* X A ft3, V = ^ . ^^ ^ ft3,
Vm(std) =^^ • V^
Bws = ^ Vwc(std) + Vwsq(std) =*. JL* Equation 6-4
wc(std) wsg(std) m(std)
Figure 6.1A Moisture content calculation form (English units).
-------
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 5 of 8
VOLUME OF WATER VAPOR CONDENSED IN IMPINGERS
vf = <*. "L L • m1/ vi = JL Q. o • ml
V . .,. = 0.001333 (V^ -V.) = o . o 2_ £ &. m3 Equation 6-1
W dr ^ ID L>U. j J_ _L
VOLUME OF WATER VAPOR COLLECTED IN SILICA GEL
wf = ,2 / s • 0 g, w. = j. o 3, . s g
J_ — — — — J_ — —
Vwsg(std) = °-001335 (wf * V = ° • ° -L £ 2 m3 Equation 6-2
SAMPLE VOLUME
1?J j^ m3, Tm = J 9 _9 . o °K, Pm = 7. 3 6 - 6 mm Hg
Y = . O
V Y P .,
v™/ +*\ = 0.3858 -JS= = vwsg(std) = e. - i J- * * m'
Vm(std) = 2 - I 2 ± ± ™3
w, - v - Mstd) + Vwsg(std) - = Equation 6-4
ws V / j_j\ + V /j.j\+V,.jX — — — t- ^•
wc(std) wsg(std) m(std)
Figure 6.IB. Moisture content calculation form (metric units).
-------
MOISTURE CONTENT
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 6 of 8
avg =
bar
= ^ i • £ 0 in. Hg, ^J 4 . £ mm Hg
in. H20, -_ 3 . £ /_ mm H20
static = - I
S.V.P. = J . ^ Q in. Hg, ,2 . Q mm Hg
r
*bar
13.6
Figure 6. 1C Moisture content calculation form using saturation
vapor pressure (English and metric units).
6 . 5 Moisture Content
V
wc(std)
V
wsg(std
ws - -
ws vwc(std) wsg(std) m(std)
Note: In moisture saturated or droplet-laden gas streams, two
calculations of the moisture content of the stack gas should be
made — one using a value based on the saturated conditions (Equa-
tion 6-5) and another using the results of the impinger
analysis. The lower of these two B values should be considered
WS
correct.
To determine the moisture content in moisture saturated or
droplet-laden gas streams, attach a temperature sensor capable of
measuring ±1°C (2°F) to the probe; measure the stack gas tempera-
ture at each traverse point during the traverse; measure the
absolute stack pressure. Determine the moisture percentage,
either by:
-------
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 7 of 8
1. Using a psychrometric chart and making appropriate
corrections if stack pressure is different from that of the
chart, or
2. Using saturation vapor pressure Tables 6.1A and 6. IB
and Equation 6-5.
B
S.V.P.
ws
bar
static
13.6
Equation 6-5
If the psychrometric chart or the saturation vapor pressure
tables are not applicable (based on evaluation of the process),
alternate methods approved by the administrator should be used.
6.6 Constant Sampling Rate Verification
For each sample point, determine the AV and calculate the
average. If the value for any sample point differs from the
average by >10%, reject the results and repeat the run.
Table 6.1A VAPOR PRESSURE OF WATER AT SATURATION (°F), in. Hg
Temp
op
50
60
70
80
90
100
110
120
130
140
150
160
170
180
0
.3626
.5218
.7392
1.032
1.422
1.932
2.596
3.446
4.525
5.881
7.569
9.652
12.20
15.29
1
.3764
.5407
.7648
1.066
1.467
1.992
2.672
3.543
4.647
6.034
7.759
9.885
12.48
15.63
2
.3906
.5601
.7912
1.102
1.513
2.052
2.749
3.642
4.772
6.190
7.952
10.12
12.77
15.98
3
.4052
.5802
.8183
1.138
1.561
2.114
2.829
3.744
4.900
6.380
8.150
10.36
13.07
16.34
4
.4203
.6009
.8462
1.175
1.610
2.178
2.911
3.848
5.031
6.513
8.351
10.61
13.37
16.70
5
.4359
.6222
.8750
1.213
1.660
2.243
2.995
3.954
5.165
6.680
8.557
10.86
13.67
17.07
6
.4520
.6442
.9046
1.253
1.712
2.310
3.081
4.063
5.302
6.850
8.767
11.12
13.98
17.44
7
.4586
.6669
.9352
1.293
1.765
2.379
3.169
4.174
5.442
7.024
8.981
11.38
14.30
17.82
8
.4858
.6903
.9666
1.335
1.819
2.449
3.259
4.289
5.585
7.202
9.200
11.65
14.62
18.21
9
.5035
.7144
.9989
1.378
1.875
2.921
3.351
4.406
5.732
7.384
9.424
11.92
14.96
18.61
-------
Section No. 3.3.6
Revision No. 0
Date January 15, 1980
Page 8 of 8
Table 6.IB VAPOR PRESSURE OF WATER AT SATURATION (°C), mm Hg
Temp
°C
10
20
30
40
50
60
70
80
0
9.20
17.50
31.83
55.32
92.51
149.38
233.68
355.09
1
9.92
18.77
33.91
58.67
97.74
157.23
245.16
371.35
2
10.67
20.1
36.12
62.20
103.20
165.43
257.05
388.37
3
11.07
20.78
37.26
64.03
106.02
169.67
263.14
4
11.65
22.23
39.65
67.87
111.91
178.41
275.84
5
12.79
23.80
42.16
71.86
118.03
187.55
289.05
6
13.73
25.15
44.83
76.07
124.46
197.08
302.77
7
14.74
27.09
47.63
80.49
131.19
207.01
316.99
8
15.26
27.98
49.07
82.78
134.67
212.12
324.36
9
16.36
29.85
52.12
87.53
141.86
222.68
339.60
Table 6.2 ACTIVITY MATRIX FOR CALCULATION CHECKS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Analytical data
form
All data and calcula-
tions are shown
Visual check
Complete miss-
ing data
values
Calculations
Difference between
check and original
calculations should
not exceed roundoff
error
Repeat all calcula-
tions starting with
raw data for hand
calculations; check
all raw data input
for computer calcu-
lations and hand
calculate one sample
per test
Indicate
errors on
analytical
data form,
Fig 4.2
-------
Section No. 3.3.7
Revision No. 0
Date January 15, 1980
Page 1 of 3
7.0 MAINTENANCE
Normal use of emission testing equipment subjects it to
corrosive gases, temperature extremes, vibrations, and shocks.
Keeping the equipment in good operating order over an extended
period of time requires routine maintenance and knowledge of the
equipment. Maintenance of the entire sampling train should be
performed either quarterly or after 1000 ft of operation, which-
ever occurs sooner. Maintenance procedures are summarized in
Table 7.1 at the end of this section. The following procedures
are recommended, but not required, to increase the reliabilty of
the equipment.
7.1 Pumps
Several types of pumps are used in commercial sampling
trains. Two of the most common types are the fiber vane pump
with in-line oiler and the diaphragm pump. ' The fiber vane pump
requires a periodic check of the oil and the oiler jar. The used
oil (usually low nondetergent or machine weight) should be about
the same translucent color as the unused or spare oil. When the
fiber vane pump starts to run erratically or when the head is
removed each year, the fiber vanes should be changed.
The diaphragm pump requires little maintenance. If the
diaphragm pump leaks or runs erratically, it is normally due to a
bad diaphragm or malfunctions in the valves; these parts are
easily replaced and should be cleaned annually by complete dis-
assembly of the train.
7.2 Dry Gas Meters
The dry gas meter should be checked for excess oil and
component corrosion by removing the top plate every 3 mo. The
meter should be disassembled and all components cleaned and
checked more often if the dials show erratic rotation, or if the
meter will not calibrate properly.
7.3 Inclined Manometer
The fluid should be changed when it is discolored or con-
tains visible matter and when it is disassembled yearly. No
-------
Section No. 3.3.7
Revision No. 0
Date January 15, 1980
Page 2 of 3
other routine maintenance is required since the inclined manom-
eter is checked during the leak checks of both the pitot tube and
the entire meter box.
7.4 Sampling Train
All remaining sample train components should be visually
checked every 3 mo, and they should be completely disassembled
and cleaned or replaced yearly. Many of the items, such as quick
disconnects, should be replaced when damaged rather than after
they are periodically checked. Normally, the best maintenance
procedure is to replace the entire unit—for example, a meter
box, sample box, or umbilical cord.
-------
Section No. 3.3.7
Revision No. 0
Date January 15, 1980
Page 3 of 3
Table 7.1 ACTIVITY MATRIX FOR EQUIPMENT MAINTENANCE CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Routine main-
tenance
No erratic behavior
Routine maintenance
quarterly; disassem-
ble and clean yearly
Replace parts
as needed
Fiber vane
pump
Leak free and required
flow
Periodic check of oil
jar; remove head, and
change fiber vanes
Replace as
needed
Diaphragm pump
Leak free valves func-
tioning properly with
required flow
Clean valves during
yearly disassembly
Replace when
leaking or
when running
erratically
Dry gas meter
No excess oil, corro-
sion, or erratic rota-
tion of the dial
Check every 3 mo for
excess oil or corro-
sion by removing
top plate; check
valves and diaphragm
when meter dial runs
erratically or when
meter will not cali-
brate
Replace parts
as needed, or
replace meter
Inclined manom-
eter
No discoloration or
visible matter in the
fluid
Check periodically;
change fluid dur-
ing yearly disassem-
bly
Replace parts
as needed
Sampling train
No damage
Visually check
every 3 mo; com-
pletely disassemble
and clean or replace
yearly
If failure
noted, use
another entire
control console,
sample box, or
umbilical cord
-------
Section No. 3.3.8
Revision No. 0
Date January 15, 1980
Page 1 of 4
8.0 AUDITING PROCEDURE
An audit is an independent assessment of data quality.
Independence is achieved by using apparatus and standards that
are different from those used by the regular field crew. Routine
quality assurance checks by a field team are necessary for
obtaining good quality data, but they are not part of the
auditing procedure. Table 8.1 at the end of this section sum-
marizes the quality assurance activities for the auditing.
Based on the results of the collaborative tests of Method 4,
a performance audit of data processing and a systems audit are
recommended. These two audits are described in the Subsections
8.1 and 8.2.
8.1 Performance Audit of Data Processing
Performance audits are conducted by the auditor to quanti-
tatively evaluate the quality of the data produced by the total
measurement system (sample collection, sample analysis, and data
processing). Due to the limited sizes of most emission-testing
companies, it is recommended that these audits be performed by
the responsible control agency once during every enforcement
source test, regardless of whether the tests are conducted by
agency or private company personnel. A source test for enforce-
ment comprises a series of runs at one source.
Calculation errors are prevalent in Method 4. Data proces-
sing errors can be determined by auditing the data recorded on
the field and the laboratory forms. The original and the check
calculations should agree. If not, all of the data and calcula-
tions should be checked. The calculation errors should be
clearly explained to the source-test team to prevent or mimimize
reoccurrence. The data processing errors may also be determined
by requesting that copies of data sets compiled in the field and
copies of manual data reductions (or computer printouts if used)
be forwarded to the evaluator for audit.
8.2 Systems Audit
A systems audit is an on-site qualitative inspection and
review of the quality assurance method used by the test team for
-------
Section No. 3.3.8
Revision No. 0
Date January 15, 1980
Page 2 of 4
the total measurement system (sample collection, sample analysis,
data processing, etc.). Initially, a systems audit specified by
a quality assurance coordinator should be conducted for each
enforcement source test, which by definition comprises three runs
at one source. After the team gains experience with the method,
the frequency of audit may be reduced--for example, once for
every four tests.
The functions of the auditor are summarized by the fol-
lowing:
1. Observe procedures and techniques of the field team
during sample collection.
2. Check/verify the records of apparatus calibration.
3. Record the results of the audit and forward them with
comments on source team management to the quality assurance
coordinator so that any needed corrective actions may be imple-
mented.
The auditor should observe the field team's overall per-
formance of the source test. Specific operations to observe
should include (but not be limited to):
1. Setting up and leak testing the sampling train.
2. Constant rate sampling check of the sampling train.
3. Final leak check of train.
4. Sample recovery.
Figure 8.1 is a suggested checklist to be used by the auditor for
developing a list of important techniques/steps to observe.
-------
Section No. 3.3.8
Revision No. 0
Date January 15, 1980
Page 3 of 4
Yes No
Operation
Presampling preparation
1. Knowledge of process conditions
2 . Calibration of pertinent equipment prior
to each field test; in particular, the
dry gas meter should be checked before
each test
On-site measurements
3 . Leak testing of sample train after sample
run
4. Addition of water and silica gel to
impingers, and correct location of
impingers
5. Constant sampling rate and not exceeding
specified rate
6. Measurement of condensed water to within
specified limits
7. Record of pertinent process condition
during sample collection
8. Probe maintained at given temperature
Postsampling
9. Calculation procedure/check
10. Calibration checks
COMMENTS
Figure 8.1 Method 4 checklist to be used by auditors.
-------
Section No. 3.3.8
Revision No. 0
Date January 15, 1980
Page 4 of 4
Table 8.1 ACTIVITY MATRIX FOR AUDITING PROCEDURES
Audit
Acceptance limits
Frequency of method
of measurement
Action if
requirements
are not met
Data processing
errors
Original and check cal-
culations should agree
Once during every
enforcement source
test, do independent
calculations starting
with recorded data
Check and cor-
rect all data
for the source
test
Systems audit--
observance of
technique
Operation/technique
described in this sec-
tion of the Handbook
Once during every
enforcement test
until experience
gained, then every
fourth test; observe
techniques; use audit
checklist, Fig 8.1
Explain to
team the devia-
tions from rec-
ommended tech-
niques; note
the deviations
on Fig 8.1
-------
Section No. 3.3.9
Revision No. 0
Date January 15, 1980
Page 1 of 1
9.0 RECOMMENDED STANDARDS FOR ESTABLISHING TRACEABILITY
To achieve data of desired quality, two considerations are
necessary: (1) the measurement process must be in a state of
statistical control, and (2) the systematic errors, when combined
with the random variations (errors of measurement), must result
in an acceptable level of uncertainty. To ensure good data, it
is necessary to perform quality control checks and independent
audits of the measurement process; and to use materials, instru-
ments, and procedures which can be traced to a standard of
reference.
The working calibration standards should be traceable to
primary or higher level standards such as those for the dry gas
meter. The dry gas meter should be calibrated against a wet test
meter which has been verified by an independent liquid displace-
ment meter.
-------
10.0 REFERENCE METHOD
Section No. 3.3.10
Revision No. 0
Date January 15, 1980
Page 1 of 5
METHOD 4—DETERMINATION or MOISTURE IN
STACK OASES
1. Principle and Applcdbility.
1.1 Principle. A gas sample is extracted
proportionally from the source and moisture
la removed from the gas stream, condensed,
and determined either volumetrically or
gravlmetrically.
1.2 Applicability. This method is ap-
plicable for the determination of moisture
in stack gas.
Two methods are given. One is a reference
method for the accurate determination of
moisture content as needed to calculate
emission data. The other is an approximation
method for moisture content to be subse-
quently used for setting isokinetic sampling
rates. For this latter purpose, the tester may
use any alternate means for approximating
the moisture content, e.g. drying tubes, wet
bulb-dry bulb techniqus, condensation tech-
niques, stoichiometrlc calculations, previous
experience, etc. However, tho actual iso-
klnetlo, rate maintained during a pollutant.
sampling run and the moisture content used
to calculate emission data will not be based
on the results of the approximation method
(see exception in note below), but will be
determined from the data of the reference
method, which is normally conducted
simultaneously with a pollutant measure-
ment run.
NOTE.—Any of the approximation methods
which are shown to the satisfaction of the
Administration of yielding results to
within 1% HaO of the reference method re-
sults may be used In lieu of the reference
method.
These methods are not applicable to gas
streams that contain liquid droplets. For
these cases, assume that the gas stream Is
saturated. Determine the average stack gas
temperature using gauges described in
Method 2 and by traversing according to
Method 1. Then obtain the moisture per-
centage by (1) using a psychometric chart
and making appropriate corrections, If stack
pressure is different from that of the chart.
for absolute pressure or (2) by using satura-
tion vapor pressure tables.
2. Reference Method.
The procedure for determining moisture
content described in Method 5 is acceptable
as a reference method.
2.1 Apparatus. A schematic of the sam-
pling train used in this reference method Is
shown in Figure 4-1. All components shall
be maintained and calibrated according to
the procedure outlined in Method 5.
2.1.1 Probe—Stainless steel or glass tub-
ing, sufficiently .heated to prevent water con-
densation and equipped with a alter (either
in-stack or heated out-sfcack) to remove
paniculate matter.
2.1.2 Condenser—Any system that cools
the sample gas stream and allows measure-
ment of the water condensed and moisture
leaving the condenser, each to within 1 ml
or 1 g. Acceptable means are to measure the
condensed water either £ravime1:.rically or
volumetrically and to me.-v.ure the moisture
leaving the condenser by (1) monitoring the
temperature and pressure at the exit of the
condenser and using Dalton's law or (2) by
passing the sample gas .strcprn through a
tared silica gel trap with exit gases kept
below 20" C (68° F) and determining the
weight gain.
2.1.3 Cooling system— Ice bath container
and crushed ice, or equivalent, to aid in con-
densing moLsture.
2.1.4 Drying tube—Tube paclied with 6-16
mesA indicating-type silica gel, or equivalent,
to dry the sample gas and protect the pump
and dry gas meter. This may be on integral
part of the condenser system, in which case
the tube shall be immersed in the ice bath
and a thermometer placed at the outlet for
monitoring purposes. II approach (1) of
section 2.1.2 is used to measure the moisture
leaving the condenser, tho temperature and
j:res..surc must be monitored before tho silica
gel tube.
2.1.5 Metering system—Vacuum gauge,
leak-free pump, thermometers capable of
measuring temperature to within 3' C (5.4'
F), dry gao meter with ±2 percent accuracy,
and related equipment, or other metering
systems approved by the Administrator, as
required to maintain a proportional sampling
rate and to determine sample gas volume.
2 1.6 Barometer—Mercury, aneroid, or
other barometers capable of measuring
atmospheric picture to within 2.5 mm Hg
(0.1 in. Hg). In many cases, the barometric
reading nay te obtained from a nearby
weather bureau station. In which case the
station value (which is the absolute baro-
metric pressure) shall be requested and an
adjustment for elevation differences between
the weather station and the .sampling point
Bhall be applied at a rate of minus 2.5 mm
Hg (0.1 in. Hg) per 30 m (100 ft) elevation
Increase or vice versa for elevation decrease.
FEDERAL REGISTER, VOL. 42, NO. 160—THURSDAY, AUGUST 18, 1977
-------
Section No. 3.3,10
Revision No. 0
Date January 15, 1980
Page 2 of 5
FILTER
•EITHER IN STACK
OR OUT Of STACK)
CONDENSER-ICE BATH SYSTEM INCLUDING
SILICA GEL TUBE —y
AIR-TIGHT
PUMP
Figure 4-1. Moislure sampling Uain-relorence method.
IOCAIION
ep£HATOH ______
DATE
•UN NO.
AMBIENT JEMKMTUIIE.
•MOUETBIC ncssuie _
MODE LENGTH rtfl)-—
SCHEMATIC OF S7ACK CDOSS SECTION
IMVCKE ravn
NUUOER
7OTAI
SAMPIKKS
TUC
lfl.«in.
AVWAGE
5IAC«
TEWCMtltC
•c |M
VELOCItY
HEAD
urjk
m»|».JH2C
nsiSUKf
CIFFEDCKTIAL
Acnoss
OWflCt METEK
I»M).
•»(I..)H20
6AJSAIVU
VOLUIK
•>|l|3)
OAS SAMH.E niPEIlATUM
. ATORVGASMEUI
INIH
lta|.IKI*n
Av«.
A>«.
OUTLET
IT"«*'*ei*'
*«9-
TEXTEDAnW
or CM
UHVIW
COXCCiniRM
LAJI IWUltUl
•CI'll
Flgura 4-2. Fltld mlslur* dtKmlnallon-raferaM* mttwd.
-------
Section No. 3.3,10
Revision No. 0
Date January 15, 1980
Page 3 of 5
j
FINAL
INITIAL
DIFFERENCE
IMPINGER
VOLUME,
ml
SILICA GEL
WEIGHT,
9
'
Figure 4-3. Analytical data-reference method.
2.1.7 Pitot tube—Type 8, or equivalent,
attached to probe to allow constant monitor-
ing of the stack gas velocity so that the
sampling flow rate can be regulated pro-
portional to the stack gaa velocity. The tips
of tb» probe and pitot tube shall be adjacent
to sarti other and the free space between
tbom shall be about 1.9 cm (0.75 In.). When
UMd with this method, the pitot tube need
not be calibrated.
2.1.8 Differential pressure guage—In-
clined manometer capable of measuring
velocity head to within 10 percent of the
minimum measured value or ±0.013 mm
(0.0006 In.), In whichever Is greater. Below a
differential pressure of 1.3 mm (0.05 In.)
water gauge, mlcromanometera with sensi-
tivities of 0.013 mm (0.0005 In.) should be
used. However, mlcromanometera are not
easily adaptable to field conditions and are
' not easy to use with the pulsating flow. Thus,
methods or other devices acceptable to the
Administrator may be used when conditions
warrant.
2.1.6 Temperature gauge—Thermocouple,
liquid filled bulb thermometer, bimetallic
thermometer, mercury-m-glaes thermometer,
or other gauges that are capable of measur-
ing temperature to within 1.5 percent of the
minimi™ absolute stack temperature.
2.1.10 Graduated cylinder and/or bal-
ing* To measure condensed water and
•Mtoture caught In the silica gel to within 1
aal or 1 g. Graduated cylinders shall have
subdivisions no greater than 2 ml. Most lab-
oratory balances are capable of weighing to
tlM mearest 0.5 g or less. These balances are
suitable 'for use here.
2.1.11 Temperature and pressure gauges—
V Dalton's law is used to monitor tempera-
. tun and pressure at condenser outlet. The
temperature gauge shall have an accuracy of
1* O (3* F). The pressure gauge shall be capa-
ble of measuring pressure to within 2.5 mm
Kg (0.1 In. Hg).
2.1.12 Silica gel—If used to measure
motature leaving condenser, indicating type,
•-!• mesh. If previously used, dry at 175* C
(MO* F) for 2 hours. New silica gel may be
used as received.
2J Procedure. The procedure below is
written for a condenser system incorporating
•Oloa gel and gravimetric analysis to measure
the> moisture leaving the condenser and volu-
Mrtrlo analysis to measure the condensed
•ototure.
2.2.1 Select the sampling site and mini-
mum number of sampling points according
«• Method 1 or a* specified by the Admin-
trtratur Dvtermin* the rang* of velocity
kMA using Ustttod 2 for ttos purpose of mak-
taf proportional sampling rate calculation*.
Select a suitable velocity head to correspond
- to about 0.014 m'/min (0.5 cfm). Select a
suitable probe and probe length such that all
traverse points can be sampled. Consider
sampling from opposite sides (four total
. sampling ports) for large stacks to enable
use of shorter probe lengths. Mark probe with
heat resistant tape or by some other method
to denote the proper distance into the stack
or duct for each sampling point. Weigh and
record weight of silica gel to the nearest 0.5 g.
2.2.2 Select a suitable total sampling time
of no less than 1 hour such that a minimum
total gas sample volume of 0.6 m* (20 ff) at
standard conditions will be collected and the
sampling time per traverse point is not less
than 2 min., or some greater time Interval
as specified by the Administrator.
2.2.3 Set up the sampling train as shown
in Figure 4-1. Turn on the probe heating sys-
tem to about 120' C (248* F) so as to prevent
water condensation and allow time for tem-
perature to stabilize. Place crushed Ice in
the ice bath container. Leak check the train
by plugging the probe inlet and pulling a 380
• mm Hg (15 in. Hg) vacuum. A leakage rate
in excess of 4 percent of the average sampling
rate or 0.00057 m'/mln. (0.02 cfm), which
ever is less, Is unacceptable.
2.2.4 During the sampling run, maintain
a sampling rate within 20 percent, or as spec-
ified by the Administrator, of constant
proportionality. For each run, record the
data required on the example data sheet
shown in Figure 4-2. Be sure to record the
Initial dry gas meter reading. Record the dry
gas meter reading at the beginning and end
of each sampling time Increment, when
changes in flow rates are made, and when
sampling Is halted. Take other data point
readings at each sample point at least once
during each time Increment.
2.2.5 To begin sampling position the probe
tip at the first traverse point. Immediately
start the pump and adjust the flow to pro-
portional conditions. Traverse the cross sec-
tion. Add more ice and, if necessary, salt to
maintain a temperature of less than 20* O
(68* F) at the silica gel outlet to avoid exces-
sive moisture losses.
2.2.6 After collecting the sample, measure
the volume Increase of the liquid to the near-
est 1 ml. Determine the increase in weight
of the silica gel tube to the nearest 0.6 g.
Record the information (see example, data
sheet, Figure 4-3) and calculate the moisture
percentage.
2.3 Calculations. Carry out calculations,
retaining at least one extra decimal figure
beyond that of the acquired data. Bound off
figures after final calculation.
2.3.1 Nomenclature.
-------
Bw.= Proportion by volume
Mw=Molecular weight of water, 18 g/g-mUe (18 Ib/lb-mole)
?»•=• Absolute pressure (for this method, same as barometric pressure) at th« dry
gas meter, mm Eg (in. Hg)
P«d—Standard absolute pressure, 760 mm Hg (29.92 In. Hg)
R«= Ideal gas constant, 0.06236 (mm hg)(ms)/(g-mole)(°K) for metric units end
21.83 (in. Hg)tft3)/(lb-mole)/(lb-mole)(°R) for English units
Tm«= Absolute temperature at meter, °K (°R)
Trtd=Absolute temperature, 293° K (528° R)
Vm"= Dry gas volume measured by meter, dcm (dcf)
V]c,ltd! = Dry gas volume measured by the dry gas meter, corrected to standard condi-
tions, dscm (dscf)
V,,(rtd)=Volume of water vapor condensed corrected to standard conditions, m* (ft*)
V»«(.,d>= Volume of water vapor collected in silica gel corrected to standard conditions,
m»
*
U)
vo
oo
o
-------
Section No, 3,3.10
Revision No, 0
Date January 15, 1980
Page 5 of 5
3.1.3 Ice bath—Container and ice,- to aid
In condensing moisture in impingers.
, 3.1.4 Drying tube—Tube packed with 0-1«
mesh indicating-type silica gel, or equivalent,
to dry the sample gas and to protect the
meter and pump. <
3.1.5 Valve—Needle valve, to' regulate"
sample gas flow rate.
3.1.8 Pump—Leak-free, diaphragm type,
or equivalent, to pull gas through the train.
3.1.7 Volume meter—Dry gas meter, suf-
ficiently accurate to measure the sample vol-
ume within 2 percent, and calibrated over the
range of flow rates and conditions actually
used during sampling.
3.1.8 Rate meter—Rotameter, to measure
the flow range from 0 to 3 1pm (0 to 0.11
cfm).
3.1.9 Graduated cylinder—25 ml.
3.1.10 Barometer—Mercury, aneroid, or
other barometers capable of measuring
atmospheric pressure to within '2.5 mm Hg
(0.1 In. Hg). In. many cases, the barometric
reading may be obtained from a nearby
weather bureau station, in which case the
station value (which is the absolute baro-
metric pressure) shall be requested and an
adjustment for elevation differences between
the weather station and sampling point shall
be applied at a rate of minus 2.6 mm Hg
(0.1 In. Hg) per 30 m (100 ft) elevation in-
crease or vice versa for elevation decreases.
3.1.11 Vacuum gauge—At least 760 mm
Bg (30 in. Hg) gauge, to be used for the
sampling leak check.
3.2 Procedure.
3.2.1 Place exactly 6 ml distilled water In
each Implnger. Assemble the apparatus
without the probe as shown in Figure 4-4.
Leak check by placing a vacuum gauge at the
Inlet to the first impinger and drawing a
vacuum of at least 250 mm Hg (10 in. Hg),
plugging the outlet of the rotameter, and
then turning off the pump. The vacuum shall
remain constant for a least one minute.
Carefully release the vacuum gauge before
releasing the rotameter end.
3.2.2 Connect the probe and sample at a
constant rate of 2 1pm (0.071 cfm). Continue
sampling until the dry gas. meter registers
about 30 liters (1.1 ft") or until visible liquid
droplets are carried over from the first 1m-
piuger to the second. Record temperature,
pressure, and dry gas meter readings as re-
quired by Figure 4-5.
3.3.3 After collecting the sample, combine
the contents of the two impingers and meas-
ure volume to the nearest 0.5 ml.
3.3 Calculations. The calculation method
presented Is designed to estimate the mote*
ture in the stack gas and therefore other
data, which are only necessary-for accurate
moisture determinations, are not collected.
The following equations adequately estimate
the moisture content for the purpose of de-
termining iBokinetic sampling rate settings.
3.8.1 Nomenclature.
B.
-------
Section No. 3.3.11
Revision No. 0
Date January 15, 1980
Page 1 of 1
11.0 REFERENCES
1. Martin, R. W. Construction Details of Isokinetic
Source Sampling Equipment. APTD-0581. Air Pollution
Control Office, EPA, Research Triangle Park, N.C.,
1971.
2. Rom, J. J. Maintenance, Calibration, and Operation of
Isokinetic Source Sampling Equipment. APTD-0576.
Office of Air Programs, EPA, Research Triangle Park,
N.C., 1972.
3. Midgett, M. R. The EPA Program for the Standardiza-
tion of Stationary Source Emission Test Methodology—A
Review. EPA-600/4-76-044. Environmental Monitoring
and Support Laboratory, EPA, Research Triangle Park,
N.C., 1976.
-------
Section No. 3.3.12
Revision No. 0
Date January 15, 1980
Page 1 of 14
12.0 DATA FORMS
Blank data forms are provided on the following pages for the
convenience of the Handbook user. Each blank form has the cus-
tomary descriptive title centered at the top of the page. How-
ever, the section-page documentation in the top right-hand corner
of each page of other sections has been replaced with a number in
the lower right-hand corner that will enable the user to identify
and refer to a similar filled-in form in a text section. For
example, Form M4-1.2 indicates that the form is Figure 1.2 in
Section 3.3.1 of the Method 4 Handbook. Future revisions of
these forms, if any, can be documented by 1.2A, 1.2B, etc.
Eight of the blank forms listed below are included in this sec-
tion. Four are in the Method Highlights Section, as shown by the
MH following the form number.
Form Title
1.2 Procurement Log
2.3A & B Meter Box Calibration Data and Calculation
Form (English and Metric units)
2.4A & B Posttest Meter Calibration Data Form
(English and Metric units)
2.5 (MH) Pretest Sampling Checks
3.1 (MH) Pretest Preparation Checklist
4.1 (MH) On-Site Measurement Checklist
4.2 Method 4 Field and Sample Recovery Data Form
4.3 Method 4 Analytical Data Form
5.1 (MH) Posttest Equipment Checks
6.1A & B Moisture Content Calculation Form
(English and Metric units)
6.1.C Moisture Content Calculation Form
(English and Metric units)
8.1 Method 4 Checklist To Be Used By Auditors
-------
PROCUREMENT LOG
Item description
Quantity
Purchase
order
number
Vendor
Date
Ordered
Received
Cost
Dispo-
sition
Comments
Quality Assurance Handbook M4-1.2
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM
(English units)
Date
Barometric pressure, P, =
Meter box number
in. Hg Calibrated by
Orifice
manometer
setting
(AH),
in. H20
0.5
1.0
1.5
2.0
3.0
4.0
Gas volume
Wet test
meter
(V ) ,
fl3
5
5
10
10
10
10
Dry gas
meter
(vd),
ft3
Temperature
Wet test
meter
op-
Dry gas meter
Inlet
(td_),
op-
Outlet
(td),
o
op-
Avg°
(td),
Time
(8),
min
Avg
Y.
i
AH@.
in. H,~
AH,
in.
H 0
2
0.5
1.0
1.5
2.0
3.0
4.0
AH
13.6
0.0368
0.0737
0.110
0.147
0.221
0.294
V P, (t, + 460)
Y _ w bv d
1 V (T + ^^ } fi- + A£fO
Vd(rb 13. 6} (t + A60)
f(t + 460) 0] 2
0.0317 AH V w
^i - P (t + 460) V
OQ L w J
--'
o
If there is only one thermometer on the dry gas meter, record the temperature
iir» do v i-
under t,.
d
Quality Assurance Handbook M4-2.3A (front side)
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM (English units)
Nomenclature:
3
V = Gas volume passing through the wet test meter, ft .
W
3
V, = Gas volume passing through the dry gas meter, ft .
t = Temperature of the gas in the wet test meter, °F.
W
t, = Temperature of the inlet gas of the dry gas meter, °F.
t, = Temperature of the outlet gas of the dry gas meter, °F.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average t, and
t °F i
M '
o
AH = Pressure differential across orifice, in. H20.
Y- = Ratio of accuracy of wet test meter to dry gas meter for each run; tolerance Y- =
Y ±0.02Y.
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs;
tolerance Y = Y 10.01Y.
3
AH@. = Orifice pressure differential at each flow rate that gives 0.75 ft /mm of air at
1 standard conditions for each calibration run, in. H20; tolerance = AH@ ±0.15
(recommended).
AH@ = Average orifice pressure differential that gives 0.75 ft /min of air at standard
conditions for all six runs, in. H-O; tolerance = 1.84 ±0.25 (recommended).
8 = Time for each calibration run, min.
P, = Barometric pressure, in. Hg.
Quality Assurance Handbook M4-2.3A (back side)
-------
Date
Barometric pressure, P, =
METER BOX CALIBRATION DATA AND CALCULATION FORM
(Metric units)
Meter box number
mm Hg Calibrated by
Orifice
manometer
setting
(AH),
mm HO
10
25
40
50
75
100
Gas volume
Wet test
meter
(V>
3
m
0.15
0.15
0.30
0.30
0.30
0.30
Dry gas
meter
(vd),
3
m
Temperature
Wet test
meter
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM (metric units)
Nomenclature:
3
V = Gas volume passing through the wet test meter, m .
W
3
V, = Gas volume passing through the dry gas meter, m .
t = Temperature of the gas in the wet test meter, °C.
W
td = Temperature of the inlet gas of the dry gas meter, °C.
t, = Temperature of the outlet gas of the dry gas meter, °C.
o
t-, = Average temperature of the gas in the dry gas meter, obtained by the average of t-, and
t °c i
Ld , <~. j-
o
AH = Pressure differential across orifice, mm H-O.
Y. = Ratio of accuracy of wet test meter to dry gas meter for each run; tolerance Y- =
Y +0.02Y.
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs;
tolerance Y = Y +0.01Y.
3
AH@. = Orifice pressure differential at each flow rate that gives 0.021 m of air at standard
1 conditions for each calibration run, mm H20; tolerance AH@. = AH@ +3.8 mm H-O
(recommended).
3
AH§ = Average orifice pressure differential that gives 0.021 m of air at standard con-
ditions for all six runs, mm H20; tolerance AH@ = 46.74 +6.3 mm H20 (recommended).
0 = Time of each calibration run, min.
P, = Barometric pressure, mm Hg.
Quality Assurance Handbook M4-2.3B (back side)
-------
POSTTEST DRY GAS METER CALIBRATION DATA FORM (English units)
Test number
Date
Meter box number
Plant
Barometric pressure, P, =
in. Hg Dry gas meter number
Pretest Y
Orifice
manometer
setting,
(AH),
in. H20
Gas volume
Wet test
meter
<*,]•
ftJ
10
10
10
Dry gas
meter
(vd),
ft
Temperature
Wet test
meter
°F
Dry gas meter
Inlet
(td),
i
op-
Outlet
(td),
0
°F
Average
(t,),3
°F
Time
(6),
min
Vacuum
setting,
in. Hg
Y.
i
Y.
i
V P, (t, + 460)
w b d
V, /Pb + AH Wt + A60\
d I b 13. eA w /
Y =
If there is only one thermometer on the dry gas meter, record the temperature under t-
where
3
V = Gas volume passing through the wet test meter, ft .
W 3
V, = Gas volume passing through the dry gas meter, ft .
t = Temperature of the gas in the wet test meter, °F.
t, = Temperature of the inlet gas of the dry gas meter, °F.
i
t, = Temperature of the outlet gas of the dry gas meter, °F.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average of t, and t, , °F.
AH = Pressure differential across orifice, in. H.O.
Y. = Ratio of accuracy of wet test meter to dry gas meter for each run.
Y = Average ratio of accuracy of wet test meter to dry gas meter for all three runs;
tolerance = pretest Y +0.05Y.
P, = Barometric pressure, in. Hg.
0 = Time of calibration run, min.
Quality Assurance Handbook M4-2.4A
-------
Test number
POSTTES: METER CALIBRATION DATA FORM (Metric units)
Date Meter box number
Plant
Barometric pressure, P =
mm Hg Dry gas meter number
Pretest Y
Orifice
manometer
setting,
(AH),
mm H20
Gas volume
Wet test
meter
"„>•
m
10
10
10
Dry gas
meter
(vd),
m
Temperature
Wet test
meter
a
°C
Time
(0),
min
Vacuum
setting,
mm Hg
Y.
i
Y.
i
V P, (t, + 273)
w b d
V /P + AH Vt + 273
d V b 13. 6A W
Y =
If there is only one thermometer on the dry gas meter, record the temperature under t
where
3
V = Gas volume passing through the wet test meter, m .
W 3
V, = Gas volume passing through the dry gas meter, jn .
t = Temperature of the gas in the wet test meter, °C.
t, = Temperature of the inlet gas of the dry gas meter, °C.
i
t, = Temperature of the outlet gas of the dry gas meter, °C.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average of t, and t, , °C.
i o
AH = Pressure differential across orifice, mm H«0.
Y. = Ratio of accuracy of wet test meter to dry gas meter for each run.
Y = Average ratio of accuracy of wet test meter to dry gas meter for all three runs;
tolerance = pretest Y +0.05Y.
P, = Barometric pressure, mm Hg.
6 = Time of calibration run, min.
Quality Assurance Handbook M4-2.4B
-------
METHOD 4 FIELD AND SAMPLE RECOVERY DATA FORM
Plant
Location
Operator
Date
Run number
Ambient temperature
Barometric pressure
Probe length m(ft)
Probe material _
Sample box number
Meter box number
Meter AH@ "
Meter cal.
Final
leak
(Y)
rate
Vacuum during leak check
Thermometer number _ _
Static
Final
Initial
Impinger
volume,
ml
Silica gel
weight,
8
pressure
Traverse
point
number
Sampling
time (6) ,
min
Stack
temper-
ature,
°C (°F)
Pressure
differential
across
orifice meter
(AH),
mm (in. ) H_0
Meter
reading
gas sample
volume ,
Q Q
nf* (ftJ)
*
AV ,
m
"5 Q
m-3 (fO
Gas sample temperature
at dry gas meter
Inlet
(Tin. )°C(°F)
Outlet
(Tm )°C(°F)
out
Temperature
of gas
leaving
condenser or
last impinger,
°C (°F)
Total
Average
Acceptable AV =
m
0 V final - V initial
number of points
to
Quality Assurance Handbook M4-4.2
-------
METHOD 4 ANALYTICAL DATA FORM
Plant
Date
Run number
Final
Initial
Liquid collected
Total volume collected
Volume of liquid
water collected
Impinger
volume,
ml
Silica gel
weight,
g
g*
ml
* Convert weight of water to volume by dividing total weight
increase by density of water (1 g/ml):
Increase, g . n
, a/m-\ = water volume, ml.
Quality Assurance Handbook M4-4.3
-------
MOISTURE CONTENT CALCULATION FORM
(English units)
VOLUME OF WATER VAPOR CONDENSED IN IMPINGERS
V- = . ml, V. = .ml
I — — — l — — —
Vwc(std) = 0-04707 (Vf - Vi) = _ _ . ft3 Equation 6-1
VOLUME OF WATER VAPOR COLLECTED IN SILICA GEL
Wf = . _ g, W. = _ . g
J_ — J. — — — _
Vwsg(std) = °-04715 (Wf - Wi) = _ . ft3 Equation 6-2
SAMPLE VOLUME
Vm = - - ' ft3' Tm = •_ °R, Pm =__•__ in. Hg
Y =
V Y P ,
Vm(std) = 17-64 "^ = - - ' ft Equation 6-3
MOISTURE CONTENT
Vwc(std) = ' ft ' vwsg(std) = - * ft
Vm(std) = - - • ft"
_ wc(std) wsg(std) „ . . . .
ws = v +V + V = - ' Equation 6-4
s vwc(std) wsg(std) vm(std)
Quality Assurance Handbook M4-6.1A
-------
MOISTURE CONTENT CALCULATION FORM
(Metric units)
VOLUME OF WATER VAPOR CONDENSED IN IMPINGERS
Vf = . ml, Vi = . ml
Vwc(std) = °-001333 (vf ~ vi.) =- • m3 Equation 6-1
VOLUME OF WATER VAPOR COLLECTED IN SILICA GEL
Vwsg(std) = °-001335 (Wf - Wi) = _ . m3 Equation 6-2
SAMPLE VOLUME
Vm = - • ---- *' Tm = --- • - °K' Pm = --- • _ mm Hg
V Y P
= 0.3858 -^= = . m Equation 6-3
j.
MOISTURE CONTENT
_ 3 3
Vwc(std) = - • m ' Vwsg(std) = - ' m '
Vm(std) = - ' m
- VWC(5td) + VWSg(std) _ Wmia-Hrm fi A
- v + v + v • Equation 6-4
wc(std) wsg(std) m(std)
Quality Assurance Handbook M4-6.1B
-------
MOISTURE CONTENT CALCULATION FORM
(English and metric units)
MOISTURE CONTENT
tg avg = . _. °F, . °C
P, = . in. Hg, . mm Hg
LJQ.JL
Pstatic = ----- in- H2°' - - ' - - "» H2°
S.V.P. = _ . in. Hg, . _mmHg
B = S.V.P =
ws _ + Pstatic -
13.6
Quality Assurance Handbook M4-6.1C
-------
METHOD 4 CHECKLIST TO BE USED BY AUDITORS
Yes No
Operation
Presampling preparation
1. Knowledge of process conditions
2 . Calibration of pertinent equipment prior
to each field test; in particular, the
dry gas meter should be checked before
each test
On- site measurements
3 . Leak testing of sample train after sample
run
4. Addition of water and silica gel to
impingers, and correct location of
impingers
5. Constant sampling rate and not exceeding
specified rate
6. Measurement of condensed water to within
specified limits
7. Record of pertinent process condition
during sample collection
8. Probe maintained at given temperature
Posts ampling
9. Calculation procedure/check
10. Calibration checks
COMMENTS
Quality Assurance Handbook M4-8.1
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 1 of 17
Section 3.4
METHOD 5—DETERMINATION OF PARTICULATE EMISSIONS
FROM STATIONARY SOURCES
OUTLINE
Number of
Section Documentation Pages
SUMMARY 3.4 l
METHOD HIGHLIGHTS 3.4 15
METHOD DESCRIPTION
1. PROCUREMENT OF APPARATUS
AND SUPPLIES 3.4.1 15
2. CALIBRATION OF APPARATUS 3.4.2 22
3. PRESAMPLING OPERATIONS 3.4.3 20
4. ON-SITE MEASUREMENTS 3.4.4 19
5. POSTSAMPLING OPERATIONS 3.4.5 15
6. CALCULATIONS 3.4.6 10
7. MAINTENANCE 3.4.7 3
8. AUDITING PROCEDURE 3.4.8 7
9. RECOMMENDED STANDARDS FOR
ESTABLISHING TRACEABILITY 3.4.9 1
10. REFERENCE METHOD 3.4.10 6
11. REFERENCES 3.4.11 2
12. DATA FORMS 3.4.12 21
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 2 of 17
SUMMARY
This method, when used in conjunction with Methods 1, 2, 3,
and 4, is applicable for the determination of particulate emis-
sions from stationary sources.
A gas sample is extracted isokinetically from the stack.
Particulate matter is collected on an out-of-stack, glass fiber
filter, maintained at 120° ±14°C (248° ±25°F) or at a tempera-
ture specified by an applicable subpart of the standards or
approved by the administrator. The mass of particulate matter,
which includes any material that condenses at or above the spe-
cified filter temperature, is measured gravimetrically after
removal of uncombined water.
The Method Description which follows is based on the Refer-
ence Method that was promulgated on August 18, 1977. Results of
an initial collaborative test program indicated the need for more
specific quality controls and a better defined Reference Method,
which resulted in the expansion and revisions incorporated in the
August 18, 1977 promulgation. As a result, competence of the
tester becomes the primary factor affecting the precision of
Method 5. Results of the most recent collaborative test program,
conducted with competent test teams, showed a within-laboratory
deviation (standard deviation percent of mean value) of 10.4% and
2
a between laboratory deviation of 12.1%.
The main documents used in preparing the description and in
detailing calibration and maintenance procedures are references
1, 3, and 4 (Section 3.4.11). Data forms are provided in Section
3.4.12 for the convenience of the Handbook users.
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 3 of 17
METHOD HIGHLIGHTS
EPA Method 5, collectively with EPA Methods 1, 2, 3, and 4
comprise the most widely used system for evaluating emissions
from stationary sources. Consequently, many of the special
problems and procedures common to several related methods are
discussed in depth in this section of the Handbook. As opposed
to some methods, the most significant errors associated with this
test method occur during the sample collection and recovery phase
instead of in the analysis phase. Therefore, this method re-
quires competent personnel adhering to the procedures. Compe-
tence can be determined, most accurately, through observation and
evaluation by a qualified observer on site.
The blank data forms at the end of this section may be
removed from the Handbook and used in the pretest, test, and
posttest operations. Each form has a subtitle (e.g., Method 5,
Figure 3.1) to assist the user in finding a similar filled-in
form in the method description (e.g., in Section 3.4.3). On the
blank and filled-in forms, the items/parameters that can cause
the most significant errors are designated with an asterisk.
1. Procurement of Equipment
Section 3.4.1 (Procurement of Apparatus and Supplies) gives
the specifications, criteria and design features for equipment
and materials required for performing Method 5 tests. Special
design criteria have been established for the pitot tube, probe,
nozzle, and temperature sensor assembly.
These criteria specify the necessary spacing requirements
for the various components of the assembly to prevent aerodynamic
interferences that could cause large errors in velocity pressure
measurement. Seamless, corrosion resistant metal probe liners
have also been made optional, subject to the approval of the
administrator.
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 4 of 17
Section 3.4.1 is designed as a guide for the procurement and
initial check of equipment and supplies. The activity matrix
(Table 1.1) at the end of Section 3.4.1 can be used as a quick
reference; it follows the same order as the written description
in the main text.
2. Pretest Preparation
Section 3,4.2 (Calibration of Apparatus) provides a step-by-
step description of the required calibration procedures for
components of the Method 5 sampling train. Data forms have been
developed to record the data and to provide a calibration record.
Careful attention should be given to the steps in each procedure,
since most procedures have not been previously written and re-
ferenced in the Federal Register. The calibration section can be
removed and compiled, along with calibration sections from all
other methods, into a separate quality assurance Reference Manual
for use by calibration personnel. A pretest checklist
(Figure 3.1) or a similar form should be used to summarize cali-
bration data.
Section 3.4.3 (Presampling Operations) provides the tester
with a guide for supplies and equipment preparation for field
tests. The pretest preparation form (Figure 3.2) can be used as
an equipment checkout and packing list. (Due to the length of
this figure, the blank data forms are in Section 3.4.12.) This
form was designed to provide the user with a single form that can
include any combination of Methods 1 through 8 for the same field
trip. The method for packing and the description of packing con-
tainers should help protect the equipment, but are not required.
Filter holders and impingers may be loaded and charged in the
base laboratory. If this is done, seal the inlet and outlet of
the filter holder, the impingers containing water, and the im-
pinger containing silica gel.
3. On-site Measurements
Section 3.4.4 (On-site Measurements) contains a step-by-step
procedure for performing sampling and sample recovery. Several
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 5 of 17
on-site measurement requirements have been added which will
significantly improve the accuracy and precision of the method.
These added requirements include:
1. Make a corresponding change in the sampling rate when
velocity pressure at each sampling point changes by >20%,
2. Leak check the sampling train at the conclusion of the
sampling run and prior to each component change during a sample
run,
3. Leak check the pitot tube at the conclusion of the
sampling run, and
4. Have one traverse diameter in a plane containing the
greatest expected concentration variation.
The on-site measurement checklist (Figure 4.5) is provided to
assist the tester with a quick method of checking requirements.
4. Posttest Operations
Section 3.4.5 (Postsampling Operations) gives the posttest
equipment check procedures and a step-by-step analytical proce-
dure. Figure 5.1, or a similar form, should be used to summarize
the posttest calibration checks and should be included in the
emission test report.
The posttest operation forms (Figures 5.5 and 5.6) will
provide laboratory personnel with a summary of analytical proce-
dures used to determine the sample rinse and filter weights.
This analytical procedure description can be removed from the
main text and compiled, along with analytical procedures for
other methods, into a separate quality assurance analytical ref-
erence manual for laboratory personnel. The use of blank filters
as control samples is required to provide an independent check on
the state of control of the samples. Procedures are also given
for data corrections when equipment calibration factors change.
Section 3.4.6 (Calculations) provides the tester with the
required equations, nomenclature, and suggested number of signi-
ficant digits. It is suggested that a programmable calculator be
used, if available, to reduce the chances of calculation error.
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 6 of 17
Section 3.4.7 (Maintenance) supplies the tester with a guide
for a routine maintenance program. The program is not a require-
ment, but is suggested for the reduction of equipment malfunc-
tions .
5. Auditing Procedures
Section 3.4.8 (Auditing Procedures) contains a description
of necessary activities for conducting performance and system
audits. The performance audit is a check on calculation errors,
and therefore is not needed for the analytical phase since it
consists of only a gravimetric determination. Together, a per-
formance audit of data processing and a systems audit of on-site
measurements should provide the independent assessment of data
quality needed to allow the collaborative test results to be used
in the final data evaluation.
Section 3.4.9 (Recommended Standards for Establishing Trace-
ability) recommends the primary standards to which the sample
collection and analysis should be traceable.
6. References
Sections 3.4.10 and 3.4.11 (References) provides the reader
with the Reference Method and an extensive list of all the ref-
erences used in the compilation of this section of the Handbook
along with numerous additional sources.
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 7 of 17
PRETEST SAMPLING CHECKS
(Method 5, Figure 3.1)
Date
Meter box number
Calibrated by
AH@
Dry Gas Meter*
Pretest calibration factor, Y
average factor for each calibration run)
Impinger Thermometer
Was a pretest temperature correction used?
If yes, temperature correction
over range)
Dry Gas Meter Thermometers
(within ±2% of the
yes
no
(within ±3°C (5.4°F)
yes
no
Was a pretest temperature correction made?
If yes, temperature correction (within ±3°C (5.4°F) over
range)
Stack Temperature Sensor*
Was a stack temperature sensor calibrated against a reference
thermometer? yes no
If yes, give temperature range with which the readings agreed
within ±1.5% of the reference values to K (°R)
Barometer
Was the pretest field barometer reading correct? yes no
(within ±2.5 mm (0.1 in.) Hg of the mercury-in-glass barometer)
Nozzle*
Was the nozzle calibrated to the nearest 0.025 mm (0.001 in.)?
yes no
*Most significant items/parameters to be checked.
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 8 of 17
ON-SITE MEASUREMENTS CHECKLIST
(Method 5, Figure 4.5)
Sampling Train Schematic Drawing
Apparatus
Probe nozzle: stainless steel glass
Button-hook elbow size
Clean?
Probe liner: borosilicate quartz other
Clean?
Heating system*
Checked?
Pitot tube: Type S other
Properly attached to probe?*
Modifications
Pitot tube coefficient
Differential pressure gauge: two inclined manometers
other sensitivity
Filter holder: borosilicate glass glass frit
filter support silicone gasket other
Clean?
Condenser:number of impingers
Clean?
Contents: 1st 2nd 3rd 4th
Cooling system
Proper connections?
Modifications
Barometer: mercury aneroid other
Gas density determination: temperature sensor type
pressure gauge
temperature sensor properly attached to probe?*
Procedure
Recent calibration: pitot tubes*
meter box* thermometers/thermocouples*
Filters checked visually for irregularities?*
Filters properly labeled?*
Sampling site properly selected?
Nozzle size properly selected?*
(continued)
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 9 of 17
(continued)
Selection of sampling time?
All openings to sampling train plugged to prevent pretest con-
tamination?
Impingers properly assembled?
Filter properly centered?
Pitot tube lines checked for plugging or leaks?*
Meter box leveled? Periodically?
Manometers zeroed?
AH@ from most recent calibration
Nomograph set up properly?
Care taken to avoid scraping nipple or stack wall?*
Effective seal around probe when in-stack?
Probe moved at proper time?
Nozzle and pitot tube parallel to stack wall at all times?*
Filter changed during run?
Any particulate lost?
Data forms complete and data properly recorded?*
Nomograph setting changed when stack temp changed significantly?
Velocity pressure and orifice pressure readings recorded
accurately?*
Posttest leak check performed?* (mandatory)
Leakage rate @ in. Hg
Orsat analysis from stack integrated
Fyrite combustion analysis sample location
Bag system leakchecked?*
If data forms cannot be copied, record:
approximate stack temp volume metered
% isokinetic calculated at end of each run
SAMPLE RECOVERY
Brushes: nylon bristle other
Clean?
Wash bottles: glass
Clean?
Storage containers: borosilicate glass other
Clean? Leakfree?
Petri dishes: glass polyethylene other _
Clean? _
Graduated cylinder/or balance: subdivisions <_2 ml?* ]^^^
other
Balance: type
Plastic storage containers: airtight? ZZZ^ZZIZIII^ZZ^ZI
Clean?
Probe allowed to cool sufficiently?
Cap placed over nozzle tip to prevent loss of particulate?*
(continued)
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 10 of 17
(continued)
During sampling train disassembly, are all openings capped?
Clean-up area description:
Clean? Protected from wind?
Filters: glass fiber type
Silica gel: type (6 to 16 mesh)? new? used?
Color? Condition?
Filter handling: tweezers used?
surgical gloves? other
Any particulate spilled?*
Water distilled?
Stopcock grease: acetone-insoluble?
heat-stable silicone? other
Probe handling: acetone rinse
distilled water rinse
Particulate recovery from: probe nozzle
probe fitting probe liner
front half of filter holder
Blank: acetone distilled water _
Any visible particles on filter holder inside probe?:*
All jars adequately labeled? Sealed tightly?
Liquid level marked on jars?*
Locked up?
Acetone reagent: <0.001% residue?
glass bottles (required)
acetone blanks?
*Most significant items/parameters to be checked.
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 11 of 17
POSTTEST CALIBRATION CHECKS
(Method 5, Figure 5.1)
Plant Calibrated by
Meter box number Date
Dry Gas Meter
Pretest calibration factor, Y (within ±2%)
Posttest check, Y* (within ±5% of pretest)
Recalibration required? yes no
If yes, recalibration factor, Y (within ±2%)
Lower calibration factor, Y for calculations (pretest or
posttest)
Dry Gas Meter Thermometers
Was a pretest temperature correction used? yes no
If yes, temperature correction (within ±3°C (5.4°F) over
range)
Posttest comparison with mercury-in-glass thermometer?* (within
±6°C (10.8°F) at ambient temperature)
Recalibration required? yes no
Recalibration temperature correction? (within ±3°C
(5.4°F) over range)*
If yes, no correction necessary for calculations if meter
thermometer temperature is higher; if calibration temperature
is higher, add correction to average meter temperature for
calculations
Stack Temperature Sensor
Was a pretest temperature correction used? yes no
If yes, temperature correction °C (°F) (within ±1.5% of
readings in K (°R) over range)
Average stack temperature of compliance test, T __K (°R)
Temperature of reference thermometer or solution for recalibra-
tion K (°R)* (within ±10% of T )
Temperature of stack thermometer for recalibration K (°R)
Difference between reference and stack thermometer temperatures,
AT K (°R)
Do vllues agree within ±1.5%?* yes no
If yes, no correction necessary for calculations
If no, calculations must be done twice—once with the recorded
values and once with the average stack temperature corrected to
correspond to the reference temperature differential (ATg);
both final result values must be reported since there is no way
to determine which is correct
(continued)
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 12 of 17
(continued)
Barometer
Was the pretest field barometer reading correct? yes no
Posttest comparison?* mm (in.) Hg (±2.5 mm (0.1 in.) Hg)
Was calibration required? yes no
If yes, no correction necessary for calculations when the field
barometer has a lower reading; if the mercury-in-glass reading
is lower, subtract the difference from the field data readings
for the calculation
*Most significant items/parameters to be checked.
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 13 of 17
Status
PROCEDURE FOR WEIGHING FILTERS
BEFORE AND AFTER SAMPLING
(Method 5, Figure 5.5)
Label the filter and/or the petri dish—both with
the same label number; label the filter on top and
bottom; check each filter visually against the
light for irregularities, flaws, and pinhole leaks
Check the desiccator; be sure the lid is sealed
tightly and the anhydrous calcium sulfate is dry;
if not dry, heat the desiccant in the oven for 2 h
at 180°-200°C (350° - 400°F), and let cool in the
balance room before putting it back into the des-
iccator
Take off the lid of the filter container and
desiccate the filter for 24 h; during desiccation,
be sure that filters are widely spread, and not
overlapping
Adjust the analytical balance to zero, and check
the accuracy with a 0.500-g Class-S weights (with-
in ±0.5 mg); use tweezers to carefully place the
filter on the pan of the balance, and weigh it to
the nearest 0.1 mg. The time of weighing should
not be >2 min, and the relative humidity should
be _6 h and reweigh the fil-
ter; the two recorded weights should agree to
±0.5 mg; if not, desiccate for another 6 h and
reweigh until weight is constant within ±0.5 mg;
keep the tare weight of the filter in file for
future use
Be sure the filters that arrived from the field
are handled and analyzed whenever possible by the
same person who started the project—the person
who tared the filters before sampling; use the
same balance
(continued)
-------
(continued)
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 14 of 17
7. Perform step #2, and then uncover the filter con-
tainer and visually examine the filter to see if
it is torn; write down all observations that you
think will help justify the final data
8. Desiccate the filter for 24 h, and weigh it to the
nearest 0.1 mg; record the weight then desiccate
again for 6 h, and reweigh; the difference be-
tween the two recorded weights should be within
±0.5 mg; the balance should be zeroed and checked
with a 0.500-g Class-S weight, and the relative
humidity must be <50%
9. Continue the processes of desiccating and weighing
until consistent data are obtained; however, after
the third trial, if no satisfactory data are
obtained, confer with the supervisor
Notes
1. When weighing the filter and sample, be sure to
use a clean brush and to add all particulates or
pieces of the filter that might be left in the con-
tainer
2. Be sure to use tweezers to handle the filters;
never hold them directly with your hand
3. Write down the date and time each time a filter
is weighed
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 15 of 17
PROCEDURE FOR ANALYSIS OF ACETONE RINSE SAMPLES
(Method 5, Figure 5.6)
Status
I. Preparing Containers for Shipment
1. Select the appropriate size and number of bottles
to be shipped to the field; include extra bottles
2. Clean the bottles and caps thoroughly with soap
detergent, rinse with tap water, and then rinse at
least twice with deionized distilled water
3. Rinse the clean bottles with acetone to get rid of
most of the water; remember that one batch of
acetone could be used for more than one container
4. Check the containers and the caps individually
after they are dry to be sure no detergent or
other contaminant is present; tightly cap all
containers
II. Handling and Analysis of Acetone Rinse Samples
Important; Blanks and samples should have identical ana-
lytical treatments; never handle with bare hands any ana-
lysis glassware once tared; always use tongs or disposable
gloves
1. Log the samples received from the field, and check
each container for leakage; if the sample volume
level is marked on the container, check to see if
the sample still matches the level, if not, write
a note of that
2. Use a dry, clean glass funnel to transfer the
acetone rinse into the dry, clean 250-ml graduated
cylinder
3. Record the volume of the sample to the nearest
1.0 ml, and transfer it into a dry, clean, tared
(to the nearest 0.1 mg) 250- or 300-ml beaker,
depending on the volume of the sample; add 50 ml
to the recorded sample volume to account for the
acetone rinse of all containers
(continued)
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 16 of 17
(continued)
Status
4.
Rinse the container with two 25-ml portions of
acetone (reagent grade); cap the container, and
shake very gently; transfer the acetone rinse into
the graduated cylinder to rinse it, and then pour
the rinse through the funnel into the beaker that
contains the sample; thus, the container, the
graduated cylinder, and the funnel have been
rinsed
5. Repeat steps 3 and 4 for each sample
6. Let the samples and blanks dry at room temperature
in a dust-free environment or under a watchglass
7. Weigh a clean, empty dry beaker, and place it in
the same atmosphere where the samples are drying
to find out if there was any particulate collected
on the samples from the surroundings while drying
(not mandatory)
8. Transfer the totally evaporated samples and blanks
along with the empty beaker into a tightly sealed
desiccator that contains dry anhydrous calcium
sulfate (CaSO4)
9. Desiccate for 24 h
10. Zero the balances and check the accuracy with a
100-g Class-S standard weight prior to weighing;
the reading should be 100 g ±0.5 mg, and the re-
lative humidity in the balance room should be £50%
11. Weigh the samples, blanks, and empty beaker to the
nearest 0.1 mg
It is very important to:
a. Keep the desiccator tightly closed while weighing
b. Remove the samples to be weighed from the desicca-
tor one at a time, weigh each, and put each imme-
diately back into the desiccator
c. Keep the weighing time <2 min
(continued)
-------
Section No. 3.4
Revision No. 0
Date January 15, 1980
Page 17 of 17
(continued)
Status
d.
e.
12.
13.
14.
15
Be sure that both sides of the balance are closed
when weighing
Turn all balance knobs to zero after the weighings
Record the weights of the samples, blanks, and
empty beaker; record the date and time, each time
a sample is weighed
Desiccate the samples, blanks, and empty beaker
for >_6 h; data on the first and second weighings
should agree within ±0.5 mg; if not, desiccate
again for 6 h and reweigh until consistent data
are obtained; after the third trial, consult the
supervisor
If there is >2 mg change in the weight of the
empty beaker, note it on the analytical data form
Calculate the data recorded on the data forms
(Figures 5.3 and 5.4) provided for this analysis
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 1 of 15
1.0 PROCUREMENT OF APPARATUS AND SUPPLIES
A schematic of the sampling train used in Method 5 is shown
in Figure 1.1. Commercial models of this train are available.
For those who want to build their own, construction details are
o
in APTD -0581 ; allowable modifications are described in the
following sections.
The operating, maintenance, and calibrating procedures for
4
the sampling train are in APTD-0576 . Since correct usage is
important in obtaining valid results, all users are advised to
read this document and adopt its procedures unless alternatives
are outlined herein.
In this section, applicable specifications, criteria, and/or
design features are given to aid in the selection of equipment
which assures good quality data collection. Procedures and
limits (where applicable) for acceptance checks are given.
During the procurement of equipment and supplies, it is sug-
gested that a procurement log (Figure 1.2) be used to record the
descriptive title of the equipment; the identification number, if
applicable; and the results of acceptance checks. An example of
a procurement log is shown in Figure 1.2, and a blank copy of the
log is in Section 3.4.12 for the convenience of the handbook
user. If calibration is required as part of the acceptance
r-^r-u -t-v-o r^ata arp t.o be recorded in a calibration log. Table
1.1 at the end of this section is a summary of the quality assur-
ance activities for the procurement and acceptance of apparatus
and supplies.
1.1 Sampling Apparatus
1.1.1 Probe Liner - The sampling probe should be constructed of
borosilicate (Pyrex) or quartz glass tubing with an outside
diameter (OD) of about 16 mm (0.625 in.), encased in a stainless
steel sheath with an OD of 25.4 mm (1.0 in.). Whenever practi-
cal, every effort should be made to use the borosilicate or
quartz glass liners; alternatively, metal seamless liners of 316
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 2 of 15
fi
•H
(0
in
O
£l
-p
cu
S
o
-H
-P
Q)
Jl
o
en
Q)
tn
•H
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 3 of 15
0
Pk
CO
• H
O
01
4->
0)
a
0)
W H
CO
o
u
01
u
01
PS
TJ
(-1
M
1
v)
5
O
-O
.^^
J*"*
Of
1 — ^
.^^^
cX>
rW
•J*
**^^>
f^"
3
JL
I
o-
"ji.
l/\
A
^V
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 4 of 15
stainless steel, Incoloy 825, or other corrosion resistant
metals may be used if approved by the administrator.
A heating system is required which will maintain an exit gas
temperature of 120° ±14°C (248° ±25°F) during sampling. Other
temperatures may be specified by a subpart of the regulations and
must be approved by the administrator for a particular applica-
tion. Since the actual probe outlet temperature is not usually
monitored during sampling, probes constructed in accordance to
APTD-0581 and utilizing the calibration procedures in APTD-05764
will be acceptable.
Either borosilicate or quartz glass liners may be used for
stack temperatures up to about 480°C (900°F), but quartz glass
liners must be used from 480° to 900°C (900° to 1650°F). Either
type of liner may be used at higher temperatures for short times
periods, with administrator approval. However, the absolute
upper limits—the softening temperatures of 820°C (1508°F) and
1500°C (2732°F)--for borosilicate and quartz respectively must be
observed.
Upon receiving a new probe, the user should visually check
it for specifications: that is, is it the length and composition
ordered? The probe should be visually checked for breaks or
cracks, and it should be checked for leaks on a sampling train
(Figure 1.1). This includes a proper nozzle to probe connection
with a Viton-O-ring Teflon ferrales or asbestos string. The
probe heating system should be checked as follows:
1. Connect the probe with a nozzle attached to the inlet
of the pump.
2. Electrically connect and turn on the probe heater for 2
or 3 min. The probe should become warm to the touch.
3. Start the pump and adjust the needle valve until a flow
rate of about 0.02 m3/min (0.75 ft3/min) is achieved.
4. Be sure the probe remains warm to the touch and the
heater is capable of maintaining the exit air temperature at a
minimum of 100°C (212°F). If it cannot, the probe should be
repaired, returned to the supplier, or rejected.
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 5 of 15
1.1.2 Probe Nozzle - The probe nozzle should be designed with a
sharp, tapered leading edge and constructed of either seamless
316 stainless steel tubing or glass, formed in a button-hook or
elbow configuration. The tapered angle should be <_30°, with the
taper on the outside to preserve a constant inside diameter (ID).
A range of nozzle ID's—for example, 0.32 to 1.27 cm (0.125
to 0.5 in.)—in increments of 0.16 cm (0.0625 in.) should be
available for isokinetic sampling. Larger nozzle sizes may be
required if high volume sampling trains are used or if very low
flows are encountered.
Upon receipt of the nozzle from the manufacturer, the user
should inspect it for roundness and for damage to the tapered
edge such as nicks, dents, and burrs. The diameter should be
checked with a micrometer; calibration procedures are described
in Section 3.4.2. A slight variation from exact sizes should be
expected due to machining tolerances. Each nozzle should be
engraved with an identification number for inventory and cali-
bration purposes.
1.1.3 Fitot Tube - The pitot tube, preferably of Type S design,
should meet the requirements of Method 2, Section 3.1.2. The
pitot tube is attached to the probe as shown in Figure 1.1. The
proper pitot tube-sampling nozzle configuration for prevention of
aerodynamic interference is shown in Figures 2.6 and 2.7 of
Method 2, Section 3.1.2.
The pitot tube should be visually inspected for both verti-
cal and horizontal tip alignments. If the tube is purchased as
an integral part of a probe assembly, the dimensional clearances
should be checked using Figures 2.6 and 2.7. Repair or return
any pitot tube which does not meet specifications. Calibration
procedure for a pitot tube is covered in Section 3.4.2.
1-1-4 Differential Pressure Gauge - The differential pressure
gauge should be an inclined manometer or the equivalent as speci-
fied in Method 2, Section 3.1.2. Two gauges are required. One
is utilized to monitor the stack velocity pressure, and the other
to measure the orifice pressure differential.
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 6 of 15
Initially, check the gauge against a gauge-oil manometer at
a minimum of three points: 0.64 mm (0.025 in.); 12.7 mm
(0.5 in.); and 25.4 mm (1.0 in.) H-O. The gauge should read
within 5% of the gauge-oil manometer at each test point. Repair
or return to the supplier any gauge which does not meet these
requirements.
1.1.5 Filter Holder - A filter holder of borosilicate glass with
a glass or stainless steel mesh frit filter support and a sili-
cone rubber gasket is required by the Reference Method. Other
gasket materials (e.g., Teflon or Viton) may be used if ap-
proved by the administrator. The holder design must provide a
positive seal against leakage from the outside or around the fil-
ter. The holder should be durable, easy to load, and leak free
in normal applications. It is positioned immediately following
the probe, with the filter placed toward the flow.
1.1.6 Filter Heating System - Any heating system may be used
which is capable of maintaining the filter holder at 120° ±14°C
(248° ±25°F) during sampling. Other temperatures may be speci-
fied ,by a subpart of the regulations or approved by the admini-
strator for a particular application. A gauge capable of
measuring temperatures to within 3°C (5.4°F) should be provided
to monitor the temperature around the filter during sampling.
Before sampling, the heating system and the temperature
monitoring device should be checked. It is desireable that the
heating element be easily replaceable in case of a malfunction
during sampling.
1.1.7 Condenser - Four impingers should be connected in series
with leak-free ground-glass fittings or any similar noncontami-
nating fittings. The first, third, and fourth impingers must be
the Greenburg-Smith design modified by replacing the inserts with
a glass tube that has an unconstricted 13-mm (0.5-in.) ID and
that extends to within 13 mm (0.5 in.) of the flask bottom. The
second impinger must be a Greenburg-Smith with the standard tip
and plate. Modifications—for example, using flexible connec-
tions between impingers, using materials other than glass, or
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 7 of 15
using a flexible vacuum hose to connect the filter holder to the
condenser—may be used if approved by the administrator. The
fourth impinger outlet connection must allow insertion of a
thermometer capable of measuring ±1°C (1.8°F) of true value in
the range of 0° to 25°C (32° to 77°F).
Alternatively, any system that cools the gas stream and
allows measurement of the condensed water and the water vapor
leaving the condenser, each to within 1 ml or 1 g, may be used
with approval from the administrator.
Upon receipt of a standard Greenburg-Smith impinger, the
user should fill the inner tube with water. If the water does
not drain through the orifice in 6 to 8 s or less, the impinger
tip should be replaced or enlarged to prevent an excessive pres-
sure drop in the sampling system. Each impinger should be
checked visually for damage—breaks, cracks, or manufacturing
flaws such as poorly shaped connections.
1.1.8 Metering System - The metering system should consist of a
vacuum gauge, a vacuum pump, thermometers capable of measuring
±3°C (5.4°F) of true value in the range of 0 to 90°C (32° to
194°F), a dry gas meter with 2% accuracy at the required sampling
rate; and related equipment as shown in Figure 1.1. Other meter-
ing systems capable of maintaining sampling rates within 10% of
isokinetic and determining sample volumes to within 2% may be
used if approved by the administrator. Sampling trains with
metering systems designed for sampling rates higher than that
described in APTD-05813 and APTD-05764 may be used if the above
specifications can be met.
When the metering system is used witf\ a pitot tube, the
system should permit verification of an isokinetic sampling rate
through the use of a nomograph or by calculation.
Upon receipt or after construction of the equipment, the
user should perform both positive and negative pressure leak
checks before beginning the system calibration procedure
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 8 of 15
described in Subsection 2.1 of Section 3.4.2. Any leakage re-
quires repair or replacement of the malfunctioning item.
1.1.9 Barometer - A mercury, aneroid, or other barometer capable
of measuring atmospheric pressure to within ±2.5 mm (0.1 in.) Hg
is required.
A preliminary check of a new barometer should be made
against a mercury-in-glass barometer or the equivalent. In lieu
of this, the absolute barometric pressure may be obtained from a
nearby weather service station and adjusted for elevation dif-
ference between the station and the sampling point. Either
subtract 2.5 mm Hg/30 m (0.1 in. Hg/100 ft) from the station
value for an elevation increase or add the same for an elevation
decrease. If the barometer cannot be adjusted to agree within
2.5 mm (0.1 in.) Hg of the reference barometric pressure, it
should be returned to the manufacturer or rejected.
1.1.10 Gas Density Determination Equipment - A temperature sen-
sor and a pressure gauge as described in Method 2 (Section 3.1.2)
are required. Additionally, a gas analyzer as described by
Method 3 may be required.
It is preferable that the temperature sensor be permanently
attached to either the probe or the pitot tube. In either case,
it is recommended that a fixed configuration (Figure 1.1) be
maintained. Alternatively, the sensor may be attached just prior
to field use as described in Section 3.4.2.
1.2 Sample Recovery Apparatus
1.2.1 Probe Liner and Nozzle Brushes - Nylon bristle brushes
with stainless steel wire handles are recommended. The probe
brush must be at least as long as the probe. A separate,
smaller, and very flexible brush should be used for the nozzle.
1.2.2 Wash Bottles - Two 500-ml wash bottles are recommended for
probe and glassware rinsing. Glass bottles are preferred, but
polyethylene is acceptable; however, if polyethylene is used, it
is recommended that it not be used for acetone storage for longer
than a month.
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 9 of 15
1.2.3 Sample Storage Containers - Recommended are 500- or
1000-ml chemically resistant, borosilicate glass bottles for
storage of acetone rinses. The bottles must have leak-proof
screw caps with leak-proof, rubber-backed Teflon cap liners, or
they must be constructed to preclude leakage and to resist
chemical attack. Wide-mouthed bottles are easiest to use, but
narrow mouth bottles are less prone to leakage. As an alterna-
tive to glass, polyethylene bottles may be used, but storage
times should be minimized.
Prior to field use, the cap seals and the bottle cap seating
surfaces should be inspected for chips, cuts, cracks, and manu-
facturing deformities which would allow leakage.
1.2.4 Petri Dishes - Glass or polyethylene petri dishes are
recommended for storage and for transportation of the filter and
collected sample.
1.2.5 Graduated Cylinder and/or Triple Beam Balance - Either a
graduated cylinder or a triple beam balance may be used to
measure the water condensed in the impingers during sampling.
Additionally, the graduated cylinder may be used to measure water
initially placed in the first and second impingers. In either
case, the required accuracy is 1 ml or 1 g; therefore, the
cylinder must have subdivisions <_2 ml. Most triple beam balances
are capable of weighing to the nearest 0.1 g.
142.6 Plastic Storage Containers - Several airtight plastic
containers are required for storage of silica gel.
1 .2.7 Funnel and Rubber Policeman - A funnel and rubber police-
.i.ji are needed to transfer the used silica gel from the impinger
to a storage container unless silica gel is weighed in the field
after the test. A Teflon policeman is helpful for recovery of
the filter.
1.3 Analytical Equipment
1.3.1 Glassware - Borosilicate glass dishes should be used to
facilitate filter weighing. A 250-ml glass beaker is required
for evaporation of the acetone rinse.
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 10 of 15
1.3.2 Balances - Two balances are required. One should be
analytical grade and capable of weighing the filter and the
sample beaker to within ±0.1 mg. The other should be as described
in Subsection 1.2.5.
1.4 Reagents and Other Supplies
All reagents should meet specifications established by the
Committee on Analytical Reagents of the American Chemical
Society (ACS). If reagents that meet these specifications are
not available or if other specifications are not given, use the
best grade available.
1.4.1 Sampling -
Filters - Glass fiber filters without organic binders must
be used. The filters must exhibit at least 99.95% collection
efficiency of a 0.3-|j dioctyl phthalate smoke particle, in ac-
cordance with ASTM standard method D2986 -71. Manufacturer's
quality control test data are sufficient for validation of ef-
ficiency.
Silica Gel - Use indicating type 6-16 mesh. If previously
used, dry at 175°C (347°F) for at least 2 h before reuse. New
silica gel may be used as received.
Water - When material collected by the impingers is to be
analyzed, distilled water must be used. A water blank should be
analyzed before field use to prevent false high values on test
samples. For standard particulate sampling, distilled water is
recommended, but not required.
Crushed Ice - Enough crushed ice is needed to maintain the
exit temperature of the silica gel impinger or condenser at <20°C
(68°F) throughout the test period.
Stopcock Grease - An acetone insoluble, heat stable, sili-
cone grease must be used when the sealing of ground-glass connec-
tions is required. This is not necessary if screw-on connectors
with Teflon sleeves are used.
1.4.2 Sample Recovery - Reagent ACS grade acetone with £0.001%
residue in glass bottles must be used. Acetone supplied in metal
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 11 of 15
containers is unacceptable due to the prevalently high residue
levels. An acetone blank should be run prior to field use, and
the acetone must be rejected if blank residue weight is >0.001%
of the total acetone weight.
1.4.3 Sample Analysis -
Acetone - Same as Subsection 1.4.2.
Desiccant - An indicating type anhydrous calcium sulfate is
required. Other types of desiccants may be used if approved by
the administrator.
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 12 of 15
Table 1.1 ACTIVITY MATRIX FOR PROCUREMENT OF APPARATUS
AND SUPPLIES
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Sampling
Probe liner
Specified material of
construction; equipped
with heating system
capable of maintaining
120° ± 14°C (248° ±
25°F) at the exit
Visually check and
run the heating
system
Repair, return
to supplier, or
reject
Probe nozzle
Stainless steel (316)
with sharp, tapered
angle <30°; differ-
ence in measured diam-
eters <0.1 mm (0.004
in.); no nicks, dents,
or corrosion (Subsec
1.1.2)
Visually check before
each test; use a mi-
crometer to measure
ID before field use
after each repair
Reshape and
sharpen, return
to the supplier,
or reject
Pitot tube
Type S (Sec 3.1.2);
attached to probe with
impact (high pressure)
opening plane even with
or above nozzle entry
plane
Calibrated according
to Sec 3.1.2
Repair or return
to supplier
Differential
pressure
gauge
(manometer)
Meets criteria (Sec
3.1.2); agree within
5% of gauge-oil
manometer
Check against a gauge-
oil manometer at a
minimum of 3 points:
0.64(0.025); 12.7
(0.5); 25.4(1.0) mm
(in.) H20
Repair or return
to supplier
Vacuum gauge
0-760 mm (0-30 in.) Hg
range, ±25 mm (1 in.)
at 380 mm (15 in.) Hg
Check against mer-
cury U-tube manometer
upon receipt
Adjust or return
to supplier
Vacuum pump
(continued)
Leak free; capable of
maintaining a flow
rate of 0.02-0.03
ms/min (0.66 to 1.1
ft3/min) for pump
inlet vacuum of 380 mm
(15 in.) Hg
Check upon receipt
for leaks and capaci-
ty
Repair or return
to supplier
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 13 of 15
Table 1.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Orifice meter
AH@ of 46.74 ± 6.35 mm
(1.84 ± 0.25 in.) HO
at 68°F (not mandatory)
Upon receipt, visual-
ly check for damage
and calibrate against
wet test meter
Repair if pos-
sible otherwise
return to sup-
plier
Impingers
Standard stock glass;
pressure drop not ex-
cessive (Subsec 1.1.7)
Visually check upon
receipt; check pres-
sure drop (Subsec
1.1.6)
Return to sup-
plier
Filter holder
Leak free; borosilicate
glass
Visually check before
use
As above
Dry gas meter
Capable of measuring
volume within ±2% at a
flow rate of 0.02
m /min (0.75 ftj/min)
Check for damage upon
receipt and calibrate
(Sec 3.4.2) against
wet test meter
Reject if damaged,
behaves erratic-
ally, or cannot be
properly adjusted
Thermometers
±1°C (2°F) of true
value in the range of
0° to 25°C (32° to 77°F)
for impinger thermometer
and ±3°C (5.4°F) of true
value in the range of
0°C to 90°C (32° to
194°F) for dry gas
meter thermometers
Check upon receipt
for dents or bent
stem, and calibrate
(Sec 3.4.2) against
mercury-in-glass
thermometer
Reject if unable
to calibrate
Barometer
Capable of measuring
atmospheric pressure
within ±2.5 mm (0.1
in.) Hg
Check against a mer-
cury-in-glass barom-
eter or equivalent;
calibrate (Sec 3.1.2)
Determine correc-
tion factor, or re-
ject if difference
more than ±2.5
mm (0.1 in.) Hg
Sample Recovery
Probe liner and
nozzle
Nylon bristles with
stainless steel stem;
as long as the probe;
properly sized and
shaped
Visually check for
damage upon receipt
Replace or return
to supplier
Wash bottles
Two; polyethylene or
glass; 500 ml
Visually check for
damage upon receipt
Replace or return
to supplier
(continued)
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 14 of 15
Table 1.1 (continued)
Apparatus
Storage con-
tainer
Graduated
cylinder
Funnel
Rubber police-
man
Petri dishes
Balance
Beakers and
weighing
dishes
Triple beam
balance
Analytical
balance
Filters
Acceptance limits
Polyethylene or glass;
500 or 1000 ml
Glass and class A;
250 ml with subdivi-
sions <2 ml
Glass suitable for use
with sample bottles
Properly sized
Glass or polyethylene;
sized to fit the glass
fiber filters
Capable of measuring
silica gel to ±0.5 g
Glass
500-g capacity; cap-
able of measuring with-
in ±1 g
Capable of measuring to
±0.1 mg
Glass fiber without
organic binder; 99.95%
collection efficiency
for 0.3 |J dioctyl
phthalate smoke
particles
Frequency and method
of measurements
Visually check for
damage upon receipt
Upon receipt, check
for stock number,
cracks, breaks, and
manufacturer flaws
Visually check for
damage upon receipt
Visually check for
damage upon receipt
Visually check for
damage upon receipt
Check with standard
weights upon receipt
and before each use
Upon receipt, check
for stock number,
cracks, breaks, and
manufacturing flaws
Check with standard
weights upon receipt
and before each use
As above
Manufacturer's guar-
antee that filters
were tested according
to ASTM D2986-71; ob-
serve under light
for defects
Action if
requirements
are not met
Replace or return
to supplier
Replace or return
to supplier
Replace or return
to supplier
Replace or return
to supplier
Replace or return
to supplier
Replace or return
to manufacturer
Replace or return
to manufacturer
Replace or return
to manufacturer
As above
Return to supplier
(continued)
-------
Section No. 3.4.1
Revision No. 0
Date January 15, 1980
Page 15 of 15
Table 1.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Reagents
Silica gel
Indicating type 6-16
mesh
Upon receipt, check
label for grade or
certification
Return to supplier
Distilled water
Meets ASTM D1193-74;
type 3 (only when
impinger particulate
catch included)
Check each lot, or
specify type when or-
dering
Replace or return
to manufacturer
Stopcock grease
Acetone insoluble, heat
stable silicone grease
Upon receipt, check
label for grade or
certification
Replace or return
to manufacturer
Acetone
ACS grade; <0.001%
residue in glass
bottles
Upon receipt, verify
residue by evaporat-
ing a blank sample
Replace or return
to supplier
Desiccant
Indicating type anhy-
drous calcium sulfate
Upon receipt, check
for grade and certi-
fication
Replace or return
to supplier
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 1 of 22
2.0 CALIBRATION OF APPARATUS
Calibration of apparatus is one of the most important func-
tions in maintaining data quality. The detailed calibration
procedures included in this section are designed for the equip-
ment specified by Method 5 and described in the previous section.
A laboratory log book of all calibrations must be maintained.
Table 2.1 at the end of this section summarizes the quality
assurance activities for calibration.
2.1 Metering System
2.1.1 Wet Test Meter - Wet test meters are calibrated by the
manufacturer to an accuracy of +0.5%. The calibration of the wet
test meter must be checked initially upon receipt and yearly
3
thereafter. A wet test meter with a capacity of 3.4 m /h (120
ft3/h) will be needed to calibrate the dry gas meter. For large
wet test meters (>3£/rev), there is no convenient method for
checking the calibration; for this reason, several methods are
suggested, and other methods may be approved by the administra-
tor. The initial calibration may be checked by any of the fol-
lowing methods:
1. Certification from the manufacturer that the wet test
meter is within +1% of true value at the wet test meter dis-
charge, so that only a leak check of the system is then required.
2. Calibration by any primary air or liquid displacement
method that displaces at least one complete revolution of the
wet test meter.
3. Comparison against a smaller wet test meter that has
previously been calibrated against a primary air or liquid dis-
placement method, as described in Section 3.5.2.
4. Comparison against a dry gas meter that has pre-
viously been calibrated against a primary air or liquid
displacement method.
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 2 of 22
The calibration of the test meter should be checked annual-
ly. The calibration check can be made by the same method as that
of the original calibration; however, the comparison method need
not be recalibrated if the calibration check is within +1% of the
true value. When this agreement is not obtained, the comparison
method or wet test meter must be recalibrated against a primary
air or liquid displacement method.
2.1.2 Sample Meter System - The sample meter system—consist-
ing of the pump, vacuum gauge, valves, orifice meter, and dry
gas meter--should be initially calibrated by stringent laboratory
methods before it is used in the field. After the initial
acceptance, the calibration should be rechecked after each field
test series. This recheck is designed to provide the tester with
a method that can be used more often and with less effort to
ensure that the calibration has not changed. When the quick
check indicates that the calibration factor has changed, the
tester must again use the complete laboratory procedure to
obtain the new calibration factor. After recalibration, the
metered sample volume must be multiplied by either the initial
or the recalibrated calibration factor—that is, the one that
yields the lower gas volume for each test run.
Before initial calibration of the metering system, a leak
check should be conducted. The meter system should be leak
free. Both positive (pressure) and negative (vacuum) leak
checks should be performed. Following is a pressure
leak-check procedure that will check the metering system from
the quick disconnect inlet to the orifice outlet and will
check the orifice-inclined manometer:
1. Disconnect the orifice meter line from the
downstream orifice pressure tap (the one closest to the
exhaust of the orifice), and plug this tap (Figure 2.1).
2. Vent the negative side of the inclined manometer to
the atmosphere. If the inclined manometer is equipped with a
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 3 of 22
three-way valve, this step can be performed by merely turning
the three-way valve that is on the negative side of the
orifice-inclined manometer to the vent position.
3. Place a one-hole rubber stopper with a tube through
its hole in the exit of the orifice, and connect a piece of
rubber or plastic tubing to the tube, as shown in Figure 2.1.
4. Open the positive side of the orifice-inclined
manometer to the "reading" position; if the inclined manometer
is equipped with a three-way valve, this will be the line
position.
5. Plug the inlet to the vacuum pump. If a quick
disconnect with a leak-free check valve is used on the control
module, the inlet will not have to be plugged.
6. Open the main valve and the bypass valve.
7. Blow into the tubing connected to the end of the
orifice until a pressure of 127 to 178 mm (5 to 7 in.) H-O has
built up in the system.
8. Plug or crimp the tubing to maintain this pressure.
9. Observe the pressure reading for a 1-min period. No
noticeable movement in the manometer fluid level should occur.
If the meter box has a leak, a bubbling-type leak-check
solution may aid in locating the leak(s).
After the metering system is determined to be leak free by
the positive leak-check procedure, the vacuum system to and in-
cluding the pump should be checked by plugging the air inlet to
the meter box. If a quick disconnect with a leak-free stopper
system is presently on the meter box, the inlet will not have to
be plugged. Turn the pump on, pull a vacuum within 7.5 cm
(3 in.) Hg of absolute zero, and observe the dry gas meter. If
the leakage exceeds 0.00015 m3/min (0.005 ft3/min), the leak(s)
must be found and minimized until the above specifications are
satisfied.
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 4 of 22
g
0)
-P
to
>i
to
tn
0)
-P
0)
g
m
o
o
cu
u5
o
(0
(U
>
•d
-P
•rH
to
o
Oi
CN
0)
Mg"
£ S m
Hi
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 5 of 22
Leak checking the meter system before initial calibration
is not mandatory, but is recommended.
Note: For metering systems having diaphragm pumps, the
normal leak-check procedure described above will not detect
leakages within the pump. For these cases, the following
leak-check procedure is suggested: make a 10-min calibration
run at 0.00057 m3/min (0.02 ft3/min); at the end of the run,
take the difference between the measured wet test meter and the
dry gas meter volumes; divide the difference by 10, to get the
leak rate. The leak rate should not exceed 0.00057 m3/min (0.02
ft3/min).
Initial calibration - The dry gas meter and the orifice
meter can be calibrated simultaneously and should be calibrated
when first purchased and any time the posttest check yields a Y
outside the range of the calibration factor Y +0.05Y. A
calibrated wet test meter (properly sized, with +1% accuracy)
should be used to calibrate the dry gas meter and the orifice
meter.
The dry gas meter and the orifice meter should be
calibrated in the following manner:
1. Before its initial use in the field, leak check the
metering system. Leaks, if present, must be eliminated before
proceeding.
2. Assemble the apparatus, as shown in Figure 2.2, with
the wet test meter replacing the probe and impingers—that is,
with the outlet of the wet test meter connected to a needle
valve that is connected to the inlet side of the meter box.
3. Run the pump for 15 min with the orifice meter
differential (AH) set at 12.7 mm (0.5 in.) H20 to allow the
pump to warm up and to permit the interior surface of the wet
test meter to be wetted.
-------
AIR INLET
WET TEST METER
AIR OUTLET >-\~ ^-^Jc MATER OUT
ORIFICE
MANOMETER
Figure 2.2 Sample meter system calibration setup.
MATER
LEVEL
GAUGE
^d o £d co
fa fa fl> n>
iQ rt < O
tt> (D H- rt
cn H-
(^ C.H- O
m o a
O 3 n3
H,r a
NJ K o
M
•<: '
00
o •
vo
CO
o
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 7 of 22
4. Adjust the needle valve so that the vacuum gauge on
the meter box is between 50 and 100 mm (2 to 4 in.) Hg during
calibration.
5. Collect the information required in the forms
provided (Figure 2.3A or 2.3B). Sample volumes, as shown,
should be used.
6. Calculate Y. for each of the six runs, using the
equation in Figure 2.3A or 2.3B under the Y^ column, and record
the results on the form in the space provided.
7. Calculate the average Y (calibration factor) for the
six runs using the following equation:
V
_ Yl -
h Y2 '
h Y3 -
h Y4 -
h Y5 -
- Y6 .
Record the average on Figure 2.3A or 2.3B in the space provided.
8. Clean, adjust, and recalibrate, or reject the dry gas
meter if one or more values of Y fall outside the interval Y
+0.02Y. Otherwise, the average Y is acceptable and should be
used for future checks and subsequent test runs.
9. Calculate AH@. for each of the six runs using the
equation in Figure 2.3A or 2.3B under the AH@. column, and
record on the form in the space provided.
10. Calculate the average AH@ for the six runs using the
following equation:
AH@, + AH@0 + AH@, + AH@, + AH©,- + AH@A
AH@ - i ? ^ ^ $ '
Record the average on Figure 2.3A or 2.3B in the space provided.
11. Adjust the orifice meter or reject it if AH@^ varies
by more than +3.9 mm (0.15 in.) H20 over the range of 10 to
100 mm (0.4 to 4.0 in.) H20. Otherwise, the average AH@ is
acceptable and should be used for subsequent test runs.
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 8 of 22
Date
/7?
Barometric pressure, P, =
Meter box number
in. Hg Calibrated by
Orifice
manometer
setting
(AH),
-in. H20
0.5
1.0
1.5
2.0
3.0
4.0
Gas volume
Wet test
meter
(V )
fl3
5
5
10
10
10
10
Dry gas
meter
(vd),
ft3
/30.0OO
Temperatures
Wet test
meter
oF
?>/?
Dry gas meter
Inlet
(td),
i
OF
9;
Outlet
(td),
o
OF
*»«r
Avga
(td),
^
Time
(0),
min
iiy
Avg
Y.
i
/ 00**}
AH@
in. H2<
/•79
AH,
""-frti'-'
il>.
TT f\
n2o
Oc
. J
1.0
1.5
2.0
3.0
4.0
AH
13.6
Orto^o
0.0737
0.110
0.147
0.221
0.294
V P, (t, + 460)
v - w b a
1 TT CT> -t **" 'x ft- + /.f.n}
Vd(rb * 13. 6} (tw + 460)
6-<£*9< ^v^ fs-yjj
S-.WUrt.Lrt&J/.fT^
^
_, — —
™ _ 0.0317 m ["„ + 460> Sl
^"i - Pb (t * 460) V
Da L w J
ro,£>3n)tO,5) &3J.S?{'3.'7g^-] ^,
(,0e).<0^(5^fn [_ 5" I
If there is only one thermometer on the dry gas meter, record the temperature
under t,.
d
Figure 2.3A Dry gas meter calibration data (English units)
(front side)
-------
Nomenclature:
V = Gas volume passing through the wet test meter, ft
W
.3
V, = Gas volume passing through the dry gas meter, ft"
t = Temperature of the gas in the wet test meter, °F.
W
= Temperature of the inlet gas of the dry gas meter, °F.
and
i
t, = Temperature of the outlet gas of the dry gas meter, °F.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average t.
td , °F.
o
AH = Pressure differential across orifice, in. H-O.
Y- = Ratio of accuracy of wet test meter to dry gas meter for each run. Tolerance Y- =
Y ±0.02 Y. -1
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs.
Tolerance Y = Y ±0.01 Y.
o
AH@. = Orifice pressure differential at each flow rate that gives 0.75 ft /min of air at
standard conditions for each calibration run, in. H20. Tolerance = AH@ ±0.15
(recommended).
*"d O po en
3 fu (ii ID (D
AH@ = Average orifice pressure differential that gives 0.75 ft /min of air at standard VQ rt-o o
conditions for all six runs, in. H90. Tolerance = 1.84 ±0.25 (recommended). n n £"H-
•^ VD Q H- O
6 = Time for each calibration run, min. 033
P, = Barometric pressure, in. Hg. K5.° '
Figure 2.3A. Dry gas meter calibration data (English units). (backside)
00
o
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 10 of 22
Date
Barometric pressure, P, =
Meter box number
mm Hg Calibrated by
^:A/ir-
Orifice
manometer
setting
(AH),
mm H_0
10
25
40
50
75
100
Gas volume
Wet test
meter
(V )
3
m
0.15
0.15
0.30
0.30
0.30
0.30
Dry gas
meter
(vd),
3
m
^y^£
Temperatures
Wet test
meter
°C
J ^f
* Q
Dry gas meter
Inlet
(td),
i
°C
°/9
Outlet
(td),
o
°C
%
Avg"
(td),
°C
i G?
I &
Time
(6),
min
Jo^w
Avg
Y.
i
AH + ^^ ~\ f+ + ')~t'\\
d d 13.6 w
(O'/f)) t *736? )C o? ^/ -^
(£"'•5^X1'? "2>"7^C^ Cj/\
0.00117 AH r^w^73)0!2
^1Li P (t + 273) V .
P- °o/i~i Y/Ol ~" £>9^O o Soij1 I
( 73l,^f^£f~) O , /r^,3 _l
^ ' ^*— \
If there is only one thermometer on the dry gas meter, record the temperature
under t,.
d
Figure 2.3B Dry gas meter calibration data (metric units).
(front side)
-------
Nomenclature:
q
Vw = Gas volume passing through the wet test meter, m .
q
V^ = Gas volume passing through the dry gas meter, m .
t = Temperature of the gas in the wet test meter, °C.
t^ = Temperature of the inlet gas of the dry gas meter, °C.
i
t, = Temperature of the outlet gas of the dry gas meter, °C.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average of t, and
t °C "i
o
AH = Pressure differential across orifice, mm H20.
Y. - Ratio of accuracy of wet test meter to dry gas meter for each run. Tolerance Y. =
Y +0.02 Y. x
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs.
Tolerance Y = Y +0.01 Y.
AH@. = Orifice pressure differential at each flow rate that gives 0.021 m of air at standard
conditions for each calibration run, mm H90. Tolerance AH@. = AH@ +3.8 mm H?0
(recommended).
*~U C^ ?^ C/5
AH@ = Average orifice pressure differential that gives 0.021 m of air at standard con- $ rt < o
ditions for all six runs, mm H90. Tolerance AH@ = 46.74 +6.3 mm H90 (recommended). m n £"{?.
^ ^ M C| H-O
M (a O J3
0 = Time of each calibration run, mm. 30
o c 2;
t-h v&o
h( O •
NJ t< •
to (jo
P, = Barometric pressure, mm Hg.
Figure 2.3B Dry gas meter calibration data (metric units). (backside)
Ul
VD
OO
O
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 12 of 22
Posttest calibration check - After each field test series,
conduct a calibration check of the metering system, except for
the following variations:
1. Three calibration runs at a single intermediate orifice
meter setting may be used with the vacuum set at the maximum
value reached during the test series. The single intermediate
orifice meter setting should be based on the previous field test.
A valve must be inserted between the wet test meter and the inlet
of the metering system to adjust the vacuum.
2. If a temperature-compensating dry gas meter was used,
the calibration temperature for the dry gas meter must be within
+6°C (10.8°F) of the average meter temperature during the test
series.
3. Use Figure 2.4A or 2.4B, and record the required infor-
mation.
If the calibration factor Y deviates by <5% from the initial
calibration factor Y, then the dry gas meter volumes obtained
during the test series are acceptable. If Y deviates by >5%, re-
calibrate the metering system, and use whichever meter coeffi-
cient (initial or recalibrated) that yields the lowest gas volume
for each test run.
Alternate procedures (e.g., using the orifice meter coeffi-
cients) may be used, subject to the approval of the administra-
tor.
2.2 Temperature Gauges
2.2.1 Impinger Thermometer - The thermometer used to measure
temperature of the gas leaving the impinger train should initial-
ly be compared with a mercury-in-glass thermometer which meets
ASTM E-l No. 63C or 63F specifications. The procedure is as
follows:
1. Place both the reference thermometer and the test
thermometer in an ice bath. Compare readings after they stabi-
lize.
-------
4-
c
jj
/v
^-
.OJ
*c
Q
/V
^_
R
O
^3
\fi
fx^
"'x
(J^
'
X)
>H
4J
VI
4-1
oJ 01
T— 1 Vl
Pti Pi
^
1
N
I
u:
Vl
yj
^ -Q
oi a
43 3
£3
d ^j
01
X 4J
O 01
43 B
Vl M
01 OJ
4-> 00
S ^>
ll
Q
P
*""**^
'
""""•11^,^
rtx
\J
60
.
d
• H
^
^
oi r^
CO Oo
o f>
II
It*
cc
ft-
%
^
oT
w
CO
0)
Vl
u ft
01 U
43 -H
§ M
4-) I
W tM
01 OJ
H CO
•H
>-l
^
0
VD
•O
4-1
v — /
PH
U
J>
O
VO
+
.S
*
M
^
+
VO
•
CO
iH
43
PH
T)
^>
•r-l
c
r
S
U
^
00
d
•rl
I i
03 4-1
> 01
to
01 ~
•H cF
p. ^^
01
Vl
3
4-1
OJ
Vl
01
8-
01
H
01
r— 1
O
U
OJ
Vl
01
01
B
to
OJ
00
^1
ili
Q
4-1
CO
Ol
4-1
4-1
01
^
CO
OJ
00
fr
Q
4-1
CO
01
4J
01 oj
00
o) r-
s P
00
•
d
•H
d
•H
B
n
Vl TD O
01 4-1
K* ^-*
^
4_)
0) /-
/
IS
\
iH O
4-> TJ
3 4J
4-1 ^™"
01
'd 4J
r-l •»-
Vl I-
0)
4-1 4-1
a "~
Vl
Ol /-
/
\
•H
*
\
S P
0
/
h,
\ CO
o
pC4
O
>4
4J T3 4J
S >, "-1
Vl
0) /-
4_)
K
v CO
& 4
_)
4-> 01 >" 4-1
01
Vl
01
01 4-1
u oi
•H a
4-1 0
•H d
Vl oj
o a
a ^~
*,
00
d
•H f-
4-1 ^
4.) ^
0) ^-
CO
/
O
* c
* W
' d
•H
M
A
^
-K r
*^
^
S ^
v O
O ^
fj V;
tV TV
V ^
O ?N
*^ >J
~^C ^
JN
°o
0^
6
^
rT
~*~
CYs
VJ^
r~>
\
•if^
IS
rV^
n
oO
Of
1>
_
^** /*}
10^
cocta
o
fH
""^^
*^»
~*
^"**
»
S.
I
^
o
iH
O
iH
•
T3
4J
Vl
01
II T3
Q
^ a
Vl
rj
4-1
OJ
Vl
0)
81
01
01
43
-o
O
U
01
Vl
^
Vl
01
4-)
01
a
to
00
^^
Vl
^
01
d
o
Vl
D
Ol
a
o
01
^3
4-1
d
o
r-t
d
o
M
•H
01
Vl
01
4-1
I—I
OJ
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 13 of 22
•o
d
as
CO CO
4-1 4-1
4-1 4-1
vT vT
D 01
4-1
01
4-1
01
4-1
01
s
01
4^
^"1
00
o
Vl
4-1
00
d
•H
U)
M
OJ
ft
01
3
r- 1
o
^
M
CD
II
5
t>
4-1
1
co
PM
o
Vl
0)
4-1
01
4-1
01
4-1
4-1
01
S
01
43
d
•H
W
OJ
00
0)
4-1
4-H
O
Ol
Vl
a
OJ
Vl
01
!<
01
H
II
£
4-1
O
VI
01
4-1
I
(0
tfl
00
1
01
43
4-1
<4_|
o
U)
OJ
00
4-1
01
i— i
d
•H
01
43
4-1
O
Ol
Vl
4-1
Vl
01
0)
H
II
•H
TJ
O
01
4-1
01
W
tfl
00
-o
01
•^
4-1
O
CO
OJ
00
4-1
01
1— 1
4-1
O
01
43
4-1
4-1
O
Ol
S-l
a
4-1
OJ
Vl
01
flj
EH
II
O
*O
^— i
O
01
00
OJ
Vl
81
OJ
4-1
43
"O
01
d
•H
OJ
43
O
•v
Vl
0)
4-)
01
a
co
00
1?
-o
01
43
d
•H
CO
OJ
00
01
43
4-1
4-1
O
01
VI
a
4-1
03
Vl
01
Q
01
4-1
01
00
03
Vl
01
<
II
•o
4-1
O
CM
W
d
•H
«\
01
U
• H
4-1
•rl
Vl
O
CO
CO
o
VI
u
03
r— 1
03
•r-l
4_)
d
01
Vl
01
4-1
4-1
•r-l
01
Vl
S
CO
cu
Vl
PH
II
M
<]
VI
u
03
01
l-l
O
4-1
Vl
01
4-1
01
B
00
1
t?
T)
0
Vl
0)
4-1
Ol
a
4-1
CO
01
4-1
4-1
01
4-1
O
^
u
(H
jj
U
U
03
4-1
O
0
•H
4-1
Pj
II
•rt
>H
VJ
01
01
Vl
43
iH
iH
VI
0
4-1
VI
Ol
4-1
01
B
co
a
t?
-o
o
Vl
01
4-1
01
4_)
CO
01
4-*
H
O lO
o
>^"» •
o o
II
03
Vl 01
U
oi d
00 oj
OJ Vl
Vl 01
0) iH
> 0
II
>l
•
00
*
d
•H
•H
01
Vl
a
CO
CO
01
Vl
ft
u
•H
Vl
4-1
01
a
0
Vl
0)
m
II
43
PH
*
d
•H
B
M
rj
3
VI
d
o
• H
4-1
03
Vl
o
•H
r-l
(tj
u
4-1
o
01
(,-1
H
II
Q
ialibration form (English units
u
H
<2
e
n
*D
O^
Ku
• .
rrt
'U
-p
CO
*l
T-*
•p
to
o
W
(rf
^*
Oi
CD
3
U"
'•H
-------
1
~^_
•^
-S
f^->
A
p?
Q_
£
<0
"^
PS\
H
4->
4-> CO
d o)
CO 4->
r-l Ol
(X, S-l
P-I
V.
4^>
t
^v
^
1
t .
s-i cu
CU 43
43 |
d d
M
X 01
0 4-1
43 OJ
}_J
01 CO
4-) CO
01 00
2
J_|
£
.
fV1
.**
fsp**
^
Q
&0
Hi-(
PH
**•
*^_
01 ry"S
4-* fc-'
cO I
n
n
rC
-L
(^C
v i^
^T
^"^
rJd
1 ^
0)
S-l
d
CO
CO
OJ
$^1
W Cw
j^
OJ U
,0 -H
S • *-t
13 -P
C3 QJ
s
•P o
CO S-l
0) CO
H pq
•H
X
n
CM
-o
4-1
•_<
43
>s
•CO
r--
CM
+
h
h
p
5
to
?
i
CO
iH
•*.
•J
TD
•r-l
g
».
00
d
d -H
<_
cu
4-1
4-1
00
w
S
> oi S
CO
•H ©
PH *•»'
01
S-l
d
4-1
CO
S-|
0)
t
SI 1
vJJ
EH
O)
r— t
o
^
CO
CO
o
S-l
01
s
CO
CO
oo
E?
Q
4J
co
OJ
0)
IS
CO
CO
00
S1
n
4J
CO
01
4-1
4-1
OJ
Ss
S-l
01
D 4-1
CJ 0)
•H S
4-4 O
•r-( d
t-t CO
0 E
01 CO
00
CO /-
S-l
d
•H
s
N CJ
01 4-1
4J
OJ --
I—I
4J
d 4-
o *-
4^ /"
01
1— 1
d 4-
t—t ^~
i-l /^
01
4-> 4-
s
S-l
0) /-
4->
*
N
o
•0
)
^
„
s
•rl
)
J
•*
\
S c
1 0
^
»>
N CO
T3
Ol >
S-J
0) /-
4J
»%
N CO
3
0) >
s >-
*.
00
d
•H /-
4-1 ^
•p <
Ol v-
co
J
-o
> c
1 w
^ €
a
CJ
o
CJ
o
J
3
s
M
^\ "-C
V ^
f^N
V j>
i &!
^
^g
t^Tl
^ ift
K) 'v
<2JO
0^.
O"*"1
„
*^\
*r^
fs.
^"^
rr
h
jj
V*v
f J
"•
n
»
^o
f
^0
K
^^^
^^*
Q>
-rj
5^ ^s^
S^ >£,,
-7 ,
^cr*
fu ""*
0
CO
0
o
*—— 1
rO
\ • >
'
O
CO
O
0
CO
0
T
S-l
0)
II T3
tx d
01
S-l
4->
S-l
Ol
£3
OJ
4-1
OJ
43
O
u
(U
S-l
J-l
OJ
01
s
CO
CO
00
S-l
•o
OJ
4->
gj
o
S-l
OJ
4J
OJ
s
o
s
01
43
4-1
0)
d
o
1— 1
d
o
co
•H
Ol
S-l
01
43
^
4-1
r— 1
CO
CO co
S S
OJ 0)
•P 4->
01 OJ
S E
p us
w «j
CA
CO
o
II
S
T3
01
43
t~j
00
d
o
S-l
43
4-1
60
d
•H
co
CO
CO
ft
01
3
I— 1
o
CO
CO
o
II
TD
t>
CJ
o
S-l
OJ
4-1
01
s
!S
Ol
0)
s
CU
43
4-1
d
• H
co
cO
00
Ol
43
4-1
o
OJ
S-l
0
4_)
CO
S-l
01
i*
QJ
EH
II
s
CJ
o
•s
0)
4-1
01
s
m
tfl
60
•o
01
43
4-1
4-1
o
co
CO
00
4-1
OJ
1— 1
d
•rl
01
43
4-1
0
OJ
S-l
d
4-1
CO
SH
01
t
OJ
EH
II
T
CJ
o
vs
S-l
OJ
4-1
0)
60
0)
43
4-1
4-1
0
CO
CO
00
4-1
CU
r— 1
4-1
H
O
Ol
43
4-1
O
OJ
S-J
d
4-1
CO
S-l
43
CO 4->
OJ r-f
43 r^
4-1 • CO
d
>, d s-i
43 S-l O
4-1
OJ u s-i
d CO
co 01
4-> rl S
& 0
0 4-1
CO
S-l 01 60
CU 4-1
4-1 0) >>
OJ S S-l
S *^3
co
cfl O
CO • 60 4-1
n) O
M CN M
W >. oi
>> S-l 4-1
S-i d 13 O)
T3 -rl S
O
0) - 4J 4->
43 01 co
4-1 0 S-l 0)
•rl Ol 4-1
d 4-i P
•r-l
co
<0
00
0)
43
4-1
4-1
O
01
S-l
d
4-1
CO
S-l
01
ft
s
Ol
4-1
Ol
00
CO
S-l
01
<
II
T-,
4-1
•r-l
S-l
O
CO
co
o
S-l
CJ
CO
I— (
CO
•H
4-1
d
OJ
S-l
CU
4-1
4-1
•H
X)
0)
^j
CO
CO
OJ
S-l
CU
II
hjH
<3
Oi
s
4-1
CO
CU
4-1
4-1
OJ
4-1
O
^
CJ
CO
d
o
u
CO
4-1
O
O
•H
CO
II
•H
>H
4-1
OJ
4-1 >H
O IT)
O
£^> •
CJ O
CO + 1
S-4
d ^"*
CJ
CJ P
CO CO
CU
4-1 4-1
O 01
S-l
0 ft
•r-l
4-) II
CO
S-l OJ
CJ
o) d
00 CO
CO S-l
S-l OJ
Ol r-l
> 0
< p
II
^
t
00
w
•
d
•H
•V
Ol
s^
d
CO
co
cu
S-l
ft
o
•r-l
S-l
4_)
OJ
s
o
S-l
CQ
m
n
43
eu
d
•H
s
*,
d
d
d
o
•H
4-1
CO
S-l
43
•H
rH
CO
CJ
4-1
O
§
•H
H
II
©
meter calibration data form (metric units). M
VD
00
O
•P
CO
0)
4->
i i
O
PM
-A
hM
^^
•
(NJ
-.
i
M
r^
D^
i
..
t^4
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 15 of 22
2. Remove the thermometers from the bath and allow both to
come to room temperature. Again, compare readings after they
stabilize.
3. Accept the test thermometer if its reading agrees
within 1°C (2°F) of the reference thermometer reading at both
temperatures. If the difference is greater than ±1°C (2°F), the
thermometer should be adjusted and recalibrated until the crite-
ria are met, or it should be rejected.
2.2.2 Dry Gas Thermometers - The thermometers used to measure
the metered gas sample temperature should initially be compared
with a mercury-in-glass thermometer as above, using a similar
procedure.
1. Place the dial type or equivalent thermometer and the
mercury-in-glass thermometer in a hot water bath, 40° to 50°C
(104° to 122°F). Compare the readings after the bath stabilizes.
2. Allow both thermometers to come to room temperature.
Compare readings after thermometers stabilize.
3. Accept the dial type or equivalent thermometer if the
values agree within 3°C (5.4°F) at both points or if the temper-
ature differentials at both points are within ±3°C (5.4°F) and
the temperature differential is taped to the thermometer and
recorded on the pretest sampling check form (Figure 3.1).
4. Prior to each field trip, compare the temperature
reading of the mercury-in-glass thermometer at room temperature
with that of the meter system thermometer. The values or cor-
rected values should be within ±6°C (10.8°F) of one another, or
the meter thermometer should be replaced or recalibrated. Record
any temperature correction factors on Figure 3.1 or on a similar
form.
2.2.3 Stack Temperature Sensor - The stack temperature sensor
should be calibrated upon receipt or checked before field use.
Each sensor should be uniquely marked for identification. The
calibration should be performed at three points and then extra-
polated over the range of temperatures anticipated during actual
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 16 of 22
sampling. For the three point calibration, a reference ASTM
mercury-in-glass thermometer should be used.
The following procedure is recommended for calibrating stack
temperature sensors (thermocouples and thermometers) for field
use.
1. For the ice point calibration, form a slush from
crushed ice and liquid water (preferably deionized, distilled) in
an insulated vessel such as a Dewar flask.
Taking care that they do not touch the sides of the flask,
insert the stack temperature sensor into the slush to a depth of
at least 2 in. Wait 1 min to achieve thermal equilibrium, and
record the readout on the potentiometer. Obtain three readings
taken in 1-min intervals. Note: Longer times may be required to
attain thermal equilibrium with thick-sheathed thermocouples.
2. Fill a large Pyrex beaker with water to a depth >_4 in.
Place several boiling chips in the water, and bring the water to
a full boil using a hot plate as the heat source. Insert the
stack temperature sensor(s) in the boiling water to a depth of at
least 2 in., taking care not to touch the sides or bottom of the
beaker.
Alongside the sensor(s), an ASTM reference thermometer
should be placed. If the entire length of the mercury shaft in
the thermometer cannot be immersed, a temperature correction will
be required to give the correct reference temperature.
After 3 min, both instruments will attain thermal equilib-
rium. Simultaneously record temperatures from the ASTM reference
thermometer and the stack temperature sensor three times at 1-min
intervals.
3. For thermocouple, repeat Step 2 with a liquid that has
a boiling point (such as cooking oil) in the 150° - 250°C (300° -
500°F) range. Record all data on Figure 2.5. For thermometers,
other than thermocouples, repeat Step 2 with a liquid that boils
at the maximum temperature that the thermometer is to be used, or
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 17 of 22
Date 9 - 12. -
Thermocouple number TC-
Ambient temperature 2_\
Calibrator
3C Barometric pressure 2S.6~7 in. Hg
Reference: mercury-in-glass AsrM 3C
other
Reference
point
number
Source
(specify)
Reference
thermometer
temperature,
°C
Thermocouple
potentiometer
temperature ,
Temperature,
difference,
0°
/OO"
/ce
f'C.
re
/o/°c
O./Z,
Type of calibration system used.
3r(ref temp, °C + 273) - (test thermom temp, °C + 273)
Iref temp, °C + 273
Figure 2.5 Stack temperature sensor calibration data form.
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 18 of 22
place the stack thermometer and reference thermometer in a fur-
nace or other device to reach the required temperature. Note:
If the thermometer is to be used at temperatures higher than the
reference thermometers will record, the stack thermometer may be
calibrated with a thermocouple previously calibrated with the
above procedure.
4. If the absolute values of the reference thermometer and
thermocouple(s) agree within ±1.5% at each of the three calibra-
tion points, plot the data on linear graph paper and draw the
best-fit line to the three points or calculate the constants of
the linear equation using the least-square method. The data may
be extrapolated above and below the calibration points and cover
the entire manufacturer's suggested range for the thermocouple.
For the portion of the plot or equation that agrees within 1.5%
of the absolute reference temperature, no correction need be
made. For all other portions that do not agree within ±1.5% use
the plot or equation to correct the data.
If the absolute values of the reference thermometer and
stack temperature sensor (other than the thermocouple) agree
within ±1.5% at each of the three points, the thermometer may be
used over the range of calibration points for testing without
applying any correction factor. The data cannot be extrapolated
outside the calibration points.
2,3 Probe Heater
The probe heating system should be calibrated prior to field
A
use according to the procedure outlined in APTD-0576. Probes
3
constructed according to APTD-0581 need not be calibrated if the
4
curves of APTD-0576 are used.
2.4 Barometer
The field barometer should be adjusted initially and before
each test series to agree within ±2.5 mm (0.1 in.) Hg of the
mercury -in -glass barometer or with the station pressure value
reported by a nearby National Weather Service station and cor-
rected for elevation. The correction for elevation difference
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 19 of 22
between the station and the sampling point should be applied at
a rate of -2.4 mm Hg/30 m (-0.1 in. Hg/100 ft). Record the 're-
sults on the pretest sampling check form (Figure 3.1 of Section
3.4.3).
2.5 Probe Nozzle
Probe nozzles should be calibrated before initial use in the
field. Using a micrometer, measure the ID of the nozzle to the
nearest 0.025 mm (0.001 in.). Make three measurements using
different diameters each time, and obtain the average. The
difference between the high and the low numbers should not exceed
0.1 mm (0.004 in.). When nozzles become nicked, dented, or
corroded, they should be reshaped, sharpened, and recalibrated
before use. Each nozzle should be permanently and uniquely
identified. Figure 2.6 is an example of a nozzle calibration
data form.
2.6 Pitot Tube
The Type S pitot tube assembly should be calibrated using
the procedure outlined in Section 3.1.2 of Method 2.
2.7 Trip Balance
The trip balance should be calibrated initially by using
Class-S standard weights and should be within ±0.5 g of the
standard weight. Adjust or return the balance to the manufac-
turer if limits are not met.
2.8 Analytical Balance
The analytical balance should initially be checked with
Class-S weights, and the data should be recorded on an analytical
balance calibration log or on a similar form. The balances
should be adjusted to agree within ±2 mg of the Class-S weight,
or it should be adjusted or returned to manufacturer.
-------
r--r.-H.on No. 3.4.2
- vision No. 0
>it,e January 15, 1980
Page 20 of 22
Date
Calibrated by
Nozzle
identification
number
37
Nozzle Diameter3
D,,
mm (in. )
0,251
D2'
mm tm. )
0.ZS2L
V -
mm (in. )
a 253
AD,b
mm (in. )
0. 002
D C
avg
c?.ZSZ
where:
1 ? ^
J. , ^ , O ,
three different nozzles diamet'
diameter must be within (0.025
(in.); each
;1 in.
AD = maximum difference between an}
AD £(0.10 mm) 0.004 in.
.eters, mm (in. ),
D
avg
= average of D-, , D2, and D
Figure 2.6 Nozzle calibration date form.
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 21 of 22
Table 2.1. ACTIVITY MATRIX FOR CALIBRATION OF EQUIPMENT
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Wet test meter
Capacity >3.4 m /h
(120 ft /h); accuracy
within ±1.0%
Calibrate initially,
and then yearly
by liquid dis-
placement
Adjust until
specifications
are met, or
return to manu-
facturer
Dry gas meter
Y. = Y +0.02 Y
i —
Calibrate vs wet
test meter initially,
and when posttest
check exceeds
Y +0.05 Y
Repair, or re-
place and then
recalibrate
Thermometers
Impinger thermometer
+1°C (2°F); dry gas
meter thermometer
+3°C (5.4°F) over
range; stack tempera-
ture sensor ±1.5% of
absolute temperature
Calibrate each ini-
tially as a separate
component against a
mercury-in-glass
thermometer; then
before each field
trip compare each as
part of the train
with the mercury-in-
glass thermometer
Adjust; de-
termine a con-
stant correc-
tion factor;
or reject
Probe heating
system
Capable of maintaining
120° ±14°C (248° ±
25°F) at a flow rate of
20£/min (0.71 ft /min)
Calibrate component
initially by
APTD-0576; if con-
structed by APTD-
0581, or use
published calibra-
tion curves
Repair, or re-
place and then
reverify the
calibration
Barometer
+2.5 mm (0.1 in.) Hg of
mercury-in-glass barom-
eter
Calibrate initially
vs mercury-in-glass
barometer; check
before and after
each field test
Adjust to
agree with a
certified
barometer
Probe nozzle
Average of three ID
measurements of nozzle;
difference between high
and low <0.1 mm
(0.004 in.)
Use a micrometer to
measure to near-
est 0.025 mm (0.001
in.)
Recalibrate,
reshape, and
sharpen when
nozzle becomes
nicked, dented,
or corroded
(continued)
-------
Section No. 3.4.2
Revision No. 0
Date January 15, 1980
Page 22 of 22
Table 2.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Analytical
balance
±1 mg of Class-S
weights
Check with Class-S
weights upon receipt
Adjust or
repair
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 1 of 20
3.0 PRESAMPLING OPERATIONS
The quality assurance activities for presampling operations
are summarized in Table 3.1 at the end of this section. See
Section 3.0, of this Handbook for details on preliminary site
visits.
3.1 Apparatus Check and Calibration
A pretest check will have to be made on most of the sampling
apparatus. Figure 3.1 should be used to record the pretest
calibration checks. Figure 3.2 or a similar form is recommended
to aid the tester in preparing an equipment checklist, status
form, and packing list for Methods 1 through 8, Method 17, and
particle sizing.
3.1.1 Sampling Train - A schematic of the EPA Method 5 sampling
train is Figure 1.1. Commercial models of this system are
available. Each train must be in compliance with the specifica-
tions of the Reference Method, Section 3.4.10.
3.1.2 Probe and Nozzle - Clean the probe and the nozzle inter-
nally by brushing first with tap water, then with deionized dis-
tilled water, and finally with acetone; allow both to dry in the
air. In extreme cases, the probe liner can be cleaned with
stronger reagents. In either case, the objective is to leave the
probe liner free from contaminants. The probe's heating system
should be checked to see that it is operating properly. The
probe should be sealed at the inlet or tip and checked for leaks
at a vacuum of 380 mm (15 in. ) Hg, and the probe must be leak
free under these conditions.
3.1.3 Impingers, Filter Holder, and Glass Connectors - All
glassware should be cleaned first with detergent and tap water
and then with deionized distilled water. All glassware should be
visually inspected for cracks or breakage and then repaired or
discarded if defective.
3.1.4 Pump - The vacuum pump should be serviced as recommended
by the manufacturer, or every 3 mo, or upon erratic behavior
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 2 of 20
Date 9/^/79 Calibrated by
Meter box number F&'l AH@ / 8 ~?
Dry Gas Meter*
Pretest calibration factor Y /, O/3 (within ±2% of the
average factor for each calibration run).
Impinger Thermometer
Was a pretest temperature correction used? ____^_ yes ^ no
If yes, temperature correction (within ±3°C (5.4°F)
over range)
Dry Gas Meter Thermometers
Was a pretest temperature correction made? yes /\ no
If yes, temperature correction (within ±3°C (5.4°F) over
range)
Stack Temperature Sensor*
Was a stack temperature sensor calibrated against a reference
thermometer? >s yes _____ no
If yes, give temperature range with which the readings agreed
within ±1.5% of the reference values to K (°R)
Barometer
Was the pretest field barometer reading correct? X^ yes no
(within ±2.5 mm (0.1 in.) Hg of the mercury-in-glass barometer)
Nozzle*
Was the nozzle calibrated to the nearest 0.025 mm (0.001 in.)?
X yes no
*Most significant items/parameters to be checked.
Figure 3.1 Pretest sampling checks.
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 3 of 20
Client
Project manager
Date needed by
PN
Transport vehicle
Presurveyed by
Loaded by
1. General Pretest Checklist
Asbestos wrapping matt.rr'.al, roll
Auxiliary parts box
Balance, triple ct,i • ]. weights
Bucket
Calibration Data
Camera
Certificate of insi -.: <
Clamps
Carpenter
C-Clamps
Hose
Cleanup box
Clipboards
Clocks
Condenser, coil type
Containers
Size
Type
Conveyor stands
High
Low
Quantity
Ready
Loaded
Figure 3.2 General pretest preparation form.
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 4 of 20
Figure 3.2 (continued)
Data forms
Detector tubes
Type
Range
Electrical equipment
Adapters, multioutlet
Extension cords (length)
Lights
Filter holder
Glass, 3 in. glass frit
Glass, 3 in. s.s. frit
Gelman, 47 mm
Alundum thimble
Impactor (type)
Fire extinguisher
First-aid kit
Fuses for meter box
Glassware sets
EPA-5 w/cyclone
EPA-5 w/cyclone bypass
EPA-5 hotbox only
EPA-6 S02
EPA-8 sulfuric acid mist
EPA-13A fluoride
EPA-13B fluoride
Other
Quantity
Ready
Loaded
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 5 of 20
Figure 3.2 (continued)
Gloves
Work
Asbestos
Heaters
Catalytic
Electric
Hoist
Hotplate
Ice chest
Ladder
Manometers
Inclined/micro/magnehelix
0-0.25 in. H2
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 6 of 20
Figure 3.2 (continued)
Manifold kit with attachments
2-.fi. flask w/stoppers
0-36 in. Hq manometer
0-27 in Hq vacuum pump
Variac for probe heat
25 ft extension
cord
Orsat gas sampling apparatus
Probe (length)
Sample line
Condenser
Pump assembly
Bags
Orsat analyzer w/squeeze
bulb
small
large
Nitrogen cylinder w/valve
Fyrite sampler w/squeeze
bulb
Orsat and Fyrite reagents
CO.
£.
o.
CO
Probes (except NO )
A.
Stainless steel
2 ft
3 ft
4 ft
5 ft
Total
length
Gasket
Quantity
Ready
Loaded
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 7 of 20
Figure 3.2 (continued)
6 ft
8 ft
10 ft
14 ft
Glass tube
2 ft
3 ft
4 ft
5 ft
6 ft
8 ft
10 ft
14 ft
Method 17 and impactor
"Nozzles" w/caps
1/8 in.
3/16 in.
1/4 in.
5/16 in.
3/8 in.
7/16 in.
1/2 in.
Quantity
Ready
Loaded
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 8 of 20
Figure 3.2 (continued)
Nozzle calipers
Pipe wrench (large)
Pi tot tube type
Effective
length
2 ft
3 ft
4 ft
5 ft
6 ft
8 ft
10 ft
14 ft
Potentiometer
-160° to 2450°F
-150° to 1800°F
Pulley
Radios (2 -way)
Rags
Reagents
Acetone, gal
H00 (distilled), gal
Methylene chloride, gal
H?(X> (30%) pint
Isopropyl alcohol (80%) gal
H2S04 (concentrated)
Silica gel, Ibs
jars @ 200 g
Quantity
Ready
Loaded
(continued)
-------
Section No. 3.4.3
Revision No. 0 ,
Date January 15, 1980
Page 9 of 20
Figure 3.2 (continued)
Ropes
Size
Safety equipment
Glasses
Goggles
Hardhats
Respirators
Harness
Earplugs
Sample boxes
EPA 5 - hotbox only
EPA 5 - particulate
EPA 6 - SO,,
EPA 8 - sulfuric acid mist
EPA 13A - fluoride
EPA 13B - fluoride
Other
Sample box hook and straps
Impinger-umbilical cord connector
Standard
Hotbox only
Sample port cover
Sample containers
Glass jars, petri dishes, etc.
Sample shipping boxes
Screwjacks
Tape
Duct
Electrical
High temp glass
Quantity
Ready
Loaded
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 10 of 20
Figure 3.2 (continued)
Tape measures
0-8 ft
0-100 ft
Tarps
Test literature
Thermocouple
Effective length
2 ft
3 ft
4 ft
5 ft
6 ft
8 ft
10 ft
14 ft
Thermometer, dial type, long stem
50°-450°F
150°-750°F
200°-1000°F
Tie cord (spool)
Toolbox (additional to standard)
Circular saw
Drill and bits
Jigsaw
Hacksaw
Handsaw
Handtools
Quantity
Ready
Loaded
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 11 of 20
Figure 3.2 (continued)
Traverse board
Type
Tubing
Polyethylene
Tygon
Teflon
Stainless ste
Copper
Other
Umbilical cord
Standard
Length
Size
jel
Leng
Length
th
Quantity
Ready
Loaded
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 12 of 20
Figure 3.2 (continued)
Hotbox
Method 17 and impactor
Variacs
Warming cords
Weather gear
Jumpsuits
Rainsuits
Boots
Ski masks
Wood assortment
Quantity
Ready
Loaded
2. Source Test Analytical Cleanup Checklist
Ballpoint pens,
Barometer, calibrated
Beakers, 250 ml
Brush, balance
Nozzle
Probe 6 ft
10 ft
16 ft
Quantity
Standard
6
1
1
1
1
1
1
Additional
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 13 of 20
Figure 3.2 (continued)
Caps
Nozzle
Probe, screw type
Serum
Clamps
Hose
Pinch no. 12
Pinch no. 28
Tubing
Cleanup rack
Filter holders, standard
Hotbox
S02
Filter media
G.F. 47 mm
G.F. 3 in.
Paper, 3 in. Whatman
Impactor
Thimbles
Funnels, standard
Silica gel
Polyethylene
Glass wool
Graduated cylinders,
25 ml
50 ml
100 ml
250 ml
500 ml
Quantity
Standard
2
6
2
1 box-12
1 box-12
1
1
2
1
0
20
2
2
1
1 jar
1
1
1
2
1
Additional
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 14 of 20
Figure 3.2 (continued)
Guth bottles
Acetone
Spare
Water
Kimwipes
Knife
Labels
Marking pens (sharp, water resistant)
Parafilm, box
Pipe cleaners
Rubberbands
Pencils
Grease
Regular
Petri dishes, 3 in.
Pipette bulbs
Pipettes, 5 ml
10 ml
25 ml
Policemen, Teflon
Scissors
Screwdriver
Phillips
Regular
Stopcock grease, tube
Tape
Duct
High temp
Label
Quantity
Standard
1
1
1
2 boxes
10
1
1
6
10
4
6
4-5
1
1
1
1
1
1
1
Additional
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 15 of 20
Figure 3.2 (continued)
Tape measure, 8 ft
Thermometer, mercury, 6 in. pocket
Thimble gaskets
Filter
Holder
Tubing
Rubber, assorted sizes, 3 ft
Tygon, assorted sizes, 3 ft
Tweezers
Wrenches
Adjustable
Pipe
Quantity
Standard
1
1
Assorted
Assorted
2
2
Additional
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 16 of 20
(nonuniform or insufficient pumping action). Check oiler jars,
if used, every 10 tests.
3.1.5 Dry Gas Meter - A dry gas meter calibration check should
be made using the procedure in Section 3.4.2.
3.1.6 Silica Gel - Either dry the used silica gel at 175°C
(350°F) or use fresh silica gel and weigh several 200- to 300-g
portions in airtight containers to the nearest 0.5 g. Record the
total weight (silica gel plus container) for each container. The
silica gel does not have to be weighed if the moisture content is
not to be determined.
3.1.7 Thermometers - The thermometers should be compared to the
mercury-in-glass reference thermometer at ambient temperature.
3.1.8 Barometer - The field barometer should be compared with
the mercury-in-glass barometer or the weather station reading,
after making an elevation correction, prior to each field trip.
3.2 Reagents and Equipment
3.2.1 Sampling
Filters - Check the filters visually against light for
irregularities, flaws, and pinhole leaks. Either label the
filters on the backside near the edge using numbering machine
ink, or label the petri dishes and keep the filters in their
respective dishes except during actual sampling and weighing.
Dessicate the filters at 20° ±5.6°C (68° ±10°F) and at
ambient pressure for at least 24 h, and then weigh at 6-h in-
tervals until weight changes of <0.5 mg from the previous
weighings are achieved. During each weighing, the filter must
not be exposed to the laboratory atmosphere for >2 min or to a
relative humidity of >50%. An alternative procedure is oven
drying the filters at 105°C (220°F) for 2 to 3 h followed by
desiccation for 2 h and by weighing to a constant weight, as
described above. A 0.5-g Class-S standard weight (Class-S
weight within 1 g of the filter weight) should be placed on the
analytical balance prior to each series of weighings. Either
the balance should agree within +0.5 mg of the Class-S weight(s)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 17 of 20
or the balance should be corrected. A data form should be kept
with the balance at all times for recording the dates and accept-
abilities of the balance checks. Record the final weight to the
nearest 0.1 mg.
Water - 100 ml of deionized distilled water is needed for
each of the first two impingers.
Ice - Crushed ice is needed to keep the gas that exits into
the last impinger below 21°C (70°F).
Stopcock grease - Silicone grease that is acetone insoluble
and heat stable may be used sparingly at each connection point of
the sampling train to prevent gas leaks. This is not necessary
if screw-on connectors with Teflon (or similar) sleeves are used.
Acetone recovery - Acetone will be required on site for
rinsing the probe and the glassware that is upstream from the
filter holder. Deionized distilled water will be required if the
impinger solutions are to be recovered for analysis.
3.3 Equipment Packing
The accessibility, condition, and functioning of measurement
devices in the field depend on careful packing and on the careful
movement on site. Equipment should be packed to withstand severe
treatment during shipping and field handling operations. One
major consideration in shipping cases is the construction mate-
rials. The following containers are suggested, but are not
mandatory.
3.3.1 Probe - Seal the inlet and outlet of the probe to protect
the probe from breakage. Then pack the probe inside the con-
tainer lined with polyethylene or other suitable material. An
ideal container is a wooden case (or the equivalent) lined with
foam material with separate compartments to hold the individual
probes. The case should have handles or eye-hooks that can with-
stand hoisting and that will be rigid enough to prevent bending
or twisting during shipping and handling.
3.3.2 Impingers, Connectors, and Assorted Glassware - All
impingers and glassware should be packed in rigid containers
and protected by polyethylene or other suitable material.
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 18 of 20
Individual compartments for glassware will help to organize and
protect each piece.
3.3.3 Volumetric Glassware - A sturdy case lined with foam
material can contain drying tubes and assorted volumetric glass-
ware.
3.3.4 Meter Box - The meter box—which contains the manometers,
orifice meter, vacuum gauge, pump, dry gas meter, and thermom-
eters—should be packed in a shipping container unless its
housing is sufficient to protect components during travel.
Additional pump oil should be packed if oil is required. It is
advisable to carry a spare meter box in case of failure.
3.3.5 Wash Bottles and Storage Containers - Storage containers
and miscellaneous glassware should be packed in a rigid foam-
lined container.
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 19 of 20
Table 3.1 ACTIVITY MATRIX FOR PRESAMPLING OPERATIONS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Probe
1. Probe liner free of
contaminants and con-
structed of borosili-
cate glass, quartz, or
equivalent; metal liner
must be approved by
by administrator
2. Probe leak free
at 380 mm (15 in.) Hg
3. Probe heating
system prevents mois-
ture condensation
1. Clean probe in-
ternally by brushing
with tap water, de-
ionized distilled wa-
ter, and acetone; air
dry before test
2. Visually check be-
fore test
3. Check heating
system initially and
when moisture cannot
be prevented during
testing (Sec 3.4.1)
1. Repeat clean-
ing and assembly
procedures
2. Replace
3. Repair or re-
place
Impingers,
filter
holders, and
glass con-
tainers
Clean and free of
breaks, cracks, leaks,
etc.
Clean with detergent,
tap water, and
deionized distilled
water
Repair or discard
Pump
Sampling rate of 0.02-
0.03 mVmin (0.66 to
1.0 ftVmin) up to 380
mm (15 in.) Hg at pump
inlet
Service every 3 mo
or upon erratic be-
havior; check
oiler jars every 10
tests
Repair or return
to manufacturer
Dry gas meter
Clean and readings
within ±2% of average
calibration factor
Calibrate according
to Sec 3.4.2; check
for excess oil
As above
Reagents and
Equipment
Sampling fil-
ters
Free of irregularities,
flaws, pinhole leaks;
desiccate 24 h at 20°
±5.6°C (68° ± 10°F),
or oven dry at 105°C
(220°F) 2 to 3 h;
constant weight ±0.1 mg
Visually check prior
to testing; weigh on
balance to 0.1 mg
prior to field use
Replace
(continued)
-------
Section No. 3.4.3
Revision No. 0
Date January 15, 1980
Page 20 of 20
Table 3.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Water
Deionized distilled
conforming to
ASTM-D1193-74, Type 3
Run blank evapora-
tions prior to field
use to eliminate high
solids (only required
if impinger contents
to be analyzed)
Redistill or re-
place
Stopcock grease
Acetone insoluble,
heat stable silicone
grease
Check label data upon
receipt
Replace
Sample recovery
acetone
Reagent grade, <0.001%
residue, in glass
bottles
Run blank evapora-
tions upon receipt
Replace or return
to supplier
Packing Equip-
ment for
Shipment
Probe
Rigid container pro-
tected by polyeth-
ylene foam
Prior to each ship-
Repack
ment
Impingers, con-
tainers , and
assorted
glassware
Rigid container pro-
tected by polyeth-
ylene foam
As above
As above
Pump
Sturdy case lined with
polyethylene foam ma-
terial if not part of
meter box
As above
As above
Meter box
Meter box case and/or
additional material to
protect train compon-
ents; pack spare meter
box
As above
As above
Wash bottles
and storage
containers
Rigid foam-lined con-
tainer
As above
As above
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 1 of 19
4.0 ON-SITE MEASUREMENTS
The on-site activities include transporting equipment to the
test site, unpacking and assembling the equipment, making duct
measurements, performing the velocity traverse, determining
molecular weights and stack gas moisture contents, sampling for
particulates, and recording the data. Table 4.1 at the end of
this section summarizes the quality assurance activities for on-
site activities. Blank data forms are in Section 3.4.12 for the
convenience of the Handbook user.
4.1 Handling of Equipment
The most efficient means of transporting or moving the
equipment from ground level to the sampling site should be de-
cided during the preliminary site visit (or prior correspon-
dence). Care should be exercised to prevent damage to the test
equipment or injury to test personnel during the moving phase. A
"laboratory" area should be designated for assembling the sam-
pling train, placing the filter in the filter holder, charging
the impingers, recovering the sample, and documenting the re-
sults; this area should be clean and free of excessive drafts.
4.2 Sampling
The on-site sampling includes preliminary measurements and
setup, placing the filter in the filter holder, setting up the
sampling train, preparing the probe, checking for leaks along the
entire train, inserting the probe into the stack, sealing the
port, checking the temperature of the probe, sampling at desig-
nated points, and recording the data. A final leak check must
always be performed upon completion of the sampling.
4.2.1 Preliminary Measurements and Setup - The sampling site
should be selected in accordance with Method 1. If this is
impossible due to duct configuration or other reasons, the site
should be approved by the administrator. A 115-V, 30-A electri-
cal supply is necessary to operate the standard sampling train.
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 2 of 19
Either measure the stack and determine the minimum number of
traverse points by Method 1, or check the traverse points deter-
mined during the preliminary site visit (Section 3.0). Record
all data on the traverse point location form shown in Method 1.
These measurements will be used to locate the pitot tube and the
sampling probe during preliminary measurements and actual sam-
pling.
4.2.2 Stack Parameters - Check the sampling site for cylonic or
nonparallel flow as described in Method 1 (Section 3.0). The
sampling site must be acceptable before a valid sample can be
taken. Determine the stack pressure, temperature, and the range
of velocity heads encountered (Method 2). Determine the moisture
content using the approximation Method 4 or its alternatives for
the purpose of setting the isokinetic sampling rate. If the
particular source has been tested before or if a good estimate of
the moisture is available, this should be sufficient. The Refer-
ence Method (Section 3.4.10) uses the condensate collected during
sampling to determine the moisture content used in final calcu-
lations. If the stack is saturated with moisture or has water
droplets, the moisture content must also be determined by partial
pressure with the use of a more accurate stack gas temperature
sensor (Method 4).
Determine the dry molecular weight of the stack gas, as
required in Method 2. If an integrated gas sample is required,
follow Method 3 procedures and take the gas sample simultaneously
with and for the same total length of time as the particulate
run. The sampling and the analytical data forms for molecular
weight determinations are in Method 3.
Using the stack parameters obtained by these preliminary
measurements, the user can set up the nomograph as outlined in
APTD-0576. An example nomograph data form is Figure 4.1.
Select a nozzle size based on the range of velocity heads,
so that it is not necessary to change the size to maintain isoki-
netic sampling rates during the run. Install the selected nozzle
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 3 of 19
Plant
Date
7-/I-77
Sampling location
Calibrated pressure differential across
orifice, in. EUO
Average meter temperature (ambient + 20°F),
Percent moisture in gas stream by volume, %
Barometric pressure at meter, in. Hg
•
Static pressure in stack, in. Hg
(P ±0.073 x stack gauge pressure, in. f^O)
Ratio of static pressure to meter pressure
Average stack temperature, °F
Average velocity head, in. H20
Maximum velocity head, in. ELO
C factor
Calculated nozzle diameter, in.
Actual nozzle diameter, in.
Reference Ap, in. ELO
AH
@
m
avg
wo
m
avg
Ap
avg
^
max
o.oL
-f).0\
n.l
0-3
0-3(15"
Figure 4.1 Nomograph data form (English units).
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 4 of 19
using a Vitron A 0-ring when either glass or stainless steel
liners are used. The tester may opt to install the nozzle on a
stainless steel liner by a leak-free mechanical connection (see
4
APTD-0576 for details ). Other connecting systems such as Teflon
ferrules may be used. Mark the probe with heat resistant tape or
by some other acceptable method to denote the proper distance
into the stack or duct for each sampling point.
Select a total sampling time greater than or equal to the
minimum total sampling time specified in the test procedures for
the specific industry so that:
1. The sampling time per point is >_2 min (greater time
interval may be specified by the administrator).
2. The sample volume corrected to standard conditions
exceeds the required minimum total gas sample volume.
The latter can be based on an approximate average sampling rate.
It is recommended that the number of minutes sampled at each
point be either an integer or an integer plus one-half minute to
avoid timekeeping errors. In some circumstances (e.g., batch
cycles), it may be necessary to sample for shorter times at the
traverse points and to obtain smaller gas sample volumes. In
these cases, the administrator's approval must be obtained first.
4.2.3 Sampling Train Preparation - During preparation of the
sampling train, keep all openings where contamination can occur
covered until just prior to assembly or until sampling commences.
Place 100 ml of distilled water (a graduated cylinder may be
used) in each of the first two impingers; leave the third im-
pinger empty; and place ^200-300 g of preweighed silica gel in
the fourth impinger. Record the weight of the silica gel and the
container on the appropriate data form. Place the empty con-
tainer in a safe place for use later in the sample recovery. If
moisture content is to be determined by impinger analysis, weigh
each of the first three impingers to the nearest 0.5 g, and re-
cord these weights.
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 5 of 19
Using a tweezer or clean disposable surgical gloves, place a
filter in the filter holder. Be sure that the filter is properly
centered and that the gasket is properly placed to prevent the
sample gas stream from circumventing the filter. Check the
filter for tears after the assembly is completed.
4.2.4 Sampling Train Assemblage - Assemble the train as shown in
Figure 1.1, using (if necessary) a very light coat of silicone
grease only on the outside of all ground-glass joints to avoid
contamination. Place crushed ice and water around the impingers.
If not already an integral part of the probe assembly, a
temperature sensor should be attached to the metal sheath of the
sampling probe so that the sensor extends beyond the probe tip
and does not touch any metal. Its position should be about 1.9
to 2.54 cm (0.75 to 1 in.) from the pitot tube and the nozzle to
avoid interference with the gas flow. Alternative arrangements
are shown in Method 2.
4.2.5 Sampling Train Leak Checks - Leak checks are necessary to
assure that the sample has not been biased low by dilution air.
The Reference Method (Section 3.4.10) specifies that leak checks
be performed at certain times as discussed below.
Pretest - A pretest leak check is recommended, but not re-
quired. If the tester opts to conduct the pretest leak check,
the following procedure should be used:
After the sampling train has been assembled, set the filter
heating system at the desired operating temperature. Allow time
for the temperature to stabilize. If a Vitron A 0-ring or other
leak-free gasket is used in connecting the probe nozzle to the
probe liner, leak check the train at the sampling site by plug-
ging the nozzle and pulling a 380 mm (15 in.) Hg vacuum.
Note: A lower vacuum may be used if it is not exceeded during
the test.
If an asbestos string is used for the probe gasket, do not
connect the probe to the train during the leak check. Instead,
leak check the train by first plugging the inlet to the filter
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 6 of 19
holder and pulling a 380 mm (15 in.) Hg vacuum (see previous
note). Then connect the probe to the train and leak check at
about 25 mm (1 in.) Hg vacuum; alternatively, the probe may be
leak checked with the rest of the sampling train in one step at a
380 mm (15 in.) Hg vacuum. Leakage rates >4% of the average
3 3
sampling rate or 0.00057 m /min (0.02 ft /min), whichever is
less, are unacceptable.
The following leak-check instructions for the sampling train
3 4
are taken from APTD-0581 and APTD-0576. Start the pump with
the bypass valve fully open and the coarse adjust valve closed.
Open the coarse adjust valve and then slowly close the bypass
valve until the desired vacuum is reached. Do not reverse the
direction of the bypass valve; this will cause distilled water to
back up from the impingers into the filter holder. If the de-
sired vacuum is exceeded, either leak check at this higher vacuum
or end the leak check as described below and start over.
When the leak check is complete, first slowly remove the
plug from the inlet to the probe or the filter holder and then
close the coarse adjust valve and immediately turn off the vacuum
pump. (This prevents the water in the impingers from being
forced back into the filter holder and prevents the silica gel
from being forced back into the third impinger.) Visually check
to be sure water did not contact the filter and that the filter
has no tears before beginning the test.
During the Sampling - If a component (e.g., filter assembly
or impinger) change is necessary during the sampling run, a leak
check should be conducted before the change. The leak check
should be done according to the procedure outlined above, except
that it should be at a vacuum equal to or greater than the maxi-
mum value recorded up to that point in the test. If the leakage
3 / 3
rate is £0.00057 m xmin (0.02 ft /min) or 4% of the average
sampling rate (whichever is less), the results are acceptable,
and no correction need be applied to the total volume of dry gas
metered. If, however, a higher leakage rate is obtained, the
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 7 of 19
tester either should record the leakage rate and plan to correct
the sample volume as shown in Section 6.3(b) of the Reference
Method (Section 3.4.10), or should void the sampling run. Note:
Be sure to record the dry gas meter reading before and after each
leak check performed during and after each test run so that the
sample volume can be corrected.
Posttest - A leak check is mandatory at the conclusion of
each sampling run. The leak check should be in accordance with
the procedures in this section and at a vacuum equal to or
greater than the maximum value reached during the sampling run.
If the leakage rate is £0.00057 m3/min (0.02 ft3/min) or 4% of
the average sampling rate (whichever is less), the results are
acceptable, and no correction need be applied to the total volume
of dry gas metered. If, however, a higher leakage rate is ob-
tained, the tester either should record the leakage rate and
correct the sample volume as shown in Section 6.3(a) or 6.3(b) of
the Reference Method (Section 3.4.10), or should void the sample
run. Note; Be sure to record the dry gas meter reading before
and after performing the leak check so that the sample volume can
be corrected.
4.2.6 Sampling Train Operation - Just prior to sampling, clean
the portholes to minimize the chance of sampling deposited mate-
rial. Verify that the probe and the filter heating systems are
up to the desired temperatures and that the pitot tube and the
nozzle are located properly. Follow the procedure below for
Ou.lil£/-L-Hiy .
1. Record the initial dry gas meter readings, barometric
pressure, and other data as indicated in Figure 4.2.
2. Position the tip of the probe at the first sampling
point with the nozzle tip pointing directly into the gas stream.
When in position, block off the open area around the probe and
the porthole to prevent flow disturbances and unrepresentative
dilution of the gas stream.
-------
Plant ACME Pn\A/^K Ft-/\i
City M£<$A-WA-TT . Off
Location ///v/7~~ ^ ntJ7~L£~r
Operator >/ ft£:ftn££
Date 2,-^l-T-f,
Run number /\pp- 1
Stack diam, yaxC (in.) //V2-
Sample box number ^
V7- Meter calibration (Y) /.O/2>
Pitot tube (C ) o g,^
Probe length P 7/7 frr
Probe liner material ^5 ^•rr^frL-
Probe heater setting t-~>,~j-
Ambient temperature ^/;
Barometric pressure (P, ) ^_q. 2_3 -
Assumed moisture g%
Static pressure (P ) -^ ^ -HI
Sheet L of /
Nozzle identification number ^/
Nozzle diameter Q.^oftO <»*™ (in.)
Thermometer number C,f~^-£,
Final leak rate^7,^£7/ m^/min (cfm)
Vacuum during leak check J.Q
»«r(in.) Hg ^^(in.) Hg
Filter number /o l~7-
nr (in.) HO Remarks
Meter box number
Meter AH@ / #?- Reference AP n 2.^5 -mm- (in.) H?0
Traverse
point
number
START
A/-/
2-
3
4
5
6
£-1
2_
3
4
5
6
Sampling
time,
(0) , min
O
s
/o
15
2O
25
-5O
35
40
45
50
35
6O
Total ^
Clock
time,
(24 h)
/ ?l£.
/•^Oj?,
/4-2.n
/445
Vacuum,
mm
-etirrT Hg
_-—
/ f)
/ Q
2 n
2,.o
2, .5
?..a
2,3
2. .5
?, 5
?. 5
2..1
2..0
Max^
Stack
tempera-
ture
(TJ,
X(SF)
_— —
^
3/Z
?>/4
311
3L5
3 13
3/1
5/4
313
3)3
3'Z
311
Avgj^.3
Velocity
head
(APs),
mm-"
(in.) H00
_— -
0-37
0,35
ff,3
0,4-3
0,^3
O,4O
0,35
0,29
0.28
Pressure
differ-
ential
across
orifice
meter (AH),
^jam —
(in.) H00
_^-
e.A
&&
2,. 2 3
2. 2S>
2 5
Z.,4-
2.3-
2,^h
2,..5
?..z
1 .ft
1,?
Gas sample
volume XV ),
X (ft3)"1
It*/ *tt
18^.70,2.
/e>°>3M-
793. 77,3
/W.fttt
2,02, . MM
Znb . f<$9
2.// ./04
2,/4-.84P>
2,A? . OSf>
2,? 3. /<&-
£2,6 .793
^3^.J»0
Total>#,^
Gas sample temp-
erature at dry
gas meter
Inlet,
,2€-(°F)
*5
.5?
56
Ib0
6f
6f
62,
6Z,
6i
6i
6^
6ZL
Avg5^
Outlet,
X"(0F)
— -
^
f^
^
4?
50
50
.57
^7
Jl
3ft
.
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 9 of 19
3. Turn on the pump and immediately adjust the sample flow
to attain isokinetic conditions. Nomographs, calculator pro-
grams, and routines are available to aid in the rapid determina-
tion of the orifice pressure drop corresponding to the isokinetic
sampling rate. If the nomograph is designed as shown in
4
APTD-0576, it can be used only with an Type S pitot tube which
has a C coefficient of 0.85 ± 0.02 and when the stack gas dry
molecular weight (M ) is 29 ± 4. If C and M are outside these
s PS
ranges, do not use the nomograph without compensating for the
differences. Recalibrate isokinetic rate or reset nomograph if
the absolute stack temperature (T ) changes more than 10%.
S
4. Take other readings reguired by Figure 4.2 at least
once at each sampling point during each time increment.
5. Record the dry gas meter readings at the end of each
time increment.
6. Repeat steps 3 through 5 for each sampling point.
7. Turn off the pump, remove the probe from the stack, and
record the final readings after each traverse.
8. Conduct the mandatory posttest leak check (Subsec-
tion 4.2.5) at the conclusion of the last traverse. Record any
leakage rate. Also, leak check the pitot lines (Method 2, Sec-
tion 2.1); the lines must pass this leak check to validate the
velocity pressure data.
9. Disconnect the probe, and then cap the nozzle and the
end of the probe with polyethylene or equivalent caps.
During the test run, a sampling rate of ±10% of the isoki-
netic rate must be maintained unless otherwise specified by the
administrator. The sampling rate must be adjusted at any sam-
pling point if a 20% variation in velocity pressure occurs.
Periodically during the test, observe the connecting glass-
ware—from the probe, through the filter, to the first impinger—
for water condensation. If any is evident, adjust the probe
and/or filter heater setting upward until the condensation is
eliminated; add ice around the impingers to maintain the silica
gel exit temperature at 20°C (68°F).
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 10 of 19
The manometer level and zero should also be checked periodi-
cally during each traverse. Vibrations and temperature fluctua-
tions can cause the manometer zero to shift.
4.3 Sample Recovery
The Reference Method (Section 3.4.10) requires that the
sample be recovered from the probe, from all glassware preceding
the filter, from the front half of the filter holder, and from
the filter in an area sheltered from wind and dust to prevent
contamination of the sample. The capped-off impinger box and
the capped sampling probe can be transported to the cleanup area
without risk of losing or contaminating the sample.
4.3.1 Filter - Initially take three unused filters for each
field test series and label them as filter blanks. (These three
should have been tared when the sample filters were tared, since
they are used as the control samples for the check on the analyt-
ical balance.) The filter used for the sample run should be
recovered. Using a pair of tweezers and/or clean disposable
surgical type gloves, carefully remove the filter from the filter
holder, and place it in its designated petri dish. Any filter
fibers or particulates which adhere to the filter gasket should
be removed with a nylon bristle brush or a sharp blade and placed
in the container, which should then be closed, sealed, and
labeled.
4.3.2 Probe and Connecting Glassware - Initially, put a minimum
of 200 ml of the acetone used for sample recovery in .=> ^amp1^
bottle, mark the liquid level, seal, and label the bottle
(Figure 4.3). Then enter the bottle number on the sample re-
covery and integrity form (Figure 4.4). A single sample bottle
is usually adequate for the collection of all the rinses; it
should be labeled and recorded in the same manner as the blank
sample.
Clean the outside of the probe, the pitot tube, and the
nozzle to prevent particulates from being brushed into the
sample bottle. Carefully remove the probe nozzle, and rinse the
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 11 of 19
Plant Hcme. r£u>er TVs/tf/" City GreewloioNj L^isC-ONSiN
Site "Boiler owf/ef Sample type Adeioue. Rinse.
Date 7- £2- 78 Run number ftPP~)
Front rinse H Front filterD Front solution D
Back rinse D Back filter D Back solution D
Solution /9fie-/Y>/i/e. Level marked ueS
Volume: Initial /OO ml Final / GO ml %
e
Clean up by T. SI /
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 12 of 19
Plant /7£/y)€ ntusf/t /
Sample location j3#//f/£
Sample recovery person
Filter(s) number
^##T
/ au-rtCT
77 ?/-7?
MOISTURE
Silica gel
Impingers
Final volume (wt)
Initial volume (wt)
Net volume (wt)
Total moisture
Color of silica gel
Description of impinger water $//<* /i f/y £, /g
.
3.1S
Jic £>
-74"
&S
mi
ml
ml
^
(g)
(g)
(g)
g
sp*.
Final wl
Initial
Net wt
/vr
'- J-/O
wt jo a
/0
g
g
g
g
g
g
got
RECOVERED SAMPLE
Blank filter container number £3066
Filter container number
23 O0 J C,
Description of particulate on filter
Sealed?
Sealed?
tf £ S
Acetone rinse
container number
Acetone blank
container number
3.3.06 O
Samples stored and locked?
Remarks
Liquid level
marked?
Liguid level
marked?
£S
Date of laboratory custody /?-"
Laboratory personnel taking custody
Remarks
Figure 4.4 Sample recovery and integrity data form.
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 13 of 19
5. Rinse the brush to collect any particulates which may
be retained within the bristles.
6. Wipe all the connecting joints clean of silicone
grease, and clean the inside of the front half of the filter
holder by rubbing the surface with a nylon bristle brush and
rinsing it with acetone. Repeat the procedure at least three
times or until no particles are evident in the rinse.
7." Make a final rinse of the filter holder and brush.
8. Clean any connecting glassware which precedes the
filter holder, using step 6.
After all the rinsings have been collected, tighten the lid
on the sample bottle securely. As a precaution in case of leak-
age, mark the acetone level on the bottle, and note it on the
sample recovery form (Figure 4.4).
4.3.3 Impinger Water - Make a notation on the sample recovery
form (Figure 4.4) of any color or film in the impinger water.
Determine the liquid quantity in the impingers either by mea-
suring the volume to the nearest 1 ml with a graduated cylinder
or by weighing it to the nearest 0.5 g with a balance. Record
the data appropriately on the same sample recovery form. If a
different type of condenser is used, determine the liquid catch
gravimetrically or volumetrically employing a suitable procedure.
After determining the liquid gain, discard the water unless
it is to be further analyzed. In this case, follow the sample
recovery procedures recommended by the control agency requiring
the analysis.
4.3.4 Silica Gel - Note the color of the indicating silica gel
to determine whether it has been completely spent, and make a
notation of its condition on Figure 4.4.
I. Transfer the silica gel from the fourth impinger to its
original container using a funnel and a rubber policeman, and
seal the container. It is not necessary to remove the small
amount of dust particles that may adhere to the impinger wall;
since the weight gain is used for moisture calculations, do not
use water or other liquids to transfer the silica gel.
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 14 of 19
2. Determine the final weight gain to the nearest 0.5 g,
if a balance is available.
4.4 Sample Logistics (Data) and Packing of Equipment
Follow the above procedures until the required number of
runs are completed. Log all data on the sample recovery form
(Figure 4.4). If the probe and glassware (impinger, filter
holder, and connectors) are to be used in the next test, rinse
all with distilled deionized water and then acetone. The follow-
ing are recommended after the test.
1. Check all sample containers for proper labeling (time,
date, and location of tests, number of tests, and any other
pertinent data). Be sure a blank has been taken and labeled.
2. Record all data taken during the field test in dupli-
cate by using either carbon paper or data forms and a field
laboratory notebook. Avoid the use of water soluble pens. One
set of data should be mailed to the base laboratory, given to
another team member, or given to the agency; the other set should
be handcarried. Duplication can prevent costly embarrassing mis-
takes .
3. Examine all sample and blank containers and sampling
equipment for damage and for proper packing for shipment to the
base laboratory. Label all shipping containers to prevent loss
of samples or equipment.
4. A quick check of sampling and sample recovery proce-
dures can be made using the on-site checklist, Figure 4.5.
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 15 of 19
Apparatus
Probe nozzle: stainless steel i/ glass
Button-hook S_ elbow size
Clean?
Probe liner: borosilicate ^ quartz other
Clean?
Heating system*
Checked?
Pitot tube: Type S ^ other
Properly attached to probe?*
Modifications
Pitot tube coefficient
Differential pressure gauge: two inclined manometers
other _ ^ sensitivity Q, Ql - O *f-q I
Filter holder: borosilicate glass ^ _ glass frit
filter support _ silicone gasket _ other
Clean?
Condenser: number of impingers
Clean? »X
_
Contents! 1st l&on] H^O 2nd foo ml /^O 3rd 4th Allies ae/
Cooling system _ /<*& / uo
Proper connections?
Modifications
Barometer: mercury __^ _ aneroid ^ other
__^ _
Gas density determination : temperature sensor type -M er/y?o e.
pressure gauge tZOi*/. - U-~fube.
temperature sensor properly attached to probe?* ^
Procedure
r.ecent calibration: pitot tubes* yX (//MANS ION a I (.
meter box* ^ thermometers/thermocouples *
Filters checked visually for irregularities?* ^
Filters properly labeled?* ues
ampling site properly selected?^ ues
Nozzle size properly selected?*
Selection of sampling time?
All openings to sampling train ''plugged to prevent pretest con
tamination?
Impingers properly assembled?
Filter properly centered?
Pitot tube lines checked for plugging or leaks?*
Meter box leveled? t*e$ Periodically?
Manometers zeroed? T~
Figure 4.5 On-site measurements.
(continued)
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 16 of 19
Figure 4.5 (continued)
AH@ from most recent calibration ^
Nomograph setup properly? fas
Care taken to avoid scraping nipple or stack wall?*
Effective seal around probe when in-stack?
Probe moved at proper time?
Nozzle and pitot tube parallel to stack wall at all times?*
Filter changed during run? f]/p
Any particulate lost?
Data forms complete and data properly recorded?*
Nomograph setting changed when stack temp changed significantly?
_ .
Velocity pressure and orifice pressure readings recorded
accurately?*
_
Posttest leak check performed?* fas (mandatory)
Leakage rate g>. &/ _ @ in. Hg
_
Orsat analysis fas from stack _ integrated
Fyrite combustion analysis _ sample location
Bag system leakchecked?*
If data forms cannot be copied, record:
approximate stack temp 317°F volume metered 81 -fj- 3
% isokinetic calculated at end of each run _
SAMPLE RECOVERY
Brushes: nylon brisl
Clean? fas
Wash bottles: glass
Clean? fas,
Storage containers :
Clean? fi?5
Petri dishes: glass
Clean? Ves
~le fas other
tes
borosilicate glass fas
Leakfree?
fas polyethylene
other
fas
other
_ _
Graduated cylinder/or balance: subdivisions <2 ml?*
other
Bal ancel type
Plastic storage containers : airtight?
Clean? fas
_ , _
Probe allowed to cool sufficiently? V£S
Cap placed over nozzle tip to prevent loss of particulate?*
_, Ves ,
During sampling train disassembly, are _all openings capped?
Clean-up area description: Potver
_
Clean? fas Protected from wind?
Filters: glass fiber fas type //£>&> BH
Silica gel: type (6 to 16 mesh)? new? fas used?
Color? blue. Condition? good
(continued)
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 17 of 19
Figure 4.5 (continued)
Filter handling: tweezers used?
surgical gloves? other
Any particulate spilled?*
Water distilled?
Stopcock grease: acetone-insoluble?
heat-stable silicone? other
Probe handling: acetone rinse
distilled water rinse
Particulate recovery from:probe nozzle
probe fitting _ probe liner
front half of filter holder
Blank: acetone Ves _ distilled water
Any visible particles on filter holder inside probe?:*
All jars adequately labeled? yfes Sealed tightly? Yes
Liquid level marked on jars?*
Locked up?
Acetone reagent: <0.001% residue? gjill be gKecked ai lab tWiNg aioa(uS
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 18 of 19
Table 4.1 ACTIVITY MATRIX FOR ON-SITE MEASUREMENT CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Sampling
Filter
Centered in holder; no
breaks, damage, or con-
tamination during load-
ing
Use tweezers or surg-
ical gloves to load
Discard filter,
and reload
Condenser
(addition of
reagents)
100 ml of distilled
water in first two
impingers; 200-300 g of
silica gel in fourth
impinger
Use graduated cylinder
to add water, or weigh
each impinger and its
contents to the near-
est 0.5 g
Reassemble system
Assembling
sampling
train
1. Assembly specifica-
tions in Fig 1.1
2. Leak rate <4% or
0.00057 m /min (0.02
ft /rain), whichever is
less
1. Before each sam-
pling run
2. Leak check before
sampling by plugging
the nozzle or inlet
to first impinger and
by pulling a vacuum of
380 mm (15 in.) Hg
1. Reassemble
2. Correct the
leak
Sampling
(isokineti-
cally)
1. Within ±10% of
isokinetic condition
2. Standard checked
for minimum sampling
time and volume; sam-
pling time/point >2 min
3. Minimum number of
points specified by
Method 1
4. Leakage rate
<0.00057 m /min (0.02
ft /min) or 4% of the
average sampling vol-
ume, whichever is less
1. Calculate for
each sample run
2. Make a quick cal-
culation before test,
and exact calculation
after
3. Check before the
first test run by mea-
suring duct and using
Method 1
4. Leak check after
each test run or be-*
fore equipment re-
placement during test
at the maximum vacuum
during the test (man-
datory)
1. Repeat the
test run
As above
3. Repeat the
procedure to com-
ply with specifi-
cations of Method 1
4. Correct the
sample volume, or
repeat the sam-
pling
(continued)
-------
Section No. 3.4.4
Revision No. 0
Date January 15, 1980
Page 19 of 19
Table 4.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Sample recovery
Noncontaminated sample
Transfer sample to
labeled polyethylene
containers after
each test run; mark
level of solution in
the container
Repeat the
sampling
Sample
logistics,
data collec-
tion, and
packing of
equipment
1. All data recorded
correctly
2. All equipment exam-
ined for damage and
labeled for shipment
3. All sample contain-
ers and blanks properly
labeled and packaged
1. After completion
of each test and be-
fore packing
2. As above
1. Complete data
3. Visually check
upon completion of
each sampling
2. Repeat the
sampling if
damage occurred
during the test
3. Correct when
possible
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 1 of 15
5.0 POSTSAMPLING OPERATIONS
Table 5.1 at the end of this section summarizes the quality
assurance activities for the postsampling operations.
5.1 Apparatus Checks
Posttest checks will have to be made on most of the sampling
apparatus. These checks will include three calibration runs at a
single orifice meter setting; cleaning; and/or routine mainte-
nance. Cleaning and maintenance are discussed in Section 3.4.7
4
and in APTD -0576. Figure 5.1 should be used to record the
posttest checks.
5.1.1 Metering System - The metering system has two components
that must be checked—the dry gas meter and the dry gas meter
thermometer(s).
The dry gas meter thermometer(s) should be compared with the
ASTM mercury-in-glass thermometer at room temperature. If the
two readings agree within 6°C (10.8°F), they are acceptable; if
not, the thermometer must be recalibrated according to Subsec-
tion 2.2 of Section 3.4.2 after the posttest check of the dry gas
meter. For calculations, use the dry gas meter thermometer
readings (field or recalibration values) that would give the
higher temperatures. That is, if the field readings are higher,
no correction is necessary, but if the recalibration value is
higher, add the difference in the two readings to the average dry
gas meter temperature reading.
The posttest check of the dry gas meter is described in Sec-
tion 3.4.2. The metering system should not have any leaks that
were corrected prior to the posttest check. If the dry gas meter
calibration factor (Y) deviates by <5% from the initial calibra-
tion factor, the dry gas meter volumes obtained during the test
series are acceptable. If Y deviates by >5%, recalibrate the
metering system (Section 3.4.2). For the calculations, use the
calibration factor (initial or recalibration) that yields the
lower gas volume for each test run.
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 2 of 15
Plant /\fc/ml mirgf (fJMZX' Calibrated by
Meter box number Fti-l Date T/3 lj?9
Dry Gas Meter
Pretest calibration factor, Y Q.'JBb (within ±2%)
Posttest check, Y* p . f 87 (within ±5% of pretest)
Recalibration required? yes ^L—-—- no
If yes, recalibration factor, Y _ (within ±2%)
Lower calibration factor, Y 0, ^8Ce> for calculations (pretest or
posttest)
Dry Gas Meter Thermometers
Was a pretest temperature correction used? yes i**—no
If yes, temperature correction (within ±3°C (5.4°F) over
range)
Posttest comparison with mercury-in-glass thermometer?* (within
±6°C (10.8°F) at ambient temperature)
Recalibration required? yes t no
Recalibration temperature correction? (within ±3°C
(5.4°F) over range)*
If yes, no correction necessary for calculations if meter
thermometer temperature is higher; if calibration temperature
is higher, add correction to average meter temperature for
calculations
Stack Temperature Sensor
Was a pretest temperature correction used? yes <-—" no
If yes, temperature correction °C (°F) ("within ±1.5% of
readings in K (°R) over range)
Average stack temperature of compliance test, T 7%O K ^ .
Temperature of refe^eace thermometer or solution for recalibra-
tion £3$ K (^Ry1 (within ±10% of T )
Temperature of stacTT^thermometer for recalibration JT28 __
Difference between reference and stack thermometer temperature!
AT Q K (°R)
Do values agree within ±1.5%?* L-^ yes no
If yes, no correction necessary for calculations
If no, calculations must be done twice—once with the recorded
values and once with the average stack temperature corrected to
correspond to the reference temperature differential (AT ) both
final result values must be reported since there is no way to
determine which is correct
Figure 5.1 Posttest calibration checks.
(continued)
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 3 of 15
Figure 5.1 (continued)
Barometer
Was the pretest field barometer reading correct? __^yes no
Posttest comparison?* Xjfff mm (in.) Hg (±2.5 mm (0.1 in.) Hg)
Was calibration required? yes ^ ^ no
If yes, no correction necessary for calculations when the field
barometer has a lower reading; if the mercury-in-glass reading
is lower, subtract the difference from the field data readings
for the calculation
*Most significant items/parameters to be checked.
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 4 of 15
5.1.2 Stack Temperature Sensors - The stack temperature sensor
readings should be compared with the reference thermometer read-
ings .
For thermocouple(s), compare the thermocouple and reference
thermometer values at ambient temperature. If the values agree
within ±1.5% of the absolute temperature, the calibration is con-
sidered valid. If the values do not agree within ±1.5%, recali-
brate the thermocouple as described in Section 3.4.2 to determine
the difference (AT ) at the average stack temperature (T ).
•3 S
Note; This comparison may be done in the field immediately fol-
lowing the tests.
For thermometers, compare the reference thermometer (1) at
ambient temperatures for average stack temperature below 100°C
(212°F), (2) in boiling water for stack temperatures from 100°C
to 200°C, and (3) in a boiling liquid with the boiling point
above 200°C for stack temperature between 200°C to 405°C. For
stack temperatures above 405°C compare the stack thermometer with
a thermocouple at a temperature within ±10% of the average stack
temperature. If the absolute values agree within ±1.5% the cali-
bration is considered valid. If not, determine the error (AT )
S
to correct the average stack temperature.
5.1.3 Barometer - The field barometer should be compared to the
mercury-in-glass barometer. If the readings agree within ±5 mm
(0.2 in.) Hg, the field readings are acceptable; if not, use the
lesser calibration value for the calculations. If the field
barometer reads lower than the mercury-in-glass barometer, the
field data are acceptable. If the mercury-in-glass barometer
gives the lower reading, use the difference in the two readings
(the adjusted barometric value) in the calculations.
5.2 Analysis (Base Laboratory)
The analytical procedures consist of evaporations and
weighings. Although both types of procedures are relatively
simple, it is essential that sample handling be minimized and be
done carefully to avoid loss and contamination.
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 5 of 15
For these procedures, the term "constant weight" means
either a difference between two consecutive weighings of <_0.5 mg
or 1% in the total weight less the tare weight (whichever is
greater) with a minimum of 6 h of desiccation between weighings.
Class-S standard weights should be used to check the balance
before each series of weighings and these weights should be re-
corded on the analytical balance calibration form (Figure 5.2).
The balance results should agree within ±2 mg of the Class-S
weights.
Acetone evaporations should be performed at ambient tempera-
ture and pressure. However, they may be performed at elevated
temperatures with close supervision if the following precautions
are observed:
1. Acetone is highly flammable and has a low flashpoint,
15°C (59°F); therefore, adequate ventilation is essential to
prevent vapor concentration around the heat source.
2. The temperature must be below the boiling point of
acetone, approximately 56°C (133°F), to prevent "bumping".
3. The acetone solution must be swirled occasionally to
maintain an even temperature.
5.2.1 Filter - Leave the filter in the petri dish or transfer
the filter and any loose particulate matter to a tared weighing
dish and desiccate for a minimum of 24 h. Weigh the filter to a
constant weight and record the results to the nearest 0.1 mg on
the analytical data form, Figure 5.3.
Alternatively, the sample filter may be oven dried at 105°C
(220°F) for 2 to 3 h, allowed to cool in a desiccator and then
weighed to a constant weight. Treat the blank filter in the same
manner as the sample filter. The average final weight of the
blank filters should be within ±5 mg of the initial tare weight
or 2% of the sample weight, whichever is greater. If the above
limit is not met, complete the analysis and calculation using the
standard procedures and make a note in the test report of the
nonagreement. The blank filter may be used in a later test, so
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 6 of 15
Balance name
Classification of standard weights
Number
S
Date
7/^/7?
0.500 g
o. so
1.0000 g
j.600^
10.0000 g
/£-O££)3
50.0000 g
0"O-OOO/
100.0000 g
WO. 6003
Analyst
A/2>
Figure 5.2 Analytical balance calibration form.
-------
Plant
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 7 of 15
Run number
Sample location
Relative humidity SD%
/
Density of acetone (p=)
St.
.79 Off
g/ml
Sample
type
Acetone rinse
filter (s)
Sample
identifiable
yM
(j&>
Liquid level marked
and/or container sealed
^
^
Acetone rinse container number
2-2-007-
Acetone rinse volume (V „) 5~9/9
aw f • :" •• •
Acetone blank residue concentration (C_) 0,009
ml
mg/g
/99 mg
d d dW u. •
Date and time of wt 7-5/9-TF ' tf.'flCkiui Gross wt /04QOfi.5~ mg
/
Date and time of wt ^2--"?^ . 'J ,'/$*& Gross wt /
Average gross wt /
Tare wt j_
Less acetone blank wt (W=)
Weight of particulate in acetone rinse (m )
Filter(s) container number ^Z,OC)'^C^
Date and time of wt "7' 3$ - "} % > Q! 4^5*** Gross wt
X
Date and time of wt jf- / -"Iff • /O.' /^AHI Gross wt
Average gross wt
Tare wt
Weight of particulate on filter (s) (m,.)
Weight of particulate in acetone rinse
Total weight of particulate (m )
t049On. 5" mg
'O^nO,^ mg
'n4?J!Ot O mg
4. 1 19 mg
faM. "3%! mg
535 0 mg
539, 0 mg
5"39,^ mg
4(9, 4 mg
//9, ^ mg
&06>. "381 mg
^^-5" 981 mg
Note: In no case should a blank residue >0.01 mg/g or 0.001% of
the weight of acetone used be subtracted from the sample weight.
Remarks
Signature of analyst
/•—•
Signature of revieweir
LJ^"
/
C
^
Figure 5.3 Sample analytical data form.
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 8 of 15
record the blank filter weight on the blank analysis form,
Figure 5.4. To aid the reviewer or the analyst in the filter
weighing procedures, the analytical steps are summarized in
Figure 5.5.
5.2.2 Acetone Rinse and Acetone Blank - Initially, confirm that
no leakage has occurred during transportation of the sample. If
a noticeable amount of leakage has occurred, either void the
sample or use methods approved by the administrator to correct
the final results. Measure the contents in the container either
volumetrically to the nearest 1 ml or gravimetrically to the
nearest 0.5 g. Transfer the contents to a tared 250-ml beaker.
Evaporate to dryness and then desiccate for a minimum of 24 h.
Weigh to a constant weight and record the data to the nearest
0.1 mg on the analytical data form (Figure 5.3); record the data
for the acetone blank on a separate form, (Figure 5.4). To aid
the reviewer or the analyst in the acetone rinse weighing proce-
dures, the analytical steps are summarized in Figure 5.6.
5.2.3 Silica Gel - If not completed in the field, weigh the used
silica gel to the nearest 0.5 g, and record the data on the
sample recovery form (Figure 4.4).
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 9 of 15
plant J{-CM£ f&A^ rtasvrf
Sample location "/^tf//^"
1 fhuf-fvf-
Relative humidity *TO%
Liquid level marked and
Density of acetone (p )
Blank volume (V^) ^/OD
Date and time of wt ^-^
Date and time of wt jf- 1
container sealed (*£/}
f
0.7-90%
W'1% > F;OOA*t Gross wt 9/
/
-'Jff* 7','OOAM Gross wt 9^
/
Average gross wt 9/F
Tare wt 9^
Weight of blank (m , )
g/mi
ml
'^^. 5" mg
'3-F^r mg
3/^, ^ mg
'^tfO- 3&5~ mg
2< /55~ mg
Ca =
Note: In no case should a blank residue greater than 0.01 mg/g
(or 0.001% of the blank weight) be subtracted from the sample
weight.
Filters Filter number 2^)00
Date and time of wt 7~!$-7/; X'^W? Gross wt _ #/O. J mg
Date and time of wt /-/- 7/ 1 %','4'5'AM Gross wt _ ^/O,'? mg
Average gross wt _ 4^/0 , 7 mg
Tare wt _ rftO.'J mg
Difference wt _ f),Q mg
Note: Average difference must be less than ±5 mg or 2% of total
sample weight whichever is greater.
Remarks
Signature of analyst C^UYl^ fk)$P//i/lOsi.
Signature of reviewer
Figure 5.4 Blank analytical data form.
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 10 of 15
Status
Label the filter and/or the petri dish—both with
the same label number; label the filter on top and
bottom; check each filter visually against the
light for irregularities, flaws, and pinhole leaks
Check the desiccator; be sure the lid is sealed
tightly and the anhydrous calcium sulfate is dry;
if not dry, heat the desiccant in the oven for 2 h
at 180-200°C (350°-400°F), and let cool in the
balance room before putting it back into the des-
iccator
Take off the lid of the filter container and
desiccate the filter for 24 h; during desiccation,
be sure that filters are widely spread, and not
overlapping
Adjust the analytical
the accuracy with a 0.
(within ±0.5 mg); use
the filter on the pan
to the nearest 0.1 mg,
should not be >2 min,
should be <50%
balance to zero, and check
500-g Class-S weights
tweezers to carefully place
of the balance, and weigh it
The time of weighing
and the relative humidity
Very important; Desiccator should be tightly
covered immediately after removing the filter to
be weighed; never leave the desiccator open while
weighing a sample because samples in the desi-
ccator will be exposed to moisture in the room,
which will cause gains in their weights
Put the filter back into the petri dish without
the lid, desiccate for >_6 h and reweigh the fil-
ter; the two recorded weights should agree to
±0.5 mg; if not, desiccate for another 6 h and
reweigh until weight is constant within ±0.5 mg;
keep the tare weight of the filter in file for
future use
Be sure the filters that arrived from the field
are handled and analyzed whenever possible by the
same person who started the project—the person
who tared the filters before sampling; use the
same balance
Figure 5.5 Procedure for weighing filters before and after
sampling.
(continued)
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 11 of 15
Figure 5.5 (continued)
7. Perform step #2, and then uncover the filter con-
tainer and visually examine the filter to see if
it is torn; write down all observations that you
think will help justify the final data
8. Desiccate the filter for 24 h, and weigh it to the
nearest 0.1 mg; record the weight then desiccate
again for 6 h, and reweigh; the difference be-
tween the two recorded weights should be within
±0.5 mg; the balance should be zeroed and checked
with a 0.500-g Class-S weight, and the relative
humidity must be <50%
9. Continue the processes of desiccating and weighing
until consistent data are obtained; however, after
the third trial, if no satisfactory data are
obtained, confer with the supervisor
Notes
1. When weighing the filter and sample, be sure to
use a clean brush and to add all particulates or
pieces of the filter that might be left in the con-
tainer
2. Be sure to use tweezers to handle the filters;
never hold them directly with your hand
3. Write down the date and time each time a filter
is weighed
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 12 of 15
Status
I. Preparing Containers for Shipment
1. Select the appropriate size and number of bottles
to be shipped to the field; include extra bottles
2. Clean the bottles and caps thoroughly with soap
detergent, rinse with tap water, and then rinse at
least twice with deionized distilled water
3. Rinse the clean bottles with acetone to get rid of
most of the water; remember that one batch of
acetone could be used for more than one container
4. Check the containers and the caps individually
after they are dry to be sure no detergent or
other contaminant is present; tightly cap all
containers
II. Handling and Analysis of Acetone Rinse Samples
Important; Blanks and samples should have identical
analytical treatments; never handle with bare hands any
analysis glassware once tared; always use tongs or
disposable gloves
*S 1. Log the samples received from the field, and check
each container for leakage; if the sample volume
level is marked on the container, check to see if
the sample still matches the level, if not, write
a note of that
2. Use a dry, clean glass funnel to transfer the
acetone rinse into the dry, clean 250-ml graduated
cylinder
3. Record the volume of the sample to the nearest
1.0 ml, and transfer it into a dry, clean, tared
(to the nearest 0.1 rag) 250- or 300-ml beaker,
depending on the volume of the sample; add 50 ml
to the recorded sample volume to account for the
acetone rinse of all containers
Figure 5.6 Procedure for analysis of acetone rinse samples.
(continued)
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 13 of 15
Figure 5.6 (continued)
Status
iX 4. Rinse the container with two 25-ml portions of
acetone (reagent grade); cap the container, and
shake very gently; transfer the acetone rinse into
the graduated cylinder to rinse it, and then pour
the rinse through the funnel into the beaker that
contains the sample; thus, the container, the
graduated cylinder, and the funnel have been
rinsed
5. Repeat steps 3 and 4 for each sample
*/ 6. Let the samples and blanks dry at room temperature
in a dust-free environment or under a watchglass
S 7. Weigh a clean, empty dry beaker, and place it in
the same atmosphere where the samples are drying
to find out if there was any particulate collected
on the samples from the surroundings while drying
(not mandatory)
^ 8. Transfer the totally evaporated samples and blanks
along with the empty beaker into a tightly sealed
desiccator that contains dry anhydrous calcium
sulfate (CaS04)
9. Desiccate for 24 h
* 10. Zero the balances and check the accuracy with a
100-g Class-S standard weight prior to weighing;
the reading should be 100 g ±0.5 mg, and the rela-
tive humidity in the balance room should be £50%
11. Weigh the samples, blanks, and empty beaker to the
nearest 0.1 mg
It is very important to:
a. Keep the desiccator tightly closed while weighing
b. Remove the samples to be weighed from the desic-
cator one at a time, weigh each, and put each im-
mediately back into the desiccator
c. Keep the weighing time <_2 min
d. Be sure that both sides of the balance are closed
when weighing
(continued)
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 14 of 15
Figure 5.6 (continued)
Status
e. Turn all balance knobs to zero after the weighings
12. Record the weights of the samples, blanks, and
empty beaker; record the date and time, each time
a sample is weighed
13. Desiccate the samples, blanks, and empty beaker
for H> h; data on the first and second weightings
should agree within ±0.5 mg; if not, desiccate
again for 6 h and reweigh until consistent data
are obtained; after the third trial, consult the
supervisor
14. If there is >2 mg change in the weight of the
empty beaker, note it on the analytical data form
15. Calculate the data recorded on the data form
(Figures 5.3 and 5.4) provided for this analysis
-------
Section No. 3.4.5
Revision No. 0
Date January 15, 1980
Page 15 of 15
Table 5.1 ACTIVITY MATRIX FOR POSTSAMPLING OPERATIONS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Sampling
Dry gas meter
Within ±5% of calibra-
tion factor
Make three runs at a
single, intermediate
orifice setting and
at highest vacuum
occurring during test
(Sec 3.4.2)
Recalibrate and
use calibration
factor that gives
lesser sample vol-
ume
Meter thermome-
ter
Within ±6°C (10.8°F)
at ambient pressure
Compare with ASTM
mercury-in-glass
thermometer after
each field test
Recalibrate and
use higher temp-
erature for cal-
culations
Barometer
Within ±5 mm (0.2 in.)
Hg at ambient pressure
Compare with mercury-
in-glass barometer
after each field
test
Recalibrate and
use lower barome-
tric values for
calculations
Stack tempera-
ture
Within ±1.5% of the
reference check temp-
erature (°R)
After each run, com-
pare with reference
temperature
Recalibrate and
calculate with
and without tem-
perature correc-
tion
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 1 of 10
6.0 CALCULATIONS
Calculation errors due to mathematical mistakes can be a
large part of total system error. Therefore, each set of calcu-
lations should be repeated or spot checked by a team member other
than the one who performed them originally. If a difference
greater than a typical roundoff error is detected, the calcula-
tions should be checked step by step until the source of error is
found and corrected. A computer program can be advantageous in
reducing calculation errors. If a standardized computer program
is used, the original data entry should be checked; if differ-
ences are observed, a new computer run should be made. Table 6.1
at the end of this section summarizes the quality assurance
activities for calculations.
Carry out calculations, retaining at least one significant
digit figure beyond that of the acquired data. Roundoff after
final calculations to two significant digits for each run or sam-
ple in accordance with the ASTM 380-76 procedures. Record the
results on Figure 6.1A or 6.IB.
6.1 Nomenclature
The following terms defined and listed alphabetically herein
are to be used in calculating dry gas and water vapor volumes,
moisture contents, acetone residues, particulate weights and
concentrations, and isokinetic variations for each test.
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 2 of 10
SAMPLE VOLUME (ENGLISH UNITS)
3
Vm = £ . & f/ 2 ft, Tm = J-gf
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 3 of 10
SAMPLE VOLUME (METRIC UNITS)
Vm = 1 - 3 7 2 m3, Tm = 3 g£T °K, Pbar = 7 ±/£ . nun Hg
Y = 7 . Q 13_, AH = _ 5*£. mm H20
/Ph_ + (AH/13. 6 )\ , -
vm(std)= °-3858 vm Yr^; r - • ^^m Equation 6-1
PARTICULATE CONCENTRATION (METRIC UNITS)
mg
C = 1 x iQ-— - = _£). Q3lj_ g/dscm
m(std)/ Equation 6-8
Figure 6.IB Particulate calculation form (metric units).
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 4 of 10
2 2
An = Area of nozzle, cross-sectional, m (ft )
B = Water vapor in the gas stream, proportion by
volume
C = Concentration of acetone blank residue, mg/g
ci
C = Concentration of stack gas particulates,
s
dry basis corrected to standard conditions,
g/dscm (Ib/dscf)
AH = Average pressure differential across orifice
meter, mm (in.) H^O
I = Variation of sampling from isokinetic
conditions, %
La = Maximum acceptable leakage rate for either a
pretest leak check or a leak check following
a component change; equal to 0.00057 m /min
(0.02 ft /min) or 4% of the average sampling
rate, whichever is less
L^ = Individual leakage rate observed during the
leak check conducted prior to the "ith" „
component change (i = 1, 2, 3, ... n), m /min
(ft /min)
L = Leakage rate observed during the posttest
p leak check, m /min (ft /min)
m = Mass of acetone residue after evaporation cor-
rected for blank (m =m'-W), mg
a a a
m' = Mass of acetone residue after evaporation, mg
cL
m , = Mass of acetone blank residue after evaporation,
mg
mf = Filter weight gain, mg
m = Total amount of particulates collected, mg
Mw = Molecular weight of water, 18.0 g/g-mole
(18.0 Ib/lb-mole)
P, = Barometric pressure at sampling site, mm (in.) Hg
P = Absolute stack pressure, mm (in.) Hg
S
Pstd = standard absolute pressure, 760 mm (29.92 in.) Hg
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 5 of 10
p = Density of acetone, mg/ml (see bottle label)
3.
PTI = Density of water, 0.9982 g/ml (0.0022 Ib/ml)
w
T = Absolute average dry gas meter temperature,
V / ° "D \
JS. \ Ix)
T = Absolute average stack gas temperature,
K (°R)
T td = standard absolute temperature, 293K (528°R)
0 = Total sampling time, min
0, = Interval of sampling time from beginning of
a run until first component change, min
0. = Interval of sampling time between two suc-
cessive component changes, beginning with
first and second changes, min
0 = Interval of sampling time from final (nth)
™ component change until the end of the sampling
run, min
V = Volume of acetone blank, ml
Cl
V = Volume of acetone used in wash, ml
clW
V. = Total volumes of liquid and silica gel col-
ic
lected in impingers, ml
V = Volume of gas sample measured by dry gas
meter, dcm (dcf)
V , .,. = Volume of gas sample measured by the dry gas
^ ' meter, corrected to standard conditions, dscm
(dscf)
v = Stack gas velocity, calculated by Method 2,
s
using data from Method 5, m/s (ft/s)
V, . ,. = Volume of water vapor in the gas sample,
'w(std)
corrected to standard conditions, scm (scf)
W_ = Weight of residue due to acetone blank, mg
a.
Y = Dry gas meter calibration factor
13.6 = Specific gravity of mercury (Hg)
60 = Seconds per minute (s/min)
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 6 of 10
100 = Conversion to percent, %
6.2 Dry Gas Volume, Corrected to Standard Conditions
Correct the sample volume measured by the dry gas meter to
standard conditions 20°C (68°F) and 760 mm (29.92 in.) Hg by
using Equation 6-1. The average dry gas meter temperature (Tm)
and the average orifice pressure drop (AH) are obtained by
averaging the field data (see Figure 4.1).
Vm(std) VmY
(AH/13-6>
m
,'Pbar + (AH/13.6)\
= Kl VmY I T J Equation 6-1
\ m /
where
K-, = 0.3858 K/mm Hg for metric units, or
= 17.64 °R/in. Hg for English units.
Note: If the leakage rate observed during any mandatory leak
check exceeds the maximum acceptable rate (L=), either the value
a.
of V in Equation 6-1 may be corrected by using Equation 6-1A or
6-1B, or the test may be invalidated.
1. If no component changes were made during the sampling
run, replace V in Equation 6-1 with:
V - (L - L )0. Equation 6-1A
2. If one or more component changes were made, replace Vm
in Equation 6-1 with:
Vm - 01 -2 6p
Equation 6-1B
Substitute for only those leakage rates L^ or L which exceed La.
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 7 of 10
6.3 Water Vapor Volume, Corrected to Standard Conditions
Vw(std) = Vic -P = K2 Vic Equation 6-2
where
3
K2 = 0.001333 m /ml for metric units, or
= 0.04707 ft3/ml for English units.
6.4 Gas Stream Moisture Content
B = r= w(std) . Equation 6-3
ws Vm(std) + Vw(std)
Note; If liquid droplets are in the gas stream, assume the
stream to be saturated and use a psychrometric chart or saturated
vapor pressure table to approximate the mixture percentage.
6.5 Acetone Blank Concentration
mab
C = ~ . Equation 6-4
6.6 Acetone Wash Residue
W = C V p . Equation 6-5
a a aw a
Or combining Equations 6-4 and 6-5:
m V
Wa = v * Equation 6-6
cl
6.7 Particulate Weight
Determine the total particulate catch from the sum of the
weights (obtained from containers 1 and 2) less the acetone wash
residue (see Section 3.4.5).
m = mf + m Equation 6-7
n i a ^
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 8 of 10
6.8 Particulate Concentration
Cs = 1 x 10
-3
m
n
iV.
C = 2.205 x 10
-6
m(std)y
m
n
(metric, mg/m ),
V
(English, Ib/ft3 ).
Equation 6-8A
Equation 6-8B
m(std);
For convenience, the following conversion factors are given.
Conversion Factors
Multiply by
0.02832
From
To
scf
g/ff
g/ft-
g/ft-
m
gr/ft-1
lb/ft"
g/m3
15.43
2.205 x 10
35.31
-6
6.9 Isokinetic Variation
6.9.1 Calculation of I from Raw Data
I =
100 Ts I K3 Vic
VTm)
,
bar
AH/13.6)]
60 8
Equation 6-9
where
K3 = 0.003464 mm Hg-m /ml-K for metric units, or
= 0.002676 in. Hg-ft3/ml-°R for English units.
6.9.2 Calculation of I from Intermediate Values
I =
100 Ts Vm(std) Pstd
60 0
- Bws)
= K
Ts Vm(std)
Equation 6-10
4 0 vs Ps An
where
K4 = 4.320 for metric units, or
= 0.09450 for English units.
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 9 of 10
6.9.3 Acceptable Results - If 90% <_ I <_ 110%, the results are
acceptable. If the results are low in comparison to the standard
and if the I is beyond the acceptable range, the administrator
may opt to accept the results; otherwise, reject them and repeat
the test.
-------
Section No. 3.4.6
Revision No. 0
Date January 15, 1980
Page 10 of 10
Table 6.1 ACTIVITY MATRIX FOR CALCULATIONS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are mot met
Analysis data
form
All data and calcula-
tions given on the
form
Visual check
Complete the miss-
ing data values
Calculations
Difference between
checked and original
calculations not in
excess of roundoff
error; at least one
decimal figure beyond
that of acquired data
retained
Repeat all calcula-
tions starting with
raw data for hand
calculations and for
one sample per test
Indicate errors
in analysis data
on Fig 6.1A or B
Isokinetic
variation
90% < I < 110%; see
Eqs 6.9 and 6.10 for
calculation of I
For each run, calcu-
late I
Repeat the test,
and adjust flow
rates to maintain
I within ±10%
variation
-------
Section No. 3.4.7
Revision No. 0
Date January 15, 1980
Page 1 of 3
7.0 MAINTENANCE
Normal use of emission testing equipment subjects it to
corrosive gases, temperature extremes, vibrations, and shocks.
Keeping the equipment in good operating order over an extended
period of time requires routine maintenance and knowledge of the
equipment. Maintenance of the entire sampling train should be
performed either quarterly or after 1000 ft of operation, which-
ever occurs sooner. Maintenance procedures are summarized in
Table 7.1 at the end of this section. The following procedures
are recommended, but not required, to increase the reliabilty of
the equipment.
7.1 Pumps
Several types of pumps are used in commercial sampling
trains. Two of the most common types are the fiber vane pump
with in-line oiler and the diaphragm pump. The fiber vane pump
requires a periodic check of the oil and the oiler jar. Used oil
(usually nondetergent or machine weight) should be about the same
translucent color as unused or spare oil. When the pump starts
to run erratically or when the head is removed each year, the
fiber vanes should be changed.
The diaphragm pump requires little maintenance. If the
diaphragm pump leaks or runs erratically, it is normally due to a
bad diaphragm or malfunctions in the valves; these parts are
easily replaced and should be cleaned annually by complete dis-
assembly of the train.
7.2 Dry Gas Meters
The dry gas meter should be checked for excess oil and
component corrosion by removing the top plate every 3 mo. The
meter should be disassembled and all components cleaned and
checked more often if the dials show erratic rotation, or if the
meter will not calibrate properly.
-------
Section No. 3.4.7
Revision No. 0
Date January 15, 1980
Page 2 of 3
7.3 Inclined Manometer
The fluid should be changed when it is discolored or con-
tains visible matter, and when it is disassembled yearly. No
other routine maintenance is required since the inclined manom-
eter is checked during the leak checks of both the pitot tube and
the entire meter box.
7.4 Sampling Train
All remaining sample train components should be visually
checked every 3 mo, and they should be completely disassembled
and cleaned or replaced yearly. Many of the items, such as quick
disconnects, should be replaced when damaged rather than after
they are periodically checked. Normally, the best maintenance
procedure is to replace the entire unit—for example, a meter
box, sample box, or umbilical cord.
-------
Section No. 3.4.7
Revision No. 0
Date January 15, 1980
Page 3 of 3
Table 7.1 ACTIVITY MATRIX FOR EQUIPMENT MAINTENANCE CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Routine main-
tenance
No erratic behavior
Routine maintenance
quarterly; disassem-
ble and clean yearly
Replace parts
as needed
Fiber vane pump
Leak free; required
flow
Periodic check of oil
jar; remove head and
change fiber vanes
Replace as needed
Diaphragm pump
Leak-free valves func-
tioning properly; re-
quired flow
Clean valves during
yearly disassembly
Replace when
leaking or when
running erratic-
ally
Dry gas meter
No excess oil, corro-
sion, or erratic dial
rotation
Check every 3 mo for
excess oil or corro-
sion by removing the
top plate; check
valves and diaphragm
when meter dial runs
erratically or when
meter will not cali-
brate
Replace parts as
needed, or re-
place meter
Inclined manom-
eter
No discoloration of or
visible matter in the
fluid
Check periodically;
change fluid during
yearly disassembly
Replace parts as
needed
Sample train
No damage or leaks
Visually check every
3 mo; completely
disassemble and clean
or replace yearly
If failure noted,
use another entire
control console,
sample box, or um-
bilical cord
Nozzle
No dents, corrosion,
or other damage
Visually check be-
fore and after each
test run
Use another nozzle
or clean, sharpen,
and recalibrate
-------
Section No. 3.4.8
Revision No. 0
Date January 15, 1980
Page 1 of 7
8.0 AUDITING PROCEDURE
An audit is an independent assessment of data quality.
Independence is achieved by using apparatus and standards that
are different from those used by the regular field crew. Routine
quality assurance checks by a field team are necessary for ob-
taining good quality data, but they are not part of the auditing
procedure. Table 8.1 at the end of this section summarizes the
quality assurance activities for the auditing.
Based on the results of collaborative tests of Method 5, two
specific performance audits are recommended:
1. Audit of sampling train volumetric flow measuring de-
vice .
2. Audit of data processing.
In addition to these performance audits, it is suggested that a
systems audit be conducted as specified by the quality assurance
coordinator. The two performance audits and the systems audit
are described in detail in Subsections 8.1 and 8.2 respectively.
8.1 Performance Audits
Performance audits are quantitative evaluations of the
quality of data produced by the total measurement system (sample
collection, sample analysis, and data processing). It is recom-
mended that these audits be performed by the responsible control
agency once during every enforcement source test. A source test
for enforcement comprises a series of runs at one source.
8.1.1 Audit of Sampling Train Volumetric Flow Metering Device -
The audit procedure described in this subsection can be used
to determine the accuracy of the flow metering device (dry gas
meter) in a sampling train. The dry gas meter is audited using a
calibrated critical flow orifice housed in a quick-connect
coupling and the following procedure:
1. Remove the critical orifice from its case and insert it
into the gas inlet quick-connect coupling on the source sampling
meter box.
-------
Section No. 3.4.8
Revision No. 0
Date January 15, 1980
Page 2 of 7
2. Turn the power to the meter box on and start the pump.
3. Completely open the coarse flow rate control valve and
close the fine flow rate control valve to give a maximum vacuum
reading. Caution: A vacuum reading of <425 mm (17 in.) Hg will
result in flow rate errors.
4. Allow the orifice and source sampling meter box to
warmup for 45 min with flow controls adjusted as described in
step 3 before starting quality assurance runs. If the audit is
made at the conclusion of the sample run, the warmup period is
not necessary.
5. Make triplicate quality assurance runs. For each run,
record the initial and the final dry gas meter volumes, the dry
gas meter inlet and outlet temperatures, the internal orifice
pressure drop (AH), the ambient temperature, and the barometric
pressure. The duration of the run should be slightly >15 min.
The following procedure is recommended and should be performed
three times to provide the required triplicate quality assurance
runs: 15 min after a run is started, watch the dry gas meter
needle closely. As the needle reaches the zero (12 o'clock)
position, stop the pump and stopwatch simultaneously. Record the
dry gas meter volume and the time.
6. Calculate the corrected dry gas volume for each run
using Equation 8.1. For each replicate, record the corrected
dry gas volume in dry standard cubic meters, the sampling time
in decimal minutes, the barometric pressure in millimeters of Hg;
and the ambient temperature in degrees celcius.
Vm(std) - VmY p ' Equation 8-1
/P AH
- K V Y I 'bar 13'6
"
-------
Section No. 3.4.8
Revision No. 0
Date January 15, 1980
Page 3 of 7
where :
K, = 0.3858 K/mm Hg for metric units, or
= 17.64°R/in. Hg for English units.
The agency/organization determines the percent accuracy, % A be-
tween the measured standard volume and the audit or known stan-
dard volume. The %A is a measure of the bias of the volume mea-
surement in the sampling phase of Method 5. Calculate %A using
Equation 8-2 .
Vstd (M) ' V
% A = - 7--Y - x 100 Equation 8-2
std (AJ
where
Vstd ^M^ = volume measured by the field crew corrected to
standard conditions, m , and
Vstd ^A^ = audit or known volume of the audit device cor-
rected to standard conditions, m .
The recommended control limit for the performance audit is
the 90 — percentile value for % A, based on the results of three
audits (5/78, 10/78, and 3/79) performed by the Environmental
Monitoring Systems Laboratory, USEPA. By definition, 90% of the
laboratory participants in the audits obtained values of % A less
than the values tabulated below. The control limit is initially
expected to be exceeded by 10% of the laboratories to be audited,
based on these three audits. The 90— percentile values are
given below for each audit.
Audit date 90— percentile for % A
05-78 ±10.7
10-78 ± 9.1
03-79 ± 9.6
Based on the results of these audits, the recommended 90— per-
centile control limit for the performance audit is ±10%. The
results of the audit should be included in the emission test
report.
-------
Section No. 3.4.8
Revision No. 0
Date January 15, 1980
Page 4 of 7
Responsible control agencies can obtain a calibrated criti-
cal orifice (when available) prior to each enforcement source
test, conduct the audit, and return the orifice and data form to
EPA for evaluation. Orifices may be obtained from the Source
Test Audit cordinator, Quality Assurance Division, Environmental
Monitoring Systems Laboratory, USEPA, Research Triangle Park,
North Carolina 27711. It is also suggested that organizations
that conduct compliance tests participate in the EPA semiannual
audit of volume meters.
8.1.2 Performance Audit of Data Processing
Calculation errors are prevalent in Method 5. Data proces-
sing errors can be determined by auditing the data recorded on
the field and the laboratory forms. The original and the check
calculations should agree; if not, all of the data and calcula-
tions should be checked. Calculation errors should be clearly
explained to the source test team to prevent or minimize reoccur-
rence. The data processing errors may also be determined by
requesting that copies of data sets compiled in the field and
copies of manual data reductions (or computer printouts if used)
be forwarded to the evaluator for audit.
8.2 Systems Audit
A systems audit is an on-site qualitative inspection and
review of the total measurement system (sample collection, sample
analysis, data processing, etc.). Initially, a systems audit is
recommended for each enforcement source test, defined here as a
series of three runs at one source. After the team gains expe-
rience with the method, the frequency of audit may be reduced—
for example, to once for every four tests.
The auditor should have extensive background experience in
source sampling, specifically with the measurement system being
audited. The functions of the auditor are summarized in the
following:
1. Observe the procedures and techniques of the field team
during sample collection.
-------
Section No. 3.4.8
Revision No. 0
Date January 15, 1980
Page 5 of 7
2. Check/verify the records of apparatus calibrations and
the quality control charts used in the laboratory analysis.
3. Record the results of the audit and forward them with
comments on source team management to the quality assurance
coordinator so that any needed corrective actions may be imple-
mented.
The auditor should observe the field team's overall per-
formance of the source test. Specific operations to observe
should include, but not be limited to:
1. Setting up and leak testing the sampling train.
2. Isokinetic sampling check of the sampling train.
3. Final leak check of train.
4. Sample recovery.
Figure 8.1 is a suggested checklist to be used by the auditor for
developing a list of important techniques/steps to observe.
-------
Section No. 3.4.8
Revision No. 0
Date January 15, 1980
Page 6 of 7
Yes
iX
S
(X
,/
,/
*
No
&jP/]fZf~
fA-UD'S'
~£M-HN
Comment
ok
OK
x
Ok
Ok
SffO^TED OC
'U%>.
OPERATION
Presampling Preparation
1. Knowledge of process conditions
2. Calibration of pertinent equipment:
in particular, the dry gas meter,
orifice meter, and pitot tube
On-Site Measurements
3. Sample train assembly
4. Pretest leak check of train
5. Isokinetic sampling
6 . Posttest check
7. Sample recovery and integrity
8. Recording of pertinent process
information during sample collec-
tion
Postsampling
9. Check of analytical balance
10. Use of acceptable detection blanks
in correcting field sample results
11. Calculation procedure/check
General Comments
ST~ ptJg/fJt> RUN 3 — T2>VT 'ZAMPL-/N(> M/4.S At 7D
Figure 8.1 Method 5 checklist to be used by auditors.
-------
Section No. 3.4.8
Revision No. 0
Date January 15, 1980
Page 7 of 7
Table 8.1 ACTIVITY MATRIX FOR AUDITING PROCEDURES
Audit
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Volumetric
sampling
phase of
Method 5
Measured pretest volume
within ±10% of the
audit volume
Once during every en-
forcement source
test, measure ref-
erence volume, and
compare with true
volume
Review operat-
ing technique
Data processing
errors
Original and check cal-
culations agree
Once during each
enforcement source
test, perform inde-
pendent calculations
starting with the
recorded data
Check and cor-
rect all data
Systems audit
Conducted method as
described in this sec-
tion of the Handbook
Once during each
enforcement test
until experience
gained, then every
fourth test, observe
techniques; use
audit checklist
Fig 8.1
Explain to team
the deviations
from recommended
techniques; note
the deviations on
Fig 8.1
-------
Section No. 3.4.9
Revision No. 0
Date January 15, 1980
Page 1 of 1
9.0 RECOMMENDED STANDARDS FOR ESTABLISHING TRACEABILITY
To achieve data of desired quality, two considerations are
necessary: (1) the measurement process must be in a state of
statistical control, and (2) the systematic errors, when combined
with the random variations (errors of measurement), must result
in a suitably small uncertainty.
To ensure good data, it is necessary to perform quality con-
trol checks and independent audits of the measurement process; to
document the data by quality control charts (as appropriate); and
to use materials, instruments, and procedures which can be traced
to a standard of reference.
The working calibration standards should be traceable to
primary or higher level standards such as those listed below.
1. The dry gas meter should be calibrated against a wet
test meter which has been verified by liquid displace-
ment, as described in Section 3.4.2.
2. The analytical balance should be checked against
Class-S weights that are traceable to NBS standards.
-------
Section No. 3.4.10
Revision No. 0
Date January 15, 1980
Page 1 of 6
10.0 REFERENCE METHOD
TPKRATUBE SENSOR
PMBE
TEMPERATURE HEATE°AREA THERMOMETER
.FILTER HOLDER
tWINGER TRAIN OPTIONAL. MAY IE REPLACED
•VAN EQUIVALENT CONDENSER
THERMOMETER
METHOD fr—DITKKHIHATIOK 01 ?ABTICPIATI EMISSIONS
FBOM SUTIONABT SOOSCM
1. PrineipU and AppllmdaUf
1.1 Principle. Partioulate matter is withdrawn too-
Hnetlcally from the source and collected on * glatt
fiber filter maintained at a temperature in the range of
120±14* C (248±25° F) or such other temperature M
specified by an applicable subpart of the standards or
approved by the Administrator, U.S. Environmental
Protection Agency, for a particular application. The
paniculate mass, which Includes any material that
condenses at or above the filtration temperature, it
determined gravimetrically after removal of uncombined
water.
1.3 Applicability. This method is applicable lor the
determination of paniculate emissions from stationary
sources.
2. Apparatus
2.1 Sampling Train. A schematic of the sampling
train used in this method is shown in Figure 5-1. Com-
plete construction details are given in APTD-0581
(Citation 2 In Section 7); commercial models of thia
train are also available. For changes from APTD-0581
and for allowable modifications of the train shown in
Figure 5-1, see the following subsections.
The operating and maintenance procedures for the
sampling train are described in APTD-0576 (Citation a
in Section 7). Since correct usage is important in obtain-
Inf valid result*, all users should read APTD-057A and
adopt the operating and maintenance procedure! out-
lined in it, unless otherwise specified herein. The sam-
pling train consists of the following component!:
UJ Probe Ntczla. 8tainleas f teal (SIR or glass with
•harp, tapered leading edge. The angle of taper shall
M itwo1, as utcribed IB Section
Z.2 of Method 2. On* manometer stall be used j>r velocity
head (dp) reading!, and the other, lor orifice rti"Tptla
gmttsurt reading*.
Z.L* rilwr Holder. BorosUfcate fclata, with a clan
wit filler support and a sUteone rubber gasket. Other
materials of construction approval of tbe Ad
raimstrator. The bolder design shall provide a positive
•eal against leakage jom the outside or around the Blur.
The holder «hall be attached inunediaUly at the outlet
ol the probe (or cyclone, if used).
I.I.6 Filter Beating System. Any beating system
capable of maintaining a temperature around the Alter
bolder during sampling « 1SO±14° C <24fck2S« F), or
such other temperature as specified by an applicable
tnbpan of the standards or approved by the Adminis-
trator for a particular application. Alternatively, the
teeter may opt to operate the equipment at a temperature
tower than that specified- A temperature gauge capable
of measuring temperature to within 3° C (5.4° F) thai]
be installed so thai the temperature around the filter
bolder can be regulated and monitored during sampling.
Heating systems other than the one shown In APTD-
0581 may be uoed.
2,1.7 Condenser. The following system shall be oned
to determine the stack gas moisture content: Four
unpingers connected in tehee with leak-tree ground
glass fittings or any similar leak-free non-contaminating
fltUngs. The first, third, and fourth impingers shall be
•I the Oreenburg-Smith design, modified by replacing
the up with 1J cm (M in.) ID glass lube extending u>
about 1.3 cm (M in.) from the bottom o1 the fiask. The
second impinger shall be ol the Oreenburg-Smith design
with thp standard Up. Modifications (e,g., using flexible
connections between the imp^ngers. using materials
other than glass, or using flexible vacuum lines to connect
the filter bolder to the condenser) may be used, subiect
lo the approval of the Administrator. The first and
second Implngers shall contain known quantities ol
water (Section 4.1.3), the third shall be empty, and the
fourth shall contain a known weight ol silica gel. or
equivalent deaiccant. A thermometer, capable of measur-
ing temperature to wltbla f C (P F) thai) be placed
at the outlet of the fourth ImpiBger tor monitoring
Alternatively, any system that cools tbe sample gas
stream and aUows measuremMH of the water condensed
and moisture leaving the condenser, tach U> within
1 ml or 1 g may be uted, subject to the approval of the
Administrator. Acceptable means are to measure the
condensed water either gravunetncally or volurnetrteally
and to measure the moisture leaving the condenser by:
(1) monitoring the temperature and pressure at the
exit of the condenser and using Dalton s law of partial
pressures; or £2) passing the sample gas stream through
a tared silica gel (or equivalent desiccant) trap with
«xu gasee kept below 20° C (68° F) and determining
Ike weight gain.
If means other than silica gel are osed to determine
tbe amount of moisture leaving the condenser. It is
recommended thai silica gel (or equivalent) still be
lued between tbe condenser system and pump to prevent
moisture condensation In tbe pump and metering devices
and to avoid the need to make corrections for moisture In
the metered volume.
NOTE.—II a determination of the paniculate matter
collected in tbe impiogers is desired in addition to mois-
ture contenl, tbe tmpinger system described above shall
be used, without modification. Individual Stales or
control agencies requiring this information shall be
contacted as to the sample recovery and analysis ol tbe
impinger contents.
2.1.8 Metering System. Vacuum gauge, teak-'ree
pump, thermometers capable ol measuring temperature
lo wiihin 3° C (5.4* F), dry gas meter capable ol measuring
volume to within 2 percenl, and relaied equipmenl. as
shown in Figure 5-1. Other metering systems capable of
maintaining sampling rates within 10 percent ol tso-
klnetic and of determining sample votume> to within 2
percent may be used, subject lo tbe approval 01 the
Administrator. When the metering system is used in
conjunction with a pitot tube, the system shall enable
checks 01 isokinetic rates.
Sampling trains ulilinngmeteringsystems designed tor
higher flo» rales than Chat described in APTD-0581 or
APTlM>57t, may be used provided that the specifica-
tions o this method are met.
2.1.y Barometer. Mercury aneroid, or other barometer
capable ol measuring atmospheric pressure lo within
2.5 rnm Hp (0.1 in. Hg). In many cases, the barometric
reading may be obtained from a nearby national weather
service station, in which case the station value (which is
TCDEIAL KGKTEft, VOL. ft, NO. 160—THURSDAY, AUGUST It, If77
-------
41779
the absolute barometric pressure) shalTbe requested an*
an adjustment to elevation differences between. th*
weather station and sampling point shall b> applied at *
rate of minus 2.5 nun Hg (0.1 m. Hg) par 90 m (100 tQ-
elevation increase or rice Tena (or eleTatlon decrease.
2.1.10 Oai Density Determination Equipment,
Temperature sensor and pressure range, a* described
In Sections 2.3 and 2.4 of Method 1, and (as analyiar,
if necessary as described In Method >. The temperature
sensor snail, preferably, be permanently attached to
the pltot tube or sampling proba in a toed configuration,
«och that the tipof the sensor extends beyond the leadtae
edge of the probe sheath and doat not touch any metaT
Alternatively, the sensor may be attached just prior
tomelntbeneld. Note, however, that Ifthe tern perataf*
aannr unattached In the flekf, the sensor must be place*
In an interfarence-fre* arrangement with respect to th»
Type S pitot tube opening* (see Method 2, rigor* 1-7).
As a second alternative, if a difference of not more than
1 percent In the average velocity measurement to to faf.
introduced, the temperature gauge need not be attached
to th* proba or pltot tab*. (This attamattv* to subject
to tbt approval of the Administrator.)
2.2 Sample Reoowrj. The following item* m
tUUS- AND
*» Assyria. Two racoiti are raqnlnd to the anari-
UEf ' Aeebn*. Same as Ut
»A1 Dtdeoant. Anhydrous calcium suHmt*, Indicat-
ing-type. Alternatively, other types of dadoeanbi may be
used, subject to the approval ofthe Administrator.
4.1 Ssmpling, The complexity of this method U such
that. In order to obtain reliable results, testers should b*
trained and experienced with the test procedures.
4.1.1 Pretest Preparation. An the components shall
be maintained and calibrated according to the procedure
described In AFTD-OoTt, unless rtberwUe specified.
Herein.
alternative, the attic*, (el need not be pnwelghed, bo*
may •» weighed directly In Its uxtpinger or aunnUng.
holder hut prior to train assembly.
Cheek filters visually againstlight
flawi or plnbole leaks. Label fllten of the proper diameter
t light to irregularities and
2.2.1 Probe-Liner and Proba-Noail* Brashes. Nyfca
bristle brashes with stainless steal win handles. Tb*
probe brush shan have extensions (at least as lent at
the probe) of stainlees steel, Nyloo, Teflon, or stoilarly
inert material. The brashes shall be property sfced and-
abaped to brush out the probe liner and nook.
2.2J. Wash Bottles-Two, Otos* waak bottle* sr*
neommended; polyethylene wash buttles may b* need,
at the option of the tester. It is recommended th*tac«toBw>
not be stored in polyethylene bottles to loafer then •
month.
2.2.» Glass Sample Storag* Container*. Chemically
resistant, boneUktie glass bottles, to acetone wash**,
«00 ml or 1000 ml. Screw cap ttnanshall either be rabbet
backed Teflon or shall be conatroeVd so at to b* Ink-tow
on the back sM< near the edge using numbering machine
ink. As an alternative, label the shipping container*
" >ep the fitters I
at: aB thnM ••Mom rfi
weighing.
Derieeste tn* fiHen at 20±&t* C («8±lo* F) and
(glMS or plastic petri dfebes) and keepthe fitters In these
eontaimn at aB time* except,, during sampling and
terval*
t pressure to at least M hours and weigh at in-
ef at least • boon to a constant weight, I.e.,
For analysis, the fcttnrtng equipment tr
.
2.1.1 Otese Weighing DJsne*.
2».» Periccator
IS.* Analytical Bakme*. To meeeur. to wtthta ftt
mg.
13.4 Balance. To umama to within 9jg.
2.I.4 Beakers. 2M ml.
2.S.* Hygrometer. To nise»ure the relative tnauOtt
ef the laboratory environment.
fan
1J.T Temperature
re of the Moratory
Gauge. Tei
nt.
ittwtempera-
—. Method 4 or Its alternative* for
the purpose of making laoilnetie sampling rate setting*.
Determine the stack fas dry molecular weight, as des-
cribed in Method 2, Action 3.8; if integrated Method S
sainpUug i»u*ed to molecular weight determination, the
integrated bag sample shan b* taken smmttaneouaty
with, and to the same-total length of time as, the par-
ticulate sample ran.
Beleet a noxsle six* based on the range of velocity head*,
such that ft to not necessary to change the noule slxe In
order to maintain tooMnetie sampling rates. Daring the
ran* do not change the noxxle sit*. Ensure that the
proper differential pressure (ange to chosen to the rang*
of velocity head* encountered fee* Section 2J of Method:
2). •
• 8ele*asQitabtoprob«liner and probe length such that
*B traverse point* can b* sampled. Forlarge stack*,
consider sampling bom opposite side* of the stack to
reduce the length of probe*. -
Select a total sampling time greater than or equal to
th* minimum total sampling tune specified in the te*t
procedures to th* speclflcTndnstry such that a) th*
sampHiw; time per pout is not less than 2 sain (or some
gnatertime interval as specified by the Administrator),
Sampling. The reagent* use* In sampling arc a*
S.1J POten. Glass floor niton, without organ!*
. binder, exhibiting at least 99 M percent efficiency ( §OM
'. percent penetration) on OJ-mlcron dloetyi phthalate
smoke particles. Th* Otter efficiency test shan be con-
ducted in socord&nee with ASTM standard method D
2MO-71. Test data from the supplier's qnaUty control
program are suffloient to this pnrpos*.
£u. Silica CM. Indicating type, « to. M merit, tt
. previously used, dry it ITS* C (sOfT) tor 2 boon. New
sliioa gal may b* ond a* received. Alternatively, other
type* at destceanta (equivalent or better) may be nsed,
- of th* Administrator.
the hnpingers is required, distilled water shall be used.
SOB blanfa nri«2IS? ns* to eUmlnrt* a Ugh blank
1.L* Creahedle*
M* Stopcock
ibl*,tte*t-*tabJ»
i tr****. Thto to not necessary if screw-on —
i with Teflon sleeves, or similar, are nsed. Attorna.
ben*ed,sub-
gnd*. /mln (0.03 cfm), whichever to toss, ara
unacceptable.
The following leak-check instructions to the sampling
traindeseribedin APTD-0679and APTD-OSgl may b*
helpful Start the pomp with bypas* valve .rally open
and coarse adjust valve completely dosed. Partially
*p*n tb* coarse adjust vatv* and slowly close th* byp**s
valve until the desired vacuum is reached. Do not reverse
direction of bypaa* valve; this will cans* water to back
op Into th* fitter holder. If tb* desired vacuum to ex-
ceeded, either leak-check at this higher vacuum or and
th* leak check as shown below and start over.
Whan the leak-check to completed, first slowly remov*
tb* plug from the Inlet to the probe. Oner holder, or
cyclon* (if applicable) and immediately turn off th*
vaccum pump. This prevents th* water in the unplngan
from befog forced backward into th* fitter holder and
silica gel from being entrained backward into the third
unpinger.
4.1.4J Leak-Checks Daring Sample Run. If, during
th* sampling run, a component (e-g., niter assembly
or inipinger; change become* necessary, a leak-check
shall b* conducted Immediately before th* change to
mad*. Th* leak-check shall b* don* according to tb*
procedure outlined In Section 4.1.4.1 above, except that
It shall b* done at a vacuum equal to or greater than th*
maximum value recorded up to that point in th* teat.
If th* leakage rate to found to be no greater than O.OOO57
m'/mln (0.02 cfm) or 4 percent of the average sampling
rat*.(whlch*ver is IMS), the results an acceptable, and
no correction win need to be applied to the total volume
of dry gas metend; if, however, a higher leakage rate
la obtained, the tester shall either record the leakage
rate and plan to correct th* sample volum* as shown In
Section 6.3 of this method, or shall- void the sampling
run.
Immediately after component changes, leak-check*
an optional: IIsuch leak-checks an done, the procedure
outlined In Section 4.1.4.1 above shall be used.
4.1.4.3 Post-test Leak-Cheek. A leak-cheek is manda-
tory at the conclusion of each sampling run. The leak—
•heck shall b* don* In accordance with the procedure*
outlined ht Section 4.1.4.1, except that it shall b* eon-
ducted at a vacuum equal to or greater than the maxi-
mum valo* reached daring tb* sampling run. If th*
leakage rate to fanndto be no greater than 0.00067 m«/mi»
(0.08 cfm) or 4 percent of the average sampling rat*
(whichever to lee*), tb* results an acceptable, and no,
correction need be applied to the total volume of dry ga*
metend. If. however, a higher leakage rate to obtained,
the taster shall either record the leakage rate and correct
the sample volume as shown in Section 9.3 of this method,
or shall void the sampling run.
4.1.* Particntato Tram Operation. Dmrtng th*
sampling run, maintain an tookin*ti* sampling rate
(within M) percent of tn* tookmetie unless otherwise-
specified bf th* Administrator) and a' tamperatnra
around th* fetor of 120*14? O 0*Jbfc2»« F), or such other
temperature a* specified by an applicable snbpart of th*)
standards or approved by tb* Administrator.
For each ran, record the data required on a data sheet
•nob as the one shown In Figure 5-2. Be son to record tb*
Initial dry gas meter reading. Record the dry gas meter
readings at the beginning and« " " " "
t beginning and end of each sampling time)
increment, wneo changes in Oow rates are made, ^ '
and after each leak check, and when sampling is 1
•BOAl HOUTBr, VOk- 47,-NO. 140—THUISDAY. AUGUST It, 1977
-------
AND REGULATIONS
Section No. 3..4.10
Revision No. 0
Date January 15, 1980
Page 3 of 6
41T79
Take other readings reqiired by Figure R-2 at least once
at eacb sample point during eaob time Increment ana
•Mltional readings when significant changes (20 percent
variation in Telocity bead readings) necessitate addi-
tional adjustments in flow rate. Level and nro tbe
manometer. Because tbe manometer level and uro may
drift due to vibrations and temperature changes, make
periodic checks during the traverse.
Clean tbe portholes prior to the teat ran to mtadmlxe
the ebanoe of sampling deposited material To begin
sampling, remove the noub cap, verily that tk* fitter
and probe beating systems an op to temperature, and
that tbe pilot tube and probe an properly positioned.
Position tbe noule at tbe first traverse point with the Up
pointing directly Into tbe gas stream. '"""«^'^«'j start
{be pump and adjust tbe flow to laokinette condition*.
Nomographs are available, which aid In tbe rapid adjust-
ment tt tta IsoMnetle sampling rate without excessive
eompnfetlona. Tbese nomographs an designed for use
when tbe Type B pilot tube coefficient li o3fct0.02. and
tbe stack gas equivalent density (dry molecular weight)
k equal to »=tL APTD-0678 details the procedure for
oslng tbe nomographs. II C, and tit an outside the
above stated ranges do not use tbe nomographs unless
appropriate steps (see Citation 7 in Section 7) are taken
to compensate lor the deviations.
PLANT
LOCATION
OPERATOR,
BATE
HUN NO
SAMPLE BOX N0._
METER BOX N0._
METER AHff
EFACTOR .
AMBIENT TEMPERATURE.
BAROMETRIC PRESSURE.
ASSUMED MOISTURE. K_
WOBE LENGTH.* (ft)
•NOZZLE IPENTIFICATION N0.__
AVERAGE CALIBRATED NOZZLE DIAMETER. «»GsJ_
PROBE HEATER 8ETTme
LEAK RATE.»3M»,(chO-—^
flTOTTUBE COEFFICIENT. C,.
SCHEMATIC OF STACK CROSS SECTION
MOBE LINER MATERIAL
STATIC PRESSURE. MI H| (h. H|L
«LTER NO.
TRAVERSE POINT
.NUMKR
TOTAL
SAMPLING
TIME
(fl.aiia.
AVERAGE
VACUUM
mm Ho.
On. Ho)
STACK
TEMPERATURE
CT$)
•CI»FJ
vaocin
HEAD
lAPjI.
ewflaJHIiO
PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE
METE*
•MUjO
IIH.H20)
OAS SAMPLE
VOLUME
•aS(ftS)
GAS SAMPLE TEMPERATURE
AT DMT OAS METER
mm
^crn
Av*
OUTUT
•c «»n
Av«.
Av9.
TEMPERATURE,
•CI»P)
TEMPERATURE
OF OAS •
LEAVING
CONDENSER OR
LAST IMPINGER.
•Clfl
When the stack Is under significant negative pressure
Qielgbt of impinger stem), take care to close the coarse
adjust valve before Inserting the probe Into the stack to
prevent water from backing into the filter holder. If
necessary, tbe pump may be turned on with the coarse
adjust valve closed.
When the probe Is in position, block 08 tbe openings
•round tbe probe and porthole to prevent unrepre-
sentative dilution of tbe gas stream.
Traverse the stack cross-section, as required by Method
I or as specified by tbe Administrator, being careful not
to bump tbe probe nonle into tbe stack walls when
jampUng near tbe walls or when removing or Inserting
tbe probe through tbe portholes; this minimises tbe
chance of extracting deposited material.
During tbe test run, make periodic eojustmento to
keep tbe temperature around tbe filter holder at tbe
proper level; add mon loe and, if necessary, salt to
maintain a temperature of less than 90° C (68° F) at the
condenser/silica gel outlet. Also, periodically check
tbe level and tero of the manometer.
isokinetiC sampling difficult to _
fitter may be replaced in the midst of a sample run. It
Is recommended that another complete filter assembly
be usedratber than attempting to change the filter Itself.
Before a new filter assembly is Installed, conduct a leak-
check (see Section 4.1.4.2). Tbe total particulate weight
•ball Include the summation of all filter assembly catches.
except!
locations within the same duct, or, i
ment (allure necessitates a change of trains. In all other
situations, the use of two or more trains will be subject to
tbe approval of the Administrator.
Figure 5-2. Particulate field data.
Mote that when two or more trains an used, separate
analyses of the front-half and Of applicable) Impingw
catches from eacb train shall be performed, unless Identi-
cal noule sizes were used on all trams, In which ease, tbe
front-half catches from the Individual trains may be
combined (as may the Impinger catches) and one analysis
el front-half catch and one analysis of impinger catch
may be performed. Consult wltb the Administrator for
details concerning the calculation of results when two or
mon trains an used.
At the end of the sample run, turn off tbe coarse adjust
valve, remove the probe and noule bom the stack, turn
off the pump, record the final dry gas meter reading, and
conduct a post-test leak-check, as outlined In Section
4.1.4.3. Also, leak-check the pltot lines as described In
Method 2, Section 3.1; the lines must pass this leak-check.
In order to validate the velocity head data.
4.1.8 Calculation of Percent Jsokmetic. Calculate
percent Isokinetic (see Calculations, Section 8) to deter-
mine whether the run was valid or another test run
should be made. If then was difficulty in m»int«itiiTi»
Isokinetic rates due to source conditions, consult with
the Administrator lor possible variance on the Isottnetie
rates.
4.2 Sample Recovery. Proper cleanup procedure
begins as soon as the probe Is removed from the staok at
the end of the sampling period. Allow the probe to cod.
When tbe probe can be safely bandied, wipe off all
external parnculate matter near the tip of the probe
noule and place a cap over It to prevent losing or raining
partloulate matter. Do not cap ofl the probe tip tightly
while the sampling train Is cooling down as this would
create a vacuum in the filter bolder, thus drawing water
from the implngers into tbe filter holder.
Before moving the sample train to the cleanup rite,
remove the probe from tbe sample train, wipe on the
stllcone grease, and cap the open outlet of the probe. Be
eararol not to loee any eondensate that might be present.
Wipe off the sllioone grease from the nlterinlet when the
probe was fastened and eap tt. Remove the umbilical
cord from the last Impinger and eap the Impinger. If •
•flexible line Is used between the-first Impinger or eon-
denser and the filter holder, disconnect tbelbw at the
filter bolder and let any condensed water or liquid
drain into the unpingers or condenser. After wiping ofl
the sllioone grease, cap ofl the filter holder outlet and
Impinger inlet. Either ground-glass stoppers, plastic
caps, or serum caps may be used to close these openings.
Transfer the probe and filter-lmpinger assembly to the
cleanup area. This area should be dean and protected
from the wind so that the chances of contaminating or
.losing the sample will be minimised.
Save a portion of the acetone used lor cleanup as a
blank. Take 200 ml of this aoetone directly from the wash
bottle being used and place It In a glass sample container
labeled "acetone blank."
Inspect the train prior to and dnrlng-dlsassembly and
note any abnormal conditions. Treat the samples as
follows:
Gmtafner No. 1. Carefully remove the filter from the
filter holder and place it in la Identified petri dish con-
tainer. Use a pair of tweeters and/or clean disposable
eurglcal gloves to handle the filter. If tt is necessary to
fold the filter, do so such that the partieulate cake is
Inside the fold. Carefully transfer to the petrl dish any
partieulate matter and/or filter fibers which adhere to
the filter holder gasket, by using a dry nylon bristle
brush and/or a sharp-edged blade. Seal the container.
Container No. I. Taking can to see that dust on the
outside of the probe or other exterior surfaces doss not
get into the sample, quantitatively recover partloulate
matter or any eondensate from the probe noule, probe
FEDERAL REGISTER, VOL 42, NO. 160—THURSDAY, AUGUST IB, 1977
-------
41780
fltttaf, prate Bn«, and front halt ol ti» ok* bald* bf
washing; tnese component! with acetone od placing, tta*
waata In • lisas container. DtatQM water mn be used
instead of acetone when approved by tbe Adimiiistzator
and shall be use* wben specified, by tbe Administrator;
mtbese cases, save a water blank and ftnlinrtft* Admtn-
istrator1! direction* on analysis. Perform tbe acetone
rinse* M follows:
Carefully remove tbe probe Book and clean tbe Inside
surface by rinsing with acetone bom a wash bottle and
brushing witb a nylon bristle brosb. Brush until tbe
acetone rime shows no visible particles, after whleh
make a final riBee el tbe Inside surface with acetone.
Brush and rinse tbe Inside parts of tbe Swagelok
fitting with acetone la » xwUar way BatO-no vWbkV
panicles remain.
Blnee tbe prab* liner wttfc aeetem ky tOttaia; aod
rotating the probe while squirting acetone Into ita upper
end so that aU inside surfacesTwffl be wetted1 with ace-
tone. Let the acetone drain from tbe lower end lot* the
sample container. A tartwi (glass or polyethylene) mar
be used to aid In transferring liquid wasbet to tbe con-
tainer, follow tbe acetone rinse with a probe braatk
Hold the probe In an Inclined posltien, jqoirt aeetooa
into the upper end as tbe probe brash is being pushed
with a twisting action through tbe probe; bold a ample
container underneath tbe lower end of tbe probe, and
eatcb any acetone and paniculate matter which 1»
brushed from tbe probe. Run the brash through the
probe three times or more until aa visible partfeolate
matter is carried out with the acetone or until none
i-«iTT»ain« tn jj|0 pcooa liner oa T4""1 limpet liiiii WHfe>
stainless steel or other. *"*»**! probes, run tha brash
tbrongh in the above prescribed manner at least six
times since metal probes have small crevices In which
paniculate matter can be entrapped. Rinse the brush
with acetone, and quantitatively collect these washings
in tbe sample container. After the crashing, make a
final aeeftoa*. rinse of the probe as described above.
It Is neomowBded tkat two people be need to dean
the prob* tB mmimlas sample kisses. Between samplinc
runs, keep brushes clean and protected from eontamiaay
tion.
After ensuring tint an Joints have been wiped clean
of silicons grease, clean tbe inside of tbe front half of tbe
filter holder by rubbing tbe surfaces with a nylon bristle
brush and rinsing witb acetone. Rinse each surfaes
three times or more If needed* to remove visible parthm-
l&te. Make a final rinse of the brush and niter holder.
Carefully rinse out tbe glass cyclone, also (if applicable).
After all acetone washings and partlculate matter have
been collected In the sample container, tighten tbe lid
en tbe sample container so that acetone will not leak
out when It Is snipped to the laboratory. Mark tbe
height of the fluid leve! to determine whether or not
leakage occurred during transport. Label tbe container
to clearly identify its contents.
Cvnlamer Wo. i. Note tbe color of tbe Indicating silica
gel to determine if it has been completely spent and make
a notation of its condition. Transfer the silica gel from
tbe fourth Impinger to Its original container and seal.
A funnel may make it easier to pour the silica gel withont
spilling. A rubber policeman may be used as an aid in
removing tbe silica gel from tbe impinger. It Is not
necessary to remove the small amount of dust psrticlsa
that may adhere to the impinger wan and are difficult
to remove. Since tbe gain in weight is to be used for
moisture calculations, do not use any water or other
liquids to transfer tbe silica gel. If a balance is available
in the field, follow the procedure for container No. S
in Section 4.3.
Imptata Water. Treat tbe implngers as follows; Main
a notation of any color or nlm in tbe Uquid catch. Measure
tbe liquid which is in tbe first three impingers to within
=•1 ml by using a graduated cylinder or by weighing it
to within »0.5 g by using a balance (if one is available).
Record tbe volume or weight of liquid present. This
information is required to calculate tbe moisture content
of the effluent gas.
Discard the Uquid after measuring and recording tbe
volume or weight, unless analysis of tbe impinger catch
is required (see Note, Section 2.1.7).
If a different type of condenser U used, measure tbe
amount of moisture condensed either volumetricanj or
gravimetricaUy.
Whenever possible, containers should be shipped In
such a way that they remain upright at all times.
4.3 Analysis. Record the data required on a sheet
sucb as the one shown in Figure 5-3. Handle each sample
container as follows:
Container No. 1. Leave the contents in the shipping
container or transfer tbe filter and any loose paniculate
from the sample container to a tared glass weighing dish.
Desiccate (or 24 hours in a desiccator containing anby-
• drous calcium snlfate. Weigh to a constant weight and
report the results to tbe nearest 0.1 mg. For purposes of
this Section, 4.3, tbe term "constant weight" means a
difference of no more than 0.5 mg or 1 percent of total
weight less tare weight, whichever Is greater, between
two consecutive weighings, witb no less than ( boon of
desiccation time between weighings.
RULES AMB BEGULATIOMS
Section No. 3.4.10
Revision No. 0
Date January 15, 1980
P.age 4 of 6
RUM Ho..
filter No..
Amount liquid lost during transport
Acetone Uank volume, ml
Acetone wash volume, ml
Acetone blank concentration, mg/mg (equation 5-4}_
Acetone wash blank, mg (equation 5-5)
CONTAINER
NUMBER
1
^
TOTAL
WEIGHT OF PARTICULATE COLLECTED.
mft
FINAL WEIGHT
Less acetoi
Weight of p
TARE WEIGHT
hxr
ie btank
irticulate matter
WEIGHT GAIN
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME,
rot
SILICA GEL
WEIGHT,
9
9*1 •»
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER (1g/ml);
INCREASE, g . VOLUi|E WATER ^
1 g/mt
Figure 5-3. Analytical data.
FDEIAL UCISTH. VOt. 4S. NO. 160—THUISDAY,. AUGUST I*, 1*7?
-------
Section No. 3.4.10
Revision No. 0
Date January 15, 1980
RULES AND REGULATIONS page 5 of 6
41781
Alternatively, the sample may be oven dried at 105° C
(220° F) for 2 to 3 hours, cooled in the desiccator, and
weighed to a constant weight, unless otherwise specified
by the Administrator. The tester may also opt to oven
dry the sample at 105 • C (220 ° F) for 2 to 3 hours, weigh
the sample, and use this weight as a final weight.
Container No. t. Note the level of liquid in the container
and confirm on the analysis sheet whether or not leakage
occurred during transport. If a noticeable amount of
leakage has occurred, either void the sample or use
methods, subject to the approval of the Administrator,
to correct the final results. Measure the liquid in this
container either volumetrically to ±1 ml or gravi-
metrically to ±0.5 g. Transfer the contents to a tared
250-ml beaker and evaporate to dryness at ambient
temperature and pressure. Desiccate for 24 hours and
weigh to a constant weight. Report the results to the
nearest 0.1 me.
Container No. i. Weigh the spent silica gel (or silica gel
plus impinger) to the nearest 0.5 g using a balance. This
step may be conducted in the field.
"Acetone Blank" Container. Measure acetone in this
container either Tolumetrieally or gravimetrically.
Transfer the acetone to a-tared 250-ml beaker and evap-
orate to dryness at ambient temperature and pressure.
Desiccate for 24 hours and weigh to a contsant weight.
Eeport the results to the nearest 0.1 rag.
NOTE.—At the option •( the tester, the contents of
Container No. 2 as well as the acetone blank container
may be evaporated at temperatures higher than ambi-
ent. If evaporation is done at an elevated temperature,
the temperature must be below the boiling point of the
solvent; also, to prevent "bumping," the evaporation
process must be closely supervised, and the contents of
the beaker must be swirled occasionally to maintain an
even temperature. Use extreme care, as acetone is highly
flammable and has a low flash point.
t. CM&racfem
Maintain a laboratory log of all calibrations.
5.1 Probe Noiile. Probe nozcles shall be calibrated
before their Initial use in the field. Using a micrometer,
measure the inside diameter of the noule to the nearest
0.025 TTITTI (0.001 in.). Make three separate measurements
using different diameters each time, and obtain the aver-
age of the measurements. The difference between the high
and low numbers shall not exceed 0.1 mm (0.004 in.).
When noizles become nicked, dented, or corroded, they
Shall be reshaped, sharpened, and recalibrated before
use. Each noczle shall be permanently and uniquely
identified.
5.2 Pilot Tube. The Type 8 pilot tube assembly shall
be calibraled according lo the procedure outlined in
Section 4 of Method 2.
6.3 Metering System. Before its initial use in the field,
the metering syslem shall be calibrated according to the
procedure outlined in APTD-0576. Instead of physically
adjusting Ihe dry gas meter dial readings to correspond
to the wet test meter readings, calibration factors may be
used to mathematically correct the gas meter dial readings
to the proper values. Before calibrating Ihe melering sys-
tem, it is suggested thai a leak-check be conducted.
For metering systems having diaphragm pumps, the
normal leak-check procedure will not detect leakages
within the pump. For these cases the following leak-
check procedure is suggested: make a 10-minute calibra-
tion run at 0.00057 m '/min (0.02 eta); at the end of the
run, take the difference of the measured wet test meter
and dry gas meter volumes; divide the difference by 10.
to get the leak rate. The leak rate should not exceed
0.00057 m »/min (0.02 dm).
After each field use, the calibration of the metering
system shall be checked by performing three calibration
runs at a single, intermediate onfice setting (based on
the previous field test), with the vacuum set at the
maximum value reached during the test series. To
adjust the vacuum, insert a valve between the wet test
meter and the inlet of the metering system. Calculate
the average value of the calibration factor. If the calibra-
tion has changed by more than 5 percent, recalibrate
the meter over the full range of orifice settings, as out-
lined in APTD-0576.
Alternative procedures, e.g., using the orifice meter
coefficients, may be used, subject to the approval of the
Administralor.
NOTE.—If the dry gas meter coefficient values obtained
before and after a test senes differ by more than 5 percent,
the test series shall either be voided, or calculations for
the test series shall be performed using whichever meter
coefficient value (i.e., before or after) gives the lower
value of total sample volume.
5.4 Probe Heater Calibration. The probe beating
system shall be calibrated before its initial use in the
field according to the procedure outlined in APTD-0570.
Probes constructed according to APTD-0581 need not
be calibrated If the calibration curves In APTD-0576
are used.
5.5 Temperature Gauges. Use the procedure in
Section 4.3 of Method 2 to calibrate In-slack temperature
gauges. Dial thermometers, such as are used for the dry
gas meter and condenser outlet, shall be calibrated
against mercury-in-glass thermometers.
5.6 Leak Check of Metering System Shown In Figure
8-1, That portion of the sampling train from the puinp
to the orifice meter should be leak checked prior to initial
use and after each shipment. Leakage after the pump will
result in less volume being recorded than is actually
sampled The following procedure Is suggested (see
Figure 5-4): Close the main valve on the meter box.
Insert a one-hole rubber stopper with rubber tubing
attached into the orifice exhaust pipe. Disconnect and
vent the low side of the orifice manometer. Close off the
low side orifice tap. Pressurite the system to 13 to 18 cm
<5 to 7 in.) water column by blowing into the rubber
tubing. Pinch off the tubing and observe the manometer
for one minute. A loss of pressure on the manometer
Indicates a leak in the meter box; leaks, If present, must
be corrected.
5.7 Barometer. Calibrate against e mercury barom-
eter.
6. Calculation!
Carry out calculations, retaining at least one extra
decimal figure beyond that of the acquired data. Round
off figures after the final calculation. Other forms of the
equations may be used as long as they give equivalent
results.
RUBBER
TUBING
RUBBER
STOPPER
ORIFICE
BY-PASS VALVE
VACUUM
GAUGE
BLOW INTO TUBING
UNTIL MANOMETER
READS 5 TO 7 INCHES
WATER COLUMN
ORIFICE
MANOMETER
AIR-TIGHT
PUMP
Figure 5-4. Leak check of meter box.
IL 1 Nomenclature
A, —Cross-sectional area of aotcle, m' (ft1).
J3- -Water vapor in the gas stream, proportion
by volume.
Cm —Acetone blank residue concentrations, mg/g.
c. —Concentration of paniculate matter in stack
gas, dry basil, corrected to standard oondi-
7 —Percent of isokinette sampling.
L, — Max imum acceptable leakage rate for either a
Pretest leak check or for a leak check fbUow-
ig a component change; equal to 0.00057
m'/min (0.02 cfm) or 4 percent of the average
sampling rate, whichever is less.
Lt —Individual leakage rate observed during the
leak check conducted prior to the N^"
component change (<—1, 2, 3 .... B),
m'/min (cfm).
L, —Leakage rate observed during the post-test
leak check, mVnun (cfm). '
*.. —Total amount of paniculate matter collected,
• »g.
H, —Molecular weight of water, 18.0 g/g-mol»
(IS.OlbAb-mole). .
•. —Mass of residue of acetone after evaporation,
mg.
Pmm, —Barometric pressure at the sampling site,
mm Hg (in. Hg).
P, —Absolute stack gas pressure, mm Hg (In. Hg).
PM —Standard absolute pressure, TOO mm Hg
(29.92 in. Hg).
1 gas constanl, 0.06236 mm Hg-m*/°IC-f-
i (21.86 in. Hg-ft'/°B4b-mole).
X -Ideal
mole
Tm —Absolute average dry gas meter temperature
(see Figure 5-2), °K (°B).
T, —Absolute average stack gas temperature (see
Figure 6-2), 'K (°K).
TM -Standard absolute temperature, 291* K
(528° R).
V, —Volume of acetone blank, ml.
Vmw —Volume of acetone used in wash, mL
Vi.=Total volume of liquid collected in tmpingen
and silica gel (see Figure 6-1), ml.
F.-Volume of gas sample as measured by dry (*s
meter, dcm (dcf).
F.<,u)=Volume of gas sample measured by the dry
fas meter, corrected to standard conditions,
dscm (dscf).
Vmiun =-Volume of water vapor in the gas sample,
corrected to standard conditions, scm (scf). '
V.=Stack gas velocity, calculated by Method 2,
Equation 2-4, using data obtained from
Method 5, m/sec (ft/sec).
IP.=Weight of residue in acetone wash, mg.
K—Dry gas meter calibration factor.
AH- Average pressure differential across the orifice
meter (see Figure 6-2), mm HiO On. HiO).
p.—Density of acetone, me/ml (see label on
bottle).
^.-Density of water, 0.9082 (/ml 01.002301
Ib/ml).
»—Total sampling time, min
$1=Sampling time Interval, from the beginning
of a run until the first component change,
min.
«,=Sampling time Interval, between two suc-
cessive component changes, beginning with
the interval between the first and second
changes, min.
»,= Sampling ttme Interval, from the final (n'>>)
component change until the erfd of the
sampling run, min.
IS.6 = Specific gravity of mercury.
60= Sec/nun.
100=Conversion to percent.
(.2 Average dry gas meter temperature and average
orifice pressure drop. See data sheet (Figure 5-2).
«.! Dry Oas Volume. Correct the sample volume
measured by the dry gas meter to standard conditions
W C, 760 mm Hg or 68° F, 29.92 in. Hg) by using
Equation 5-1.
Ptot+(Ag/13.6)
Equation 5-1
FEDERAL REGISTER, VOl. 42, NO. 160—THURSDAY, AUGUST 10, 1977
-------
41782
RULES AND REGULATIONS
where:
.£,-0.001333 n>'/ml tor metric onrta
-0.04707 ftl/ml lor English units.
U Moisture Content
B..=
V,
(•Kfi
Section No. 3.4.10
.Revision No. 0
Date January 15, 1980
Page 6 of 6
nu-0.386i*r/mm Hf lot metric unite
-17.M *B/ln. Hf for English unit*
NOTE.—Equation 5-1 can be used as -written unless
tbe leakage rate observed during any at tbe mandatary
leak checks (I.e., tbe post-test leak check or leak checks
conducted prior to component changes) exceeds L_ II
L, at In exceed! -£., Equation 5-1 must be modlned-ai
follow*;
(a) Can I. No component changes mad* dnrin«
sampling run. In this case, replace Vm in Equation 4-1
with the expression;
Vm-(Lr-L.)»\
(b) Case H. One or more component changes mad*
daring the sampling run. In Utii cue, rvptac* V«, 1m
SqnAtion 6-1 by the expressMn:
Norm.—In saturated or water droplet-laden gat
streams, two calcoJattaM ol tbe moisture content of th»
stack gas shall be made, one (rom tbe Implnger analysts.
(Equation »-»). and a second (ram tbe assumption at
saturated conditiona. Tbe lower at the two values «f
B.. shall be considered correct. Tbe procedure (or deter-
mining tbe moisture content based upon assumption at
saturated eonditiona is given In tbe Note of Section 1J
of Method 4. For tbe purposes a! this method, tbe average
stack gas temperature from Figure 5-2 may be used tn
make this determination, provided that tbe accuracy ot
tbe in-stack temperature sensor la ± 1* C (3° t).
6.» Acetone Blank Concentration.
C.=
Acetens Wash Blank
Equation 5-4
and substitute only lor those leakage rates (Li at I*)
which exoeed .£„
8.4 Volume of water vapor.
ZqnationS-J
Equation M
8J Total Particulate Weight Determine the total
particnlate catch from tbe sum of the weights obtained
from containers 1 and 2 leas tbe acetone blank (see Figure.
*-»). Nora.—Refer to Section 4.1.5 to assist In calculation
of results Involving two or more niter assemblies or two
or more sampling trains.
84 Particulste Concentration.
«V=( 0.001 ff/mg}
KcraatianJ-*
Multiply b»
T»
g/(t*
g/(f
m*
15.43
1208X1*^
Equation 4-3
e.ll laoklnetle Variation.
8.11.1 Calculation From Raw Data,
where:
JTi-0.003454 mm Hg-m'/ml-'E for metric onrta.
-0.0036«8 la. Hf-ff Anl-*R for English nnlU.
8.11.J Calculation Prom Intermediate Values.
60 it. P. An EquatienW
8. VoOara, B. F. A Survey of Commercially Available
Instrumentation For the Measurement of Law-Rang*
Gas Velocities. U.S. Environmental Protection Agencrv
Emission Measurement Branch. Research Triangla-
Park, N.C. November, 1978 (unpublished paper).
9. Annual Book of ASTM Standards. Part STaaseoua
Fuel*; Coal and Coke; Atmospheric Analyst*. American
Society for Testing and Material*. Philadelphia, Pa.
1974. pp. 817-622.
where:
J&-4JSX tor metric units
-O.UM50 (or English anils.
8.13 Acceptable Reenlts. If M percent < I <110 per-
cent, tbe results are acceptable. If the results are kjw tn
comparison to tbe standard and / ia beyond tbe accept-
able range, or, If / la less than 90 percent, the Adminis-
trator may opt to accept tbe results. Use Citation 4 to
make judgments. Otherwise, reject the results and repeat
tbe teat.
7. Btbttoqraplif
1. Addendum to Specifications tot Incinerator Testing
at Federal Facilities. PHS^ NCAPC. Dec. 8, 1967.
2. Martin, Robert M. Construction Details ol Iso-
kinetla Source-Sampling Equipment. Environmental
Protection Agency. Research Triangl* Park, N.C.
APTD-0681. April, 1971.
3. Rom, Jerome J. Maintenance, Calibration, and
Operation of laoklnetic Source Sampling Equipment.
Environmental Protection Agency. R«e«arch Triangle
Park, N.C. APTD-0678. March, 1972.
4. Smith. W. 8., R. T. Sbigehara, and W. Tf. Todd.
A Metbod of Interpreting Stack Sampling Data. Paper
Presented at tb« 83d Annual Meeting oi th« Air PoUn-
tion Control Association, St. Louis. Mo. June !«-!«,
ia*x
6. Smith, W. 8.. et a!. Stack Oat Sampling Improved
tat Simplified With New Equipment. APCA Paper
No. «7-119.1967.
i. SpecincaOona tor Incinerator Teeting at Federal
raaffltie*. PH8, NCAPC. 19«J.
7. SnlKehara, R. T. Adjustments In tbe EPA Mono-
graph (or Different Pitot Tub* Coeftoimts and Dry
Melecnlar Weights. Stack 8aapUn( New* t>4-ll.
October, 1974.
FEDERAL IEGISTH, VOL. 42, NO. 160—THURSDAY, AUGUST 1*. 1977
-------
Section No. 3.4.11
Revision No. 0
Date January 15, 1980
Page 1 of 2
11.0 REFERENCES
1. Standards of Performance for New Stationary Sources,
Federal Register, Vol. 42, No. 160. August 18, 1977.
2. Hamil, H. F. and R. E. Thomas. Collaborative Study of
Particulate Emissions Measurements by EPA Methods 2, 3,
and 5 using Paired Particulate Sampling Trains. EPA-
600/4-76-014. Environmental Protection Agency, Re-
search Triangle Park, N.C., March 1976.
3. Martin, R. M. Construction Details of Isokinetic
Source Sampling Equipment. Publication No. APTD-0581.
Air Pollution Control Office, EPA, Research Triangle
Park, N.C., 1971.
4. Rom, J. J. Maintenance, Calibration, and Operation of
Isokinetic Source Sampling Equipment. Pub No. APTD-
0576. Office of Air Programs, EPA, Research Triangle
Park, N.C., 1972.
5. Midgett, M. R. The EPA Program for the Standardization
of Stationary Source Emission Test Methodology, A Re-
view. EPA-600/4-76-044. Environmental Protection
Agency, Research Triangle Park, N.C., August 1976.
Additional References
Smith, Franklin, and Denny E. Wagoner. Guidelines for Develop-
ment of a Quality Assurance Program: Volume IV - Determination
of Particulate Emissions from Stationary Sources. Contract No.
68-02-1234, EPA-650/4-74-005-d. Research Triangle Institute,
Research Triangle Park, N.C., August 1974.
Highlights of August 18, 1977, Revisions to EPA Reference Methods
1-8. Entropy Environmentalists, Inc. Research Triangle Park, N.
C. (for EPA).
USEPA. Public Comment Summary: Revisions to Reference Methods
1-8 in Appendix A of Standards of Performance for New Stationary
Sources. Environmental Protection Agency, Research Triangle
Park, N.C., June 1977.
Vollara, Robert F. An Evaluation of the Current EPA Method 5
Filtration Temperature - Control Procedure. Environmental Pro-
tection Agency, Research Triangle Park, N.C.
-------
Section No. 3.4.11
Revision No. 0
Date January 15, 1980
Page 2 of 2
Hamil, Henry F., and David E. Camann. Collaborative Study of
Method for the Determination of Particulate Matter Emissions from
Stationary Sources (Portland Cement Plants). Contract No.
68-02-0626, EPA-650/4-74-029. Southwest Research Institute, San
Antonio, Texas, May 1974.
Hamil, Henry F. , and Richard E. Thomas. Collaborative Study of
Method for the Determination of Stack Gas Velocity and Volumetric
Flow in Conjunction with EPA Method 5. Contract No. 68-02-0626,
EPA-650/4-74-013. Southwest Research Institute, San Antonio,
Texas, May 1974.
Hamil, Henry F., and Richard E. Thomas. Collaborative Study of
Method for the Determination of Particulate Matter Emissions from
Stationary Sources (Fossil Fuel-Fired Steam Generators). Con-
tract No. 68-02-0623, EPA-650/4-74-021. Southwest Research
Institute, San Antonio, Texas, June 1974.
Hamil, Henry F., and Richard E. Thomas. Collaborative Study of
Method for Stack Gas Analysis and Determination of Moisture
Fraction with Use of Method 5. Contract No. 68-02-0626, EPA-650/
4-74-026. Southwest Research Institute, San Antonio, Texas, June
1974.
Mitchell, William J., and M. Rodney Midgett. Method for Obtain-
ing Replicate Particulate Samples from Stationary Sources. EPA-
600/4-74-025. Environmental Protection Agency, Research Triangle
Park, N.C., June 1975.
Hansen, H. A., R. J. Davini, J. K. Morgan, and A. A. Iverson.
Particulate Sampling Strategies for Large Power Plants Including
Npnuniform Flow. EPA-600/2-76-170. FluiDyne Engineering Corp.,
Minneapolis, Minnesota, June 1976.
Peters, Edward T., and Jeffrey W. Adams. Evaluation of Station-
ary Source Particulate Measurement Methods: Volume II - Oil-
Fired Steam Generators. Contract No. 68-02-0632, EPA-600/
2-77-026. Arthur D. Little, Inc., Cambridge, Massachusetts,
February 1977.
Hanson, H. A. and D. P. Saari. Effective Sampling Techniques for
Particulate Emissions from Typical Stationary Sources - Interim
Report. Contract No. 68-02-1796, EPA-600/2-77-036. FluiDyne
Engineering Corp., Minneapolis, Minnesota, February 1977.
-------
Section No. 3.4.12
Revision No. 0
Date January 15, 1980
Page 1 of 21
12.0 DATA FORMS
Blank data forms are provided on the following pages for the
convenience of the Handbook user. Each blank form has the cus-
tomary descriptive title centered at the top of the page. How-
ever, the section-page documentation in the top right-hand corner
of each page of other sections has been replaced with a number in
the lower right-hand corner that will enable the user to identify
and refer to a similar filled-in form in the text section. For
example, Form M5-1.2 indicates that the form is Figure 1.2 in
Section 3.4.1 of the Method 5 Handbook. Future revisions of
these forms, if any, can be documented by 1.2A, 1.2B, etc.
Fourteen of the blank forms listed below are included in this
section. Five are in the Method Highlights Section as shown by
the MH following the form number and one is left blank in the
text.
Form Title
1.2 Procurement Log
2.3A & B Dry Gas Meter Calibration Data Form
(English and Metric units)
2.4A & B Posttest Meter Calibration Data Form
(English and Metric units)
2.5 Stack Temperature Sensor Calibration
Data Form
2.6 Nozzle Calibration Data Form
3.1 (MH) Pretest Sampling Checks
3.2 (Text) General Pretest Checklist
4.1 Nomograph Data Form
4.2 Particulate Field Data Form
4.3 Sample Label
4.4 Sample Recovery and Integrity Data Form
4.5 (MH) On-Site Measurement Checklist
5.1 (MH) Posttest Calibration Checks
5.2 Analytical Balance Calibration Data Form
-------
Section No. 3.4.12
Revision No. 0
Date January 15, 1980
Page 2 of 21
Form Title
5.3 Sample Analytical Data Form
5.4 Blank Analytical Data Form
5.5 (MH) Procedure for Weighing Filters Before and
After Sampling
5.6 (MH) Procedure for Analysis of Acetone Rinse
Samples
6.1A & 6.IB Particulate Calculation Data Form
(English and Metric units)
8.1 Method 5 Checklist To Be Used by Auditors
-------
PROCUREMENT LOG
Item description
( uantity
Purchase
order
number
Vendor
Date
Ordered
Received
Cost
Dispo-
sition
Comments
Quality Assurance Handbook M5-1.2
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM
(English units)
Date
Barometric pressure, P, =
Orifice
manometer
setting
(AH),
in. H20
0.5
1.0
1.5
2.0
3.0
4.0
Gas volume
Wet test
meter
(V ) ,
fl3
5
5
10
10
10
10
Dry gas
meter
f
1 " Pb (td + 460) V»
If there is only one thermometer on the dry gas meter, record the temperature
under t,.
d
Quality Assurance Handbook M5-2.3A (front side)
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM (English units)
Nomenclature:
3
V = Gas volume passing through the wet test meter, ft .
W
V^ = Gas volume passing through the dry gas meter, ft .
t = Temperature of the gas in the wet test meter, °F.
W
t, = Temperature of the inlet gas of the dry gas meter, °F.
t, = Temperature of the outlet gas of the dry gas meter, °F.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average t, and
U 0. Or-. U •
td , F. l
o
AH = Pressure differential across orifice, in. H20.
Y. = Ratio of accuracy of wet test meter to dry gas meter for each run. Tolerance Y- =
Y ±0.02 Y. 1
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs.
Tolerance Y = Y ±0.01 Y.
AH@. = Orifice pressure differential at each flow rate that gives 0.75 ft /min of air at
standard conditions for each calibration run, in. H20. Tolerance = AH@ ±0.15
(recommended).
3
AH@ = Average orifice pressure differential that gives 0.75 ft /min of air at standard
conditions for all six runs, in. H2O. Tolerance = 1.84 ±0.25 (recommended).
0 = Time for each calibration run, min.
P, = Barometric pressure, in. Hg.
Quality Assurance Handbook M5-2.3A (backside)
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM
(Metric units)
Date
Barometric pressure, P, =
Meter box number
mm Hg Calibrated by
Orifice
manometer
setting
(AH),
mm HO
10
25
40
50
75
100
Gas volume
Wet test
meter
+ } (+ + 971"!
Vd(Pd + 13. 6^ (tw + 273)
0.00117 AH [(tw-273)012
^l@i P (t + 273) Vw
D U W
If there is only one thermometer on the dry gas meter, record the temperature
iinrlpr t
under t,.
d
Quality Assurance Handbook M5-2.3B (front side)
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM (metric units)
Nomenclature:
3
V = Gas volume passing through the wet test meter, m .
W
3
Vd = Gas volume passing through the dry gas meter, m .
t = Temperature of the gas in the wet test meter, °C.
W
t, = Temperature of the inlet gas of the dry gas meter, °C.
t, = Temperature of the outlet gas of the dry gas meter, °C.
o
t, = Average temperature of the gas in the dry gas meter, obtained by the average of td and
t- °r i
V
AH = Pressure differential across orifice, mm H20.
Y- = Ratio of accuracy of wet test meter to dry gas meter for each run. Tolerance Y, =
1 Y +0.02 Y.
Y = Average ratio of accuracy of wet test meter to dry gas meter for all six runs.
Tolerance Y = Y +0.01 Y.
3
AH@. = Orifice pressure differential at each flow rate that gives 0.021 m of air at standard
1 conditions for each calibration run, mm H20. Tolerance AH@^ = AH@ +3.8 mm H20
(recommended).
3
AH@ = Average orifice pressure differential that gives 0.021 m of air at standard con-
ditions for all six runs, mm H20. Tolerance AH@ = 46.74 +6.3 mm H20 (recommended).
0 = Time of each calibration run, min.
P, = Barometric pressure, mm Hg.
Quality Assurance Handbook M5-2.3B (backside)
-------
POSTTEST DRY GAS METER CALIBRATION DATA FORM (English units)
Test numbers Date Meter box number Plant
in. Hg Dry gas meter number
Pretest Y
Orifice
manometer
setting,
(AH),
in. H20
D —
Gas volume
Wet test
meter
(v<4'
ft-3
10
10
10
Dry gas
meter
(V>
ftj
Temperature
Wet test
meter
-------
Test numbers
POSTTEST METER CALIBRATION DATA FORM (Metric units)
Date Meter box number Plant
Barometric pressure, P, =
mm Hg Dry gas meter number
Pretest Y
Orifice
manometer
setting,
(AH),
mm HO
Gas volume
Wet test
meter
"„>•
m
.3
.3
.3
Dry gas
meter
cvd>,
m
Temperature
Wet test
meter
-------
STACK TEMPERATURE SENSOR CALIBRATION DATA FORM
Date
Thermocouple number
Ambient temperature
Calibrator
°C Barometric pressure
Reference: mercury-in-glass
other
in. Hg
Reference
point
number
Sourcea
(specify)
Reference
thermometer
temperature,
Thermocouple
potentiometer
temperature,
°C
Temperature
difference,
aType of calibration system used.
(ref temp, °C + 273) - (test thermom temp, °C + 273)1
ref temp, °C + 273 J
Quality Assurance Handbook M5-2.5
-------
NOZZLE CALIBRATION DATA FORM
Date
Calibrated by
Nozzle
identification
number
Nozzle Diameter3
Dl'
mm (in. )
D2'
mm tin. )
D3'
mm tin. )
AD,b
mm (in. )
D C
avg
where:
&D1 2 3
-•-1 *• i -j i
three different nozzles diameters, mm (in.); each
diameter must be within (0.025 mm) 0.001 in.
AD = maximum difference between any two diameters, mm (in.),
AD 1(0.10 mm) 0.004 in.
D
avg
= average of D^, D2, and D
Quality Assurance Handbook M5-2.6
-------
NOMOGRAPH DATA FORM (English units)
Plant
Date
Sampling location
Calibrated pressure differential across
orifice, in. H2O
Average meter temperature (ambient + 20°F), °F
Percent moisture in gas stream by volume, %
Barometric pressure at meter, in. Hg
Station pressure in stack, in. Hg
(P ±0.073 x stack gauge pressure, in. H,,0)
Ratio of static pressure to meter pressure
Average stack temperature, °F
Average velocity head, in. H~0
Maximum velocity head, in. H20
C factor
Calculated nozzle diameter, in.
Actual nozzle diameter, in.
Reference Ap, in. H?O
AH^
m
avg
B.
wo
'm
VP.
m
avg
Ap
avg
Ap.
max
Quality Assurance Handbook M5-4.1
-------
PARTICULATE FIELD DATA FORM
Plant Meter calibration
City Pitot tube (C )
Location
Operator
Date
fYl Sheet of
Nozzle
Probe length F Nozzle
identification number
diameter mm (in.)
Probe liner material Thermometer number 0
Probe heater setting Final 1
Run number Ambient
Stack dia
Sample bo
Meter box
Meter AH@
Traverse
point
number
m, mm (in.)
Baromet
Assumed
x number Static
number C Facto
temperature Vacuum
ric pressu
moisture
pressure (
r
re (P,) mm (in.) Hg
eak rate
during le
m /min (cfm)
ak check
mm (in.) Hg
Filter number
5 ) mm (in.)
a ••
H_0 Remarks
Reference AP mm (in.) H20
Sampling
time,
(9), min
Total
Clock
time,
(24 h)
Vacuum,
mm
(in.) Hg
Max
Stack
tempera-
ture
CT ),
°C(§F)
Avg
Velocity
head
(APs),
mm
(in.) H00
Pressure
differ-
ential
across
orifice
meter (AH),
mm
(in.) H,0
Gas sample
volume IV ),
3 , ... 3-.m
m (ft )
Total
Gas sample temp-
erature at dry
gas meter
Inlet,
°C(°F)
Avg
Outlet,
°C(°F)
Avg
Temperature
of gas
leaving
condenser or
last impinger,
°C (°F)
Max
Filter
temp,
°C(°F)
Quality Assurance Handbook M5-4.2
-------
SAMPLE LABEL
Plant City
Site Sample type
Date Run number
Front rinse Front filter Front solution
Back rinse Back filter Back solution
Solution Level marked
en
Volume: Initial Final "M
us
g
Clean up by Q)
Quality Assurance Handbook M5-4.3
-------
SAMPLE RECOVERY AND INTEGRITY DATA FORM
Plant Sample date
Sample location Run number
Sample recovery person Recovery date
Filter(s) number
MOISTURE
Impingers Silica gel
Final volume (wt) ml (g) Final wt g g
Initial volume (wt) ml (g) Initial wt g g
Net volume (wt) ml (g) Net wt g g
Total moisture g
Color of silica gel
Description of impinger water
RECOVERED SAMPLE
Blank filter container number Sealed
Filter container number Sealed
Description of particulate on filter
Acetone rinse Liquid level
container number marked?
Acetone blank Liquid level
container number marked?
Samples stored and locked
Remarks
Date of laboratory custody
Laboratory personnel taking custody
Remarks
Quality Assurance Handbook M5-4.4
-------
ANALYTICAL BALANCE CALIBRATION FORM
Balance name Number
classification of standard weights
Date
0.500 g
1.0000 g
10.0000 g
50.0000 g
100.0000 g
Analyst
Quality Assurance Handbook M5-5.2
-------
SAMPLE ANALYTICAL DATA FORM
Plant
Run number
Sample location
Relative humidity
Density of acetone (p )
a
g/ml
Sample
type
Acetone rinse
filter (s)
Sample
identifiable
Liquid level marked
and/or container sealed
Acetone rinse container number
Acetone rinse volume (V )
aw
Acetone blank residue concentration (C_)
cl ....
W - r V n - / } ( ) ( ) =
W ^•^V^nrrJ3 * '» ' * '
a a aw a
Date and time of wt Gross wt
Date and time of wt Gross wt
Average gross wt
Tare wt
Less acetone blank wt (W_)
Weight of particulate in acetone rinse (m_)
u "
Filter(s) container number
Date and time of wt Gross wt
Date and time of wt Gross wt
Average gross wt
Tare wt
Weight of particulate on filter (s) (m^)
Weight of particulate in acetone rinse
Total weight of particulate (m )
ml
mg/g
mg
mg
mg
mg
mg
mg
mg
mg
mg
mg
mg
mg
mg
mg
Note; In no case should a blank residue >0.01 mg/g or 0.001% of
the weight of acetone used be subtracted from the sample weight.
Remarks
Signature of analyst
Signature of reviewer
Quality Assurance Handbook M5-5.3
-------
BLANK ANALYTICAL DATA FORM
Plant
Sample location
Relative humidity
Liquid level marked and container sealed
Density of acetone (p ) 9/ml
cl •• ™ : "~ ' ~ --•--•""• --
Blank volume (V ) ml
a. '''" •"""• • """ ' "
Date and time of wt Gross wt mg
Date and time of wt Gross wt mg
Average gross wt mg
Tare wt mg
Weight of blank (m ,) mg
_ mab _ ( ) _ .
c=, - w TT~ ~ i \ i \ - rog/g
ci d
Note: In no case should a blank residue greater than 0.01 mg/g
(or 0.001% of the blank weight) be subtracted from the sample
weight.
Filters Filter number
Date and time of wt Gross wt mg
Date and time of wt Gross wt mg
Average gross wt mg
Tare wt mg
Difference wt mg
Note: Average difference must be less than ±5 mg or 2% of total
sample weight whichever is greater.
Remarks
Signature of analyst
Signature of reviewer
Quality Assurance Handbook M5-5.4
-------
PARTICULATE CALCULATION FORM (English units)
SAMPLE VOLUME (ENGLISH UNITS)
\7 =: "F"t~ T1 — °R "P —
m ' ' m '— ' bar *
Y = _ . , AH = _ . in. H20
/Pbar+ (AH/13.6)\
V , . ,, = 17.64 V Y( Dar _ )= . ftJ
m(std) m \ T /
Equation 6-1
PARTICULATE CONCENTRATION (ENGLISH UNITS)
mn = . _ mg
Cg = 2.205 x 10~6(^— )= _ . x 10~4 Ib/dscf
\ m(std)/ Equation 6-8
Quality Assurance Handbook M5-6.1A
-------
PARTICULATE CALCULATION FORM (metric units)
SAMPLE VOLUME (METRIC UNITS)
Vm = _ . m3, Tm = . OK, Pbar = . mm Hg
Y = _. , AH = . mm H2O
/Pbar+ (AH/13.6)\
Vm(std) = °-3858 Vm Y\ Tm J = - • m Equation 6-1
PARTICULATE CONCENTRATION (METRIC UNITS)
. _ mg
mn \
Cs = 1 x io'-—^ 1= . g/dscm
m(std)/ Equation 6-8
Quality Assurance Handbook M5-6.1B
-------
METHOD 5 CHECKLIST TO BE USED BY AUDITORS
Yes
No
Comment
OPERATION
Presampling Preparation
1. Knowledge of process conditions
2. Calibration of pertinent equipment:
in particular, the dry gas meter,
orifice meter, and pi tot tube
On-Site Measurements
3. Sample train assembly
4. Pretest leak check of train
5. Isokinetic sampling
6. Posttest check
7. Sample recovery and integrity
8. Recording of pertinent process
information during sample collec-
tion
Postsampling
9. Check of analytical balance
10. Use of acceptable detection blanks
in correcting field sample results
11. Calculation procedure/check
General Comments
Quality Assurance Handbook M5-8.1
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 1 of 13
Section 3.5
METHOD 6— DETERMINATION OF SULFUR DIOXIDE
EMISSIONS FROM STATIONARY SOURCES
OUTLINE
Section
SUMMARY
METHOD HIGHLIGHTS
METHOD DESCRIPTION
1. PROCUREMENT OF APPARATUS
AND SUPPLIES
2. CALIBRATION OF APPARATUS
3. PRESAMPLING OPERATIONS
4. ON-SITE MEASUREMENTS
5. POSTSAMPLING OPERATIONS
6. CALCULATIONS
7. MAINTENANCE
8. AUDITING PROCEDURE
9. RECOMMENDED STANDARDS FOR
ESTABLISHING TRACEABILITY
10. REFERENCE METHOD
11. REFERENCES
12. DATA FORMS
Number
Documentation of Pages
3.5
3.5
3.5.1
3.5.2
3. .3
3.5.4
3.5.5
3.5.6
3.5.7
3.5.8
3.5.9
3.5.10
3.5.11
3.5.12
3
9
15
15
6
12
16
6
3
7
1
3
2
13
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 2 of 13
SUMMARY
This Method 6 test procedure is applicable to the determina-
tion of sulfur dioxide emissions from stationary sources. A gas
sample is extracted from the sampling point in the stack. The
sulfur dioxide is separated from the sulfuric acid mist (includ-
ing sulfur trioxide) and is measured by the barium-thorin titra-
tion method. The barium ions react preferentially with sulfate
ions in solution to form a highly insoluble barium sulfate pre-
cipitate. When the barium has reacted with all sulfate ions,
excess barium then reacts with the thorin indicator to form a
metal salt of the indicator, resulting in a color change.
The minimum detectable limit of the method has been de-
termined to be 3.4 mg S02/m3 (2.12 x 10~7 Ib S02/ft3). Although
no upper limit has been established, tests have shown that concen-
3
trations as high as 80,000 mg S02/m can be collected efficiently
in two midget impingers, each containing 15 ml of 3% hydrogen
peroxide and the sampling rate is 1.0 £/min for 20 min. Based on
theoretical calculations, the upper concentration limit in a 20-£
sample is about 93,300 mg S02/m if two such impingers are used.
The limits may be extended by increasing the number of impingers
or by increasing the peroxide concentration.
Interferences include free ammonia, water-soluble cations,
and fluorides. The cations and fluorides are removed by glass-
wool filters and an initial isopropanol bubbler, and hence do not
affect the S02 analysis. When samples are being taken from a gas
stream with high concentrations of very fine metallic fumes (such
as from inlets to control devices), a high-efficiency glass-fiber
filter must be used in place of the glass-wool plug in the probe
to remove the cation interferences. Free ammonia interferes by
reacting with SO2 to form particulate sulfite and thus preventing
it from reaching the peroxide impingers, and by reacting with the
indicator. If free ammonia is present (as indicated by white
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 3 of 13
particulate matter in the probe and the isopropanol bubbler), an
alternative method, subject to the approval of the administrator
of the U.S. Environmental Protection Agency, is required.
The tester has the option of substituting sampling equipment
described in Method 8 for the midget impinger equipment of
Method 6. However, the Method 8 train must be modified to in-
clude a heated filter between the probe and the isopropanol
impinger and must be operated at the flow rates defined in
Method 8. The heated filter will help to eliminate the possibil-
ity of the SO2 reacting with the particulate matter.
The tester also has the option of determining the emissions
of SO2 simultaneously with particulate matter and moisture deter-
minations by (1) replacing the water in a Method 5 impinger
system with 3% peroxide solution or (2) replacing the Method 5
water impinger system with a Method 8 isopropanol-filter-peroxide
system. The analysis for S02 and the calibration of the metering
system must be consistent with the procedure in Method 8.
The method description that follows is based on the Refer-
ence Method that was promulgated on August 18, 1977, and ammended
March 23, 1978.
Section 3.5.10 contains a complete copy of the Reference
Method, and Section 3.5.12 provides blank data forms for the
convenience of the Handbook user. References are in Section
3.5.11. Reference 1 was used in preparing the method descrip-
tion. References 2, 3, and 4 are collaborative test studies of
this and other related methods. Data from these test studies
were used in establishing quality control limits using the tech-
niques of Reference 5. References 6 through 12 are included
because of their potential value to the user.
The accuracy of Method 6 was checked using three standard
3
gas mixtures containing 224, 1121, and 2082 mg 30,,/m (14, 70,
-6
and 130 x 10 Ib S02/scf), respectively. The individual meas-
urements by the participating laboratories were all within 24% of
the true concentration.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 4 of 13
The accuracy of the analytical phase of Method 6 was checked
using standard sulfuric acid solutions of three concentrations
that were equivalent to sampled concentrations of 281.9, 563.8,
and 845.7 mg S02/m3 (17.6, 35.2, and 52.8 x 10~6 Ib S02/scf), and
a blank solution. The individual measurements by all of the
participating laboratories were within 6% of the true concentra-
tion.
The estimated within-laboratory precision (relative standard
deviation) was 4.0%. The between-laboratory precision was 5.8%.
The relative standard deviation is the ratio of the standard
deviation of the measurement to the mean measured value, ex-
pressed as a percentage of this mean value.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 5 of 13
METHOD HIGHLIGHTS
Specifications described in this Method 6 (Section 3.5) are
only for the uses of midget impingers and midget bubblers with
sample rates of about 1 liter per minute (£/min). If the tester
opts to use the standard-sized impingers, the Method 8 descrip-
tion (Section 3.7) should be used as the reference for equipment
calibration, sample setup, leak check, operation, and sample
recovery. The only exceptions are that glass wool may be put in
the U-tube between the isopropanol and peroxide impinger as an
option to the filter, the sampling is to be conducted at a con-
stant rate of about 0.02 scm/min (0.75 scfm) (AH@, orifice pres-
sure differential that gives 0.75 scfm of air at 70°F at
29.92 in. Hg; and the isopropanol need not be analyzed.
The five blank data forms at the end of this section may be
removed from the Handbook and used in the pretest, test, and
the posttest operations. Each form has a subtitle (e. g.,
Method 6, Figure 3.1) for helping the user find a similar filled-
in form in the method description (Section 3.5.3). On the blank
and the filled-in forms, the items/parameters that can cause the
most significant errors are starred.
1. Procurement of Equipment
Section 3.5.1 (Procurement of Apparatus and Supplies) gives
the specifications, criteria, and design features of the equip-
ment and material required to perform Method 6 tests with the
midget impinger train. This section is designed to provide the
tester with a guide for the procurement and initial check of
equipment and supplies. The activity matrix (Table 1.1) at the
end of Section 3.5.1 can be used as a quick reference, and is a
summary of the corresponding written descriptions.
2. Pretest Preparations
Section 3.5.2 (Calibration of Apparatus) provides a step-by-
step description of the recommended calibration procedures. The
accuracy and precision for the equipment calibrations are the
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 6 of 13
same as those for Methods 5 and 8, with the exception that there
is no calibration requirement for the rotameter. The lower
sampling rate required for the midget impinger train allows the
use of a wet test meter with a capacity of 3 £/min or greater.
The calibration section can be removed along with the corre-
sponding sections for the other methods and used as a separate
quality assurance reference manual by the calibration personnel.
The calibration data are summarized on the pretest sampling
checks form (Figure 2.5, Section 3.5.2).
Section 3.5.3 (Presampling Operations) provides the tester
with a preparation guide for equipment and supplies for the field
test. The pretest sampling checks and pretest preparation forms
(Figure 3.1, Section 3.5.3) or appropriate substitutes should be
used as equipment checkout and packing lists. The sample
impingers may be charged in the base laboratory if the testing is
to be performed within 24 h of charging. The recommended method
described for packing the containers should help protect the
equipment.
3. On-Site Measurements
Section 3.5.4 (On-Site Measurements) contains step-by-step
procedures to perform the sampling and sample recovery. A check-
list (Figure 4.4, Section 3.5.4) is provided to assist the tester
with a quick method of checking that the procedures have been
completed satisfactorily. Section 3.5.4 may be taken to the
field for reference but it would not normally be needed by an
experienced crew. The most common problem with the midget
impinger train is that the hydrogen peroxide (H2O2) solution can
easily be backed up into the isopropanol solution. This causes
the SO, to be removed in the first impinger or in the glass wool.
£»
For this reason, it is important to take precautions in pre-
venting this occurrence, and it is suggested that the isopropanol
and glass-wool plug be saved. The isopropanol can then be
analyzed if any of the SO2 data indicate questionable results.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 7 of 13
4. Posttest Operations
Section 3.5.5 (Postsampling Operations) gives the posttest
equipment check procedures and a step-by-step analytical proce-
dure for determination of S02 concentration. The two posttest
data forms (Figure 5.1, Section 3.5.5) and Figure 5.4, Section
3.5.5) or similar forms should be used and the posttest sampling
checks form should be included in the emission test report to
document the calibration checks. The step-by-step analytical
procedure can be removed and made into a separate quality
assurance analytical reference manual for the laboratory per-
sonnel. Analysis of a control sample is required prior to the
analysis of the field samples. This analysis of an independently
prepared known standard will provide the laboratory with quality
control checks on the accuracy and precision of the analytical
techniques.
Section 3.5.6 (Calculations) provides the tester with the
required equations, nomenclature, and significant digits. It is
suggested that a programmed calculator be used, if available, to
reduce the chance of calculation error.
Section 3.5.7 (Maintenance) provides the tester with a guide
for maintenance procedures; these are not required, but should
reduce equipment malfunctions.
5. Auditing Procedure
Section 3.5.8 (Auditing Procedure) provides a description
of activities necessary for conducting performance and system
audits. The - performance audit of the analytical phase can be
performed using aqueous ammonium sulfate solution. Performance
audits for the analytical phase and the data processing are
described in Section 3.5.8. A checklist for a systems audit is
also included in this section.
Section 3.5.9 (Recommended Standards for Establishing Trace-
ability) recommends the primary standards for establishing the
traceability of the working standards. The volume measures are
compared to a primary liquid displacement method, and the analy-
sis of the SO- is traceable to primary standard grade potassium
acid pthalate.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 8 of 13
6. Reference Material
Section 3.5.10 (Reference Method) is the reference method
and thus the basis for the quality assurance method description.
Section 3.5.11 (References) is a listing of the references
that were used in this method description.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 9 of 13
PRETEST SAMPLING CHECKS
(Method 6, Figure 2.5)
Date Calibrated by
Meter box number AH@
Dry Gas Meter*
Pretest calibration factor = (within ±2% of average
factor for each calibration run).
Impinger Thermometer
Was a pretest temperature correction used? yes no
If yes, temperature correction ^ (within ±1°C (2°F) of
reference values for calibration and within ±2°C (4°F) of
reference values for calibration check).
Dry Gas Meter Thermometer
Was a pretest temperature correction made? yes no
If yes, temperature correction _j (within ±3°C (5.4°F) of
reference values for calibration and within ±6°C (10.8°F) of
reference values for calibration check).
Barometer
Was the pretest field barometer reading correct? yes no
(within ±2.5 mm (0.1 in) Hg of mercury-in-glass barometer).
Most significant items/parameters to be checked.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 10 of 13
PRETEST PREPARATIONS
(Method 6, Figure 3.1)
Apparatus check
Probe
Type liner
Glass
Stainless
steel
Other
Heated properly
Leak checked on
sampling train
Filter
Glass wool
Other
Glassware
Midget bubbler
Midget impinger
Size
Type
Meter System
Leak- free pumps*
Rate meter*
Dry gas meter*
Reagents
Distilled water
H202, 30%
Isopropanol, 100%*
Silica gel
Other
Barometer
Drying tube
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Loaded
and packed
Yes
No
* Most significant items/parameters to be checked.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 11 of 13
ON-SITE MEASUREMENTS
(Method 6, Figure 4.4)
Sampling
Bubbler and impinger contents properly selected, measured,
and placed in impinger?*
Impinger Contents/Parameters*
1st: 15 ml of 80% isopropanol
2nd: 15 ml of 3% ^2°2
3rd: 15 ml of 3% ^2°2
Final impinger dry?
Probe heat at proper level?
Crushed ice around impingers?
Pretest leak check at 250 mm (10 in.) Hg?
Leakage rate?
Probe placed at proper sampling point?
Flow rate constant at approximately 1.0 £/min?*
Posttest leak check at 250 mm (10 in.) Hg?*
Leakage rate?
Sample Recovery
System purged at least 15 min at test sampling rate?*
Contents of impingers placed in polyethylene bottles?
Fluid level marked?*
Sample containers sealed and identified?*
*
Most significant items/parameters to be checked.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 12 of 13
POSTTEST SAMPLING CHECKS
(Method 6, Figure 5.1)
Meter Box Number
Dry Gas Meter
Pretest calibration factor Y =
Posttest check Y, = Y2 = (+5% of pretest factor)*
Recalibration required? yes no
If yes, recalibration factor Y = (within +2% of calibra-
tion factor for each calibration run)
Lower calibration factor, Y = for pretest or posttest
calculations
Rotameter
Pretest calibration factor Y =
Posttest check Y = (within ±10% of pretest factor)
Recalibration recommended? yes no
If performed, recalibration factor Y =
Was rotameter cleaned? yes no
Dry Gas Meter Thermometer
Was a pretest meter temperature correction used? yes no
If yes, temperature correction
Posttest comparison with mercury-in-glass thermometer
within +6°C (10.8°F) of reference values
Recalibration required? yes no
Recalibration temperature correction if used within
+3°C (5.4°F) of reference values
If meter thermometer temperature is higher no correction needed
If recalibration temperature is higher, add correction to
average meter temperature for calculations
Barometer
Was pretest field barometer reading correct? yes no
Posttest comparison mm (in.) Hg within +5.0 mm
(0.2 in.) Hg) of mercury-in-glass barometer
Was recalibration required? yes no
If field barometer reading is lower, no correction is needed
If mercury-in-glass reading is lower, subtract difference from
field data readings for calculations
*Most significant items/parameters to be checked.
-------
Section No. 3.5
Revision No. 0
Date May 1, 1979
Page 13 of 13
POSTTEST OPERATIONS
(Method 6, Figure 5.4)
Reagents
Normality of sulfuric acid standard*
Date purchased Date standardized
Normality of barium perchlorate titrant*
Date standardized
Normality of control sample*
Date prepared
Volume of burette Graduations
Sample Preparation
Has liquid level noticeably changed?*
Original volume Corrected volume
Samples diluted to 100 ml?*
Analysis
Volume of aliquot analyzed*
Do replicate titrant volumes agree within 1% or 0.2 ml?
Number and normality of control samples analyzed
Are replicate control samples within 0.2 ml?
Is accuracy of control sample analysis ±5%?*
All data recorded? Reviewed by
*
Most significant items/parameters to be checked.
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 1 of 15
1.0 PROCUREMENT OF APPARATUS AND SUPPLIES
A schematic diagram of an assembled sulfur dioxide sampling
train with all components identified is shown in Figure 1.1.
Specifications, criteria, and design features are given in this
section to aid in the selection of equipment and to ensure that
the collected data are of good quality. Procedures and, where
applicable, limits for acceptance checks are given.
During the procurement of equipment and supplies, it is
suggested that a procurement log be used to record the descrip-
tive title of the equipment, the identification number, if appli-
cable, and the results of acceptance checks. An example of a
procurement log is shown in Figure 1.2. A blank form is given in
Section 3.5.12 for the Handbook user. If calibration is required
as part of the acceptance check, the data are recorded in the
calibration log book. Table 1.1 at the end of this section
summarizes the quality assurance activities for procurement and
acceptance of apparatus and supplies.
1.1 Sampling
1.1.1 Sampling Probe - The sampling probe should be either a
borosilicate (Pyrex) glass or a type-316 seamless stainless steel
tube of approximately 6-mm inside diameter (ID), encased in a
stainless steel sheath and equipped with a heating system capable
of preventing water condensation and with a filter (either in-
stack or heated out-stack) to remove particulate matter, includ-
ing sulfuric acid mist. When an in-stack filter is utilized, the
probe should have an expanded diameter (38-40 mm) for the first
4 cm on the in-stack end, and this expanded end should be packed
with glass wool prior to sampling. The probe's opposite end must
have a fitting suitable for attaching it to the midget bubbler.
A probe of approximately 1.2 m (4 ft) total length is usually
sufficient for sampling. However, the probe tip can be no closer
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 2 of 15
c
•H
(0
CP
C
•H
(0
CN
O
Q)
M
3
Cn
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 3 of 15
Jtl
s^^N V
Dispo-
sition
o
Vi
o
•a
cu
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 4 of 15
than 1 m (3.28 ft) from the inner wall of stacks >2 m in diame-
ter. When stack gas temperatures exceed 480°C (900°F), a probe
fabricated from quartz (Vycon) should be used. The main
criterion in selecting a probe material is that it be nonreactive
with the gas constituents and therefore not introduce bias into
the analysis.
A new probe should be visually checked for specifications
(i.e., the length and composition ordered). It should be checked
for cracks and breaks, and then leak checked on a sampling train,
as described in Section 3.5.3. The probe heating system should
be checked as follows:
1. Connect the probe (without filter) to the inlet of the
pump.
2. Electrically connect and turn on the probe heater for 2
or 3 min. If functioning properly, it will become warm to the
touch.
3. Start the pump and adjust the needle valve until a flow
rate of about 1.0 £/min is achieved.
4. Check the probe. It should remain warm to the touch.
The heater must be capable of maintaining the exit air
temperature at a minimum of 100°C (212°F) under these conditions.
If it cannot, the probe should be rejected. Any probe not
satisfying the acceptance check should be repaired, if possible,
or returned to the supplier.
1.1.2 Midget Bubbler/Impingers - Each sampling train requires
one midget bubbler (30 ml) of medium coarse glass frit, with
glass wool packed in the top to prevent carryover of sulfuric
acid mist. A midget impinger may be used in place of the midget
bubbler.
Each sampling train requires three midget impingers (30 ml)
with glass connections between the midget bubbler and the midget
impingers. (Plastic or rubber tubing is not permitted because
these materials absorb and desorb gaseous species.) Silicone
grease may be used to prevent leakage.
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 5 of 15
Each bubbler/impinger is checked visually for damage, such
as breaks or cracks, and for manufacturing flaws, such as poorly
shaped connections.
Other nonspecified collection absorbers and sampling flow
rates may be used, subject to the approval of the administrator,
but collection efficiency must be shown to be at least 99% for
each of three test runs and must be documented in the emission
test report. For efficiency testing, an extra absorber must be
added and analyzed separately and must not contain more than 1%
of the total SO2.
1.1.3 Vacuum Pump - The vacuum pump should be capable of main-
taining a flow rate of approximately 1 to 2 £/min for pump inlet
vacuums up to 250 mm (10 in.) Hg with the pump outlet near
standard pressure that is, 760 mm (29.92 in.) Hg. The pump must
be leak free when running and pulling a vacuum (inlet plugged) of
250 mm (10 in.) Hg. Two types of vacuum pumps are commonly
used—either a modified sliding fiber vane pump or a diaphragm
pump. For safety reasons, the pump should be equipped with a
three-wire electrical cord.
To check the pump for leaks, install a vacuum gauge in the
pump inlet line. Plug the inlet line and run the pump until the
vacuum gauge reads 250 mm (10 in.) Hg of vacuum, clamp the pump
outlet line and turn off the pump. The vacuum reading should
remain stable for 30 s.
1.1.4 Volume Meter - The dry gas meter must be capable of
measuring total volume with an accuracy of ±2%, calibrated at the
selected flow rate of 1.0 £/min and at the gas temperature
actually encountered during sampling, and must be equipped with a
temperature gauge (dial thermometer, or equivalent) capable of
measuring the gas temperature to within 3°C (5.4°F).
A new dry gas meter may be checked for damage visually and
by performing a calibration according to Section 3.5.2. Any drj
gas meter that is damaged, behaves erratically, or does not give
readings within +2% of the selected flow rate for each run is
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 6 of 15
unsatisfactory. Also upon receipt the meter should be calibrated
over a varying flow range to see if there is any effect on the
calibration.
Dry gas meters that are equipped with temperature compen-
sation must be calibrated over the entire range of temperature
that the meter encounters under actual field conditions. The
calibration must contain at least one data point at each 10°F
interval. All temperatures that are to be used in the field must
be within ±2% of the calibrated value.
The wet test meter used to check the dry test meter should
be calibrated using the primary displacement technique explained
in Section 3.5.2. The wet test meter must have a capacity of at
least 0.003 m3/min (0.1 ft3/min) with an accuracy of ±1%; other-
wise at the higher flow rates, the water will not be level and
possibly will result in an incorrect reading.
1.1.5 Rotameter - A rotameter, or its equivalent, with a range
of 0 to 2 A/min is used to monitor and control the sampling flow
rate. The rotameter is checked against the calibrated dry gas
meter with which it is to be used or against a wet test meter.
The rotameter flow setting of about 1 £/min should be determined.
Changes in pressure, density, and viscosity of the sample
gas will affect the calibrated sample rate. However, since
sampling is performed at a constant rate, which need not be
isokinetic, these changes do not affect the sample volume
measured by the dry gas meter.
1.1.6 Needle Valve - A metering valve with conveniently sized
fittings is required in the sampling train to adjust the sample
flow rate. It is recommended that the needle valve be placed on
the vacuum side of the pump.
1.1.7 Drying Tube - The drying tube should be packed with 6- to
16-mesh indicating-type silica gel, or equivalent, to dry the
sample gas and protect the meter and pump. A drying tube can be
made by filling a 10-mm polyethylene tube with silica gel and
packing glass wool in each end to hold the silicia gel and
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 7 of 15
protect the sampling system. Plastic tubing can be utilized in
any connections past the collection system without affecting the
sampling results. The drying tube should have a minimum capacity
of 30 to 50 g of silica gel and should be visually checked for
proper size and for damage.
If the silica gel has been used previously, it must be dried
at 175°C (350°F) for 2 h. New silica gel may be used, subject to
approval of the administrator.
1.1.8 Thermometers - A dial thermometer, or its equivalent, is
used to measure the temperature of gas leaving the impinger train
to within ±1°C (2°F). Dial type thermometers are easily damaged,
so each new thermometer must be checked visually for damage such
as a dented or bent stem. Each thermometer should read within
±1°C (2°F) of the true value when checked in an ice water bath
and at room temperature against a mercury-in-glass thermometer
that conforms to ASTM E-l No. 63C or 63F. Damaged thermometers
that cannot be calibrated must be rejected.
1.1.9 Meter System - For ease of use, the metering system—
which contains the dry gas meter, thermometer(s), vacuum pump,
needle valve, and rotameter—can be assembled into one unit
(meter box). After a meter box has been either constructed or
purchased, then positive and negative pressure leak checks should
be performed. The positive pressure leak check, similar to the
procedure described in Method 5 (Section 3.4), is performed as
follows:
1. Attach rubber tubing and inclined manometer, as shown
in Figure 1.3.
2. Shut off the needle valve and insert positive pressure
in the system by blowing into the rubber tubing until the in-
clined manometer or magnehelic gauge reads from 12.5 to 17.5 cm
(5 to 7 in.) H2O.
3. Pinch off the tube and observe the manometer for 1 min.
A loss of pressure indicates a leak of the apparatus in the meter
box.
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 8 of 15
u
0)
(0
CU
o
X!
0}
-p
0)
s
(U
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 9 of 15
After the meter box apparatus has passed the positive leak
check, then the negative leak check should be performed as fol-
lows:
1. Attach the vacuum gauge at the inlet to the drying
tube, and pull a 250 mm Hg (10 in.) vacuum.
2. Pinch or clamp the outlet of the flow meter. This can
be accomplished by closing the optional shutoff valve if em-
ployed.
3. Turn off the pump. Any deflection noted in the vacuum
reading within 30 s indicates a leak.
4. Carefully release the vacuum gauge before releasing the
flow meter end.
If either of these checks detects a leak that cannot be cor-
rected, the meter box must be rejected and/or returned to the
manufacturer.
The dry gas meter must be equipped with a temperature gauge
(dial thermometer or equivalent). Each thermometer is checked
visually for damage, such as dented or bent face or stem. Each
thermometer should read within ±3°C (5.4°F) of the true value
when checked at two different ambient temperatures against a
mercury-in-glass thermometer that conforms to ASTM E-l No. 63C or
63F. The two ambient temperatures used to calibrate the ther-
mometer must differ by a minimum of 10°C (18°F). Damaged ther-
mometers that cannot be calibrated are to be rejected.
1.1.10 Barometer - A mercury, aneroid, or other barometer
capable of measuring atmospheric pressure to within 2.5 mm (0.1
in.) Hg may be used. However, in many cases, the barometric
reading can be obtained from a nearby National Weather Service
Station, in which case the station value (which is the absolute
barometric pressure) is requested. The tester should be aware
that the pressure is normally corrected to sea level. The
station value is the uncorrected reading. An adjustment for
differences in elevations of the weather station and sampling
point is applied at a rate of -2.5 mm Hg/30 m (-0.1 in. Hg/100
ft) of elevation increase, or vice versa for elevation decrease.
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 10 of 15
Accuracy can be ensured by checking the field barometer
against a mercury-in-glass barometer or its equivalent. If the
field barometer cannot be adjusted to agree with the mercury-
in-glass barometer, it is not acceptable.
1.1.11 Vacuum Gauge - At least one 760-mm (29.92-in.) Hg gauge
is necessary to leak check the sampling train. An acceptable
vacuum gauge, when checked in a parallel leakless system with a
mercury U-tube manometer at 250-mm (10-in.) Hg vacuum, will agree
within ±25 mm (1.0 in.) Hg.
1.2 Sample Recovery Apparatus
1.2.1 Wash Bottles - Two 500-ml polyethylene or glass wash
bottles are needed for quantitative recovery of collected
samples.
1.2.2 Storage Bottles - One 100-ml polyethylene bottle is re-
quired to store each collected sample. An additional
polyethylene bottle is necessary to retain a blank for each
absorbing solution used in testing. Wash and storage bottles
should be visually checked for damage. In addition, check each
storage bottle seal to prevent sample leakage during transport.
1.3 Analysis Glassware
1.3.1 Pipettes - Several volumetric pipettes (Class A),
including 5-, 10-, 20-, and 25-ml sizes, are required for the
analysis.
1.3.2 Volumetric Flasks - Volumetric flasks (Class A) are re-
quired in 50-, 100-, and 1000-ml sizes.
1.3.3 Burettes - A 50-ml standard burette (Class A) is re-
quired for all titrations.
1.3.4 Erlenmeyer Flasks - One 250-ml Erlenmeyer flask is re-
quired for each sample, blank, standard, and control sample.
1.3.5 Dropping Bottle - One 125-ml glass dropping bottle is
needed to prepare the thorin indicator.
1.3.6 Graduated Cylinder - A 100-ml glass (Class A) graduated
cylinder is needed in the preparation of the thorin indicator and
the sample.
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 11 of 15
All glassware must be checked for cracks, breaks, and dis-
cernible manufacturing flaws.
1.4 Reagents
Unless otherwise indicated, it is intended that all reagents
conform to the specifications established by the Committee on
Analytical Reagents of the American Chemical Society (ACS), where
such specifications are available; otherwise the best available
grade is to be used.
1.4.1 Sampling -
Water - Use deionized distilled water to conform to ASTM
specification D1193-74, Type 3. At the option of the analyst,
the KMn04 test for oxidizable organic matter may be omitted when
high concentrations of organic matter are not expected to be
present.
Isopropanol, 80% - Mix 80 ml of reagent grade or certified
ACS isopropanol (100%) with 20 ml of deionized distilled water.
Check each lot of isopropanol for peroxide impurities as follows:
1. Shake 10 ml of isopropanol with 10 ml of freshly pre-
pared 10% potassium iodide (KI) solution.
2. Prepare a blank by similarly treating 10 ml of
deionized distilled water.
3. After 1 min, read the absorbance of the alcohol sample
against the H20 blank at 352 nm on a spectrophotometer. If
absorbance exceeds 0.1, reject the alcohol for use. Peroxides
may be removed from isopropanol by redistilling or by passing
through a column of activated alumina. After peroxides are re-
moved, check for peroxide impurities using the same method as
above. However, reagent grade isopropanol with suitably low
peroxide levels may be obtained from commercial sources. There-
fore, rejection of contaminated lots may be a more efficient
procedure.
Hydrogen Peroxide, 3% - Dilute 30% reagent grade or certi-
fied ACS hydrogen peroxide 1:9 (v/v) with deionized distilled
water. Prepare fresh daily. The 30% hydrogen peroxide should be
stored according to manufacturer's directions.
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 12 of 15
Potassium Iodide Solution, 10% - Dissolve 10.0 g of reagent
grade or certified ACS potassium iodide in deionized distilled
water and dilute to 100 ml. Prepare when needed. This solution
is used to check for peroxide impurities in the isopropanol only.
1.4.2 Sample Recovery -The following are required for sample
recovery:
Water - Use deionized distilled water, as in Subsec-
tion 1.4.1.
Isopropanol, 80% - Mix 80 ml of reagent grade or certified
ACS isopropanol with 20 ml of deionized distilled water.
1.4.3 Analysis -The following are required for sample analysis:
Water - Use deionized distilled water, as in Subsec-
tion 1.4.1.
Isopropanol, 100% - Use reagent grade or certified ACS
isopropanol.
Thorin Indicator - Use reagent grade or certified ACS
l-(o-arsonophenylazo)-2-naphthol-3, 6-disulfonic acid, disodium
salt. Dissolve 0.20 g in 100 ml of deionized distilled water.
Barium Perchlorate Solution, 0.0100N - Dissolve 1.95 g of
reagent grade or certified ACS barium perchlorate trihydrate
(Ba(ClO4)2 . 3H20) in 200 ml of distilled water and dilute to 1 £
with 100% isopropanol. Alternatively, use 1.22 g of (BaCl2 .
2H.?O) instead of the perchlorate. Standardize, as in
Section 3.5.5.
Sulfuric Acid Standard, 0.0100N - Either purchase the man-
ufacturer's certified or standardize the H2SC>4 at 0.0100N
±0.0002N against 0.0100N reagent grade or certified ACS NaOH that
has been standardized against primary standard grade potassium
acid phthalate.
1.5 Analytical Equipment
A spectrophotometer is needed to check the isopropanol for
peroxide impurities. The absorbance is read at 352 nm on the
spectrophotometer.
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 13 of 15
Table 1.1
ACTIVITY MATRIX FOR PROCUREMENT OF APPARATUS AND
SUPPLIES
Apparatus and
supplies
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sampling
Sampling probe
with heating
system
Capable of maintaining
100°C (212°F) exit air
at flow rate of
1.0 £/min
Visually check and
run heating system
checkout
Repair or
return to
supplier
Midget bubbler/
impinger
Standard stock glass
Visually check upon
receipt for breaks
or leaks
Return to manu-
facturer
Vacuum pump
Capable of maintaining
flow rate of 1 to 2
i/min; leak free
at 250 mm (10 in.) Hg
Check upon receipt
for leaks and capac-
ity
As above
Dry gas meter
Capable of measuring
total volume within +2%
at a flow rate of
1 £/min
Check for damage upon
receipt and calibrate
(Sec. 3.5.2) against
wet test meter
Reject if damaged,
behaves erratical-
ly, or cannot be
properly adjusted
Wet test meter
Capable of measuring
total volume within +1%
at a flow rate of
1 H/min
Upon assembly, leak
check all connections
and check calibration
by liquid displace-
ment
As above
Rotameter
Within +5% of manufac-
turer's calibration
curve (recommended)
Check upon receipt
for damage and cali-
brate (Sec. 3.5.2)
against wet test
meter
Recalibrate and
construct a new
calibration
curve
Drying tube
Minimum capacity of
30 to 50 g of silica
gel
Visually check upon
receipt for damage
and proper size
Return to
supplier
Thermometers
Within +1°C (2°F) of
true value in the
range of 0°C to 25°C
(32° to 77°F) for
impinger and +3°C
(5.4°F) for dry gas
meter thermometer
Check upon receipt
for damage (i.e.,
dents and bent stem) ,
and calibrate
(Sec. 3.5.2) against
mercury-in-glass
thermometer
Return to
supplier if
unable to
calibrate
(continued)
-------
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 14 of 15
Table 1.1 (continued)
Apparatus and
supplies
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sampling
(contM)
Barometer
Capable of measuring
atmospheric pressure
to within +2.5 mm
(0.1 in.) Hg calibrate
Check against mer-
cury-in-glass barome-
ter or equivalent
(Sec. 3.5.2)
Determine cor-
rection factor,
or reject if
difference is
more than ±2.5
Vacuum gauge
0 to 760 mm (0 to
29.92 in.) Hg range,
+2.5 mm (0.1 in.) Hg
accuracy at 250 mm
(10 in.) Hg
Check against U-tube
mercury manometer
upon receipt
Adjust or re-
turn to sup-
plier
Sample Recovery
Wash bottles
Polyethylene or glass,
500 ml
Visually check for
damage upon receipt
Replace or re-
turn to sup-
plier
Storage
bottles
Polyethylene, 100 ml
Visually check for
damage upon receipt ,
and be sure that caps
seal properly
As above
Analysis Glass-
ware
Pipettes, volu-
metric flasks,
burettes, and
graduated
cylinder
Glass, Class A
Upon receipt, check
for stock number,
cracks, breaks, and
manufacturer flaws
As above
Reagents
Distilled
water
Must conform to ASTM-
D1193-74, Type 3
Check each lot or
specify type when
ordering
As above
Isopropanol
100% isopropanol, re-
agent grade or certi-
fied ACS with no
peroxide impurities
Upon receipt, check
each lot for perox-
ide impurities with
a spectrophotometer
Redistill or
pass through
alumina column
or replace
(continued)
-------
Table 1.1 (continued)
Section No. 3.5.1
Revision No. 0
Date May 1, 1979
Page 15 of 15
Apparatus and
supplies
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Hydrogen
peroxide
30% HO, reagent grade
or certified ACS
Upon receipt, check
label for grade or
certification
Replace or re-
turn to manu-
facturer
Potassium
iodide solu-
tion
Potassium iodide, re-
agent grade or certified
ACS
As above
As above
Thorin indica-
tor
l-(o-arsonophenylazo)-
2-naphthol-3,6-disul-
fonic acid disodium
salt, reagent grade or
certified ACS
As above
As above
Barium per-
chlorate
solution
Barium perchlorate tri-
hydrate (Ba(C10.) .
3H_0), reagent grade
certified ACS
As above
As above
or
Sulfuric acid
solution
Sulfuric acid, 0.0100N
10.0002N
Have certified by
manufacturer or
standardize against
0.0100N NaOH that
has been standard-
ized against potas-
sium acid phthalate
(primary standard
grade)
As above
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 1 of 15
2.0 CALIBRATION OF APPARATUS
Calibration of the apparatus is one of the most important
functions in maintaining data quality. The detailed calibration
procedures included in this section were designed for the equip-
ment specified by Method 6 and described in the previous section.
If the tester opts to use Method 5 or Method 8 sampling appa-
ratus, then the calibration procedures governing that equipment
will apply and must be used. Table 2.1 at the end of this sec-
tion summarizes the quality assurance functions for calibration.
All calibrations should be recorded on standardized forms and
retained in a calibration log book.
2.1 Metering System
2.1.1 Wet Test Meter - The wet test meter must be calibrated and
have the proper capacity. For Method 6, the wet test meter
should have a capacity of at least 3 £/min. No upper limit is
placed on the capacity; however, a wet test meter dial should
make at least one complete revolution at the specified flow rate
for each of the three independent calibrations.
Wet test meters are calibrated by the manufacturer to an
accuracy of +0.5%. Calibration of the wet test meter must be
checked initially upon receipt and yearly thereafter.
The following liquid positive displacement technique can be
used to verify and adjust, if necessary, the accuracy of the wet
test meter to +1%:
1. Level the wet test meter by adjusting the legs until
the bubble on the level located on the top of the meter is cen-
tered.
2. Adjust the water volume in the meter so that the
pointer in the water level gauge just touches the meniscus.
3. Adjust the water manometer to zero by moving the scale
or by adding water to the manometer.
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 2 of 15
4. Set up the apparatus and calibration system as shown in
Figure 2.1.
a. Fill the rigid-wall 5-gal jug with distilled water
to below the air inlet tube. Put water in the
impinger or saturator and allow both to equili-
brate to room temperature (about 24 h) before use.
b. Start water siphoning through the system and
collect the water in a 1-gal container, located in
place of the volumetric flask.
5. Check operation of the meter as follows:
a. If the manometer reading is <10 mm (0.4 in.) H-O,
the meter is in proper working condition. Con-
tinue to step 6.
b. If the manometer reading is >10 mm (0.4 in.) EUO,
the wet test meter is defective or the saturator
has too much pressure drop. If the wet test meter
is defective, return to the manufacturer for
repair if the defect(s) (e.g., bad connections or
joints) cannot be found and corrected.
6. Continue the operation until the 1-gal container is
almost full. Plug the inlet to the saturator. If no leak
exists, the flow of liquid to the gallon container should stop.
If the flow continues, correct for leaks. Turn the siphon system
off by closing the valve, and unplug the inlet to the saturator.
7. Read the initial volume (V.) from the wet test meter
dial, and record on the wet test meter calibration log, Figure
2.2.
8. Place a clean, dry volumetric flask (Class A) under the
siphon tube, open the pinch clamp, and fill the volumetric flask
to the mark. The volumetric flask must be large enough to allow
at least one complete revolution of the wet test meter with not
more than two fillings of the volumetric flask.
9. Start the flow of water and record the maximum wet test
meter manometer reading during the test after a constant flow of
liquid is obtained.
10. Carefully fill the volumetric flask, and shut off the
liquid flow at the 2-8, mark. Record the final volume on the wet
test meter.
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 3 of 15
AIR INLET/
TUBE
IMPINGER
OR
SATURAIOR
AIR INLET
WATER OUT
LEVEL ADJUST
X) VALVE
2000-ML LINE
TYPE-A
.VOLUMETRIC
FLASK
Figure 2.1. Calibration check apparatus for
wet test meter.
-------
Wet test meter serial number V3 '
Date ; /'»-? /?•?
Range of wet test meter flow rate Q -
3.on A
Volume of test flask V =
s
Satisfactory leak check?
Ambient temperature of equilibrate liquid in wet test meter and reservoir 7^
Test
number
1
2
3
Manometer
reading,
mm HjO
5
S
?
Final
volume (V,.),
a
/. 99
2.00
S>.00
Initial
volume (V. ) ,
a 1
0
0
0
Total ,
volume (V ) ,
£
/.99
3L.00
£.00
Flask
volume (V ),
£ S
S.60
d.oo
Z.Oo
Percent
error,
°/
/o
6.S-
0
0
Must be less than 10 mm (0.4 in.) H20.
Calculations:
b
Vm = V, - V. .
mri
% error = 100 (Vm - V.J/V,, =
(±1%).
A
V
Signature of calibration person
Figure 2.2. Wet test meter calibration log.
^d O !5d en
CU P) CD CD
iQ ft < O
(D fD H- rt
01 H-
*» g H-0
»> O 3
I'M ^j
M 2 O
l-i- O •
ui
M U)
vo o •
-J Ul
vo •
to
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 5 of 15
11. Steps 7 through 10 must be performed three times.
Since the water temperature in the wet test meter and res-
ervoir has been equilibrated to the ambient temperature and
since the pressure in the wet test meter will equilibrate with
the water reservoir after the water flow is shut off, the air
volume can be compared directly with the liquid displacement
volume. Any temperature or pressure difference would be less
than measurement error and would not affect the final calcu-
lations .
The error should not exceed +1%; should this error magnitude
be exceeded, check all connections within the test apparatus for
leaks, and gravimetrically check the volume of the standard
flask. Repeat the calibration procedure, and if the tolerance
level is not met, adjust the liquid level within the meter (see
the manufacturer's manual) until the specifications are met.
2.1.2 Sample Meter System - The sample meter system—consisting
of the drying tube, needle valve, pump, rotameter, and dry gas
meter—is initially calibrated by stringent laboratory methods
before it is used in the field. The calibration is then re-
checked after each field test series. This recheck requires less
effort than the initial calibration. When a recheck indicates
that the calibration factor has changed, the tester must again
perform the complete laboratory procedure to obtain the new
calibration factor. After the meter is recalibrated, the metered
sample volume is multiplied by the calibration factor (initial or
recalibrated) that yields the lower gas volume for each test run.
Initial Calibration - The metering system should be cali-
brated when first purchased and at any time the posttest check
yields a calibration factor that does not agree within 5% of the
pretest calibration factor. A calibrated wet test meter (prop-
erly sized, with +1% accuracy) should be used to calibrate the
metering system.
The metering system should be calibrated in the following
manner before its initial use in the field.
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 6 of 15
1. Leak check the metering system (drying tube, needle
valve, pump, rotameter, and dry gas meter) as follows:
a. Temporarily attach a suitable rotameter (e.g.,
0-40 cm /min) to the outlet of the dry gas meter,
and place a vacuum gauge at the inlet to the
drying tube.
b. Plug the drying tube inlet. Pull a vacuum of at
least 250 mm (10 in.) Hg.
c. Note the flow rate as indicated by the rotameter.
d. A leak of <0.02 £/min must be recorded or leaks
must be eliminated.
e. Carefully release the vacuum gauge before turning
off pump.
2. Assemble the apparatus, as shown in Figure 2.3, with
the wet test meter replacing the drying tube and impingers; that
is, connect the outlet of the wet test meter to the inlet side
of the needle valve and the inlet side of the wet test meter to
a saturator which is open to the atmosphere. Note: Do not use
a drying tube.
3. Run the pump for 15 min with the flow rate set at
1 £/min to allow the pump to warm up and to permit the interior
surface of the wet test meter to become wet.
4. Collect the information required in the forms provided,
Figure 2.4A (English units) or 2.4B (metric units), using sample
volumes equivalent to at least five revolutions of the dry test
meter. Three independent runs must be made.
5. Calculate Y. for each of the three runs using Equation
2-1. Record the values in the form (Figure 2.4A or 2.4B).
. Vw [pm+ J376J (fcd + 460>
Vd Pm
Equation 2-1
-------
MANOMETER
AIR
INLET
SURGE TANK
WATER OUT
LEVEL ADJUST
IMPINGER
OR
SATURATOR
*fl D [3d C/3
P) p) fl) (D
up ft < O
(D (D H- ft
CO H-
-J g H- O
to O 3
Figure 2.3. Sample meter system calibration setup.
en > O
(-• U)
vo o •
-J un
vo
N)
-------
Date
Calibrated by "3. 3.
Meter box number
33 -I
Barometer pressure, P
m
Meter temperature correction factor
in. Hg Wet test meter number /Q f - /9
o,.
Wet test
meter
pressure
drop (Dm),a
in. H20
O.SL.T
o.a^r
o.a.f
Rota-
meter
setting
(Rs),
2
ft /min
o.oajr"
o.tfi^r
o.o'ir
Wet test
meter gas
volume
b
ft3
1.05*
1.0S°I
I.OC,!
Dry test meter
gas volume
ibl
-7t,a.09*
Final
T3fe. f»
7V- OS/
TUJfl
Wet test
meter
gas temp
-------
Date
/ 1 £s /
7g
Calibrated by &. J.
"7 *y*
Meter box number 3\f - /
Barometer pressure, P =
Meter temperature correction factor
mm Hg
Wet test meter number
/ p / -
Wet test
meter
pressure
drop (Dm),a
mm H-0
C. «/
&.V
6.*/
Rota-
meter
setting
(Rs),
Vrnin
?.o
/.0
1.0
Wet test
meter gas
volume
*^
Dry test meter
gas volume
(V ) b H
(.vd;, *
Initial
IdS. 43J
;*/. feM
Final
)\Z. 6/«
no.3>-n
Wet test
meter
gas temp
(tw>>
°C
as,
A9-
Inlet
gas temp
(td>),
°c
21
a-?
Dry test meter
Outlet
gas temp
(td),
°C
^•4
A1
Average
gas temp
(td),C
°C
a&.5"
St~) •>
Ai?- $
Time
of run
0),d
min
^O
^o
io
Average
ratio
(Y±),e
/ . 0 1 V*
/ 0/1
I-OI*
(Y ),f
/.oa
2 03-
/ 0%
D expressed as negative number.
m
Volume passing through meter. Dry gas volume is minimum for at least five revolutions of the meter.
p
The average of t, and t, if using two thermometers; the actual reading if using one thermometer.
The time it takes to complete the calibration run.
With Y defined as the average ratio of volumes for the wet test and the dry test meters, Y. = Y +0.02 Y
"""
for calibration and Y = Y +0.05 Y for the posttest checks, thus,
V (t + 273F)
Yi =
(D 713. 6)1
+ Y + Y
273°F)
(Eq.
Y .
> 2)
With Y defined as the average ratio of volumetric measurements by wet test meter to rotameter,
tolerance Y = 1 +0.05 for calibration and Y +0.1 for posttest checks.
V i
Y W
ri
J
0
+
(t
273°
+
w
F)
273
[Pm
°F)
+ (°m
Pm (°
/13. 6) 60j
.035)
(Eq. 3) and Y
(Eq. 4)
(D
vo
tn
O 5d co
P» (D (D
rt < O
(D H- rt
0) H-
S H- O
pj O £3
i 2
H 3 O
.^ o •
•
OJ
o .
tn
to
Figure 2.4B. Dry gas meter calibration data form (metric units).
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 10 of 15
where
Y. = ratio for each run of volumes measured by the wet
test meter and the dry gas meter, dimensionless
calibration factor,
3 3
V = volume measured by wet test meter, m (ft ),
w
P = barometric pressure at the meters, mm (in.) Hg,
Dm = pressure drop across the wet test meter, mm (in.) HUO,
t, = average temperature of dry gas meter, °C (°F),
3 3
V, = volume measured by the dry gas meter, m (ft ), and
t = temperature of wet test meter, °C (°F),
6. Adjust and recalibrate or reject the dry gas meter if
one or more values of Y. fall outside the interval Y +0.02Y,
where Y is the average for three runs. Otherwise, the Y (cali-
bration factor) is acceptable and will be used for future checks
and subsequent test runs. The completed form should be forwarded
to the supervisor for approval, and then filed in the calibration
log book.
An alternative method of calibrating the metering system
consists of substituting a dry gas meter, which has been properly
prepared as a calibration standard, in place of the wet test
meter. This procedure should be used only after obtaining ap-
proval of the administrator.
Posttest Calibration Check - After each field test series,
conduct a calibration check as in Subsection 2.1.2 with the
following exceptions:
1. The leak check is not conducted because a leak may have
been corrected that was present during testing.
2. Three or more revolutions of the dry gas meter may be
used.
3. Only two independent runs need be made.
4. If a temperature-compensating dry gas meter was used,
the calibration temperature for the dry gas meter must be within
±6°C (10.8°F) of the average meter temperature observed during
the field test series.
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 11 of 15
When a lower meter calibration factor is obtained as a
result of an uncorrected leak, the tester should correct the leak
and then determine the calibration factor for the leakless
system. If the new calibration factor changes the compliance
status of the facility in comparison to the lower factor, either
include this information in the report or consult with the admin-
istrator for reporting procedures. If the calibration factor
does not deviate by >5% from the initial calibration factor Y
(determined in Subsection 2.1.2), then the dry gas meter volumes
obtained during the test series are acceptable. If the calibra-
tion factor does deviate by >5%, recalibrate the metering system
as in Subsection 2.1.2, and for the calculations, use the cali-
bration factor (initial or recalibration) that yields the lower
gas volume for each test run.
2.2 Thermometers
The thermometers used to measure the temperature of gas
leaving the impinger train should be initially compared with a
mercury-in-glass thermometer that meets ASTM E-l No. 63C or 63F
specifications:
1. Place both the mercury-in-glass and the dial type or an
equivalent thermometer in an ice bath. Compare the readings
after the bath stabilizes.
2. Allow both thermometers to come to room temperature.
Compare readings after both stabilize.
3. The dial type or equivalent thermometer is acceptable
if values agree within ±1°C (2°F) at both points. If the
difference is greater than ±1°C (2°F), either adjust or recali-
brate the thermometer until the above criteria are met, or reject
it.
4. Prior to each field trip, compare the temperature
reading of the mercury-in-glass thermometer with that of the
meter thermometer at room temperature. If the values are not
within +2°C (4°F) of each other, replace or recalibrate the meter
thermometer.
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 12 of 15
The thermometer(s) on the dry gas meter inlet used to
measure the metered sample gas temperature should be initially
compared with a mercury-in-glass thermometer that meets ASTM E-l
No. 63C or 63F specifications:
1. Place the dial type or an equivalent thermometer and
the mercury-in-glass thermometer in a hot water bath, 40° to 50°C
(104° to 122°F). Compare the readings after the bath stabilizes.
2. Allow both thermometers to come to room temperature.
Compare readings after the thermometers stabilize.
3. The dial type or equivalent thermometer is acceptable
if values agree within 3°C (5.4°F) at both points (steps 1 and 2
above) or if the temperature differentials at both points are
within ±3°C (5.4°F) and the temperature differential is taped to
the thermometer and recorded on the meter calibration form
(Figure 2.4A or 2.4B).
4. Prior to each field trip, compare the temperature
reading of the mercury-in-glass thermometer at room temperature
with that of the thermometer that is part of the meter system.
If the values or the corrected values are not within ±6°C
(10.8°F) of each other, replace or recalibrate the meter ther-
mometer .
2.3 Rotameter
The Reference Method does not require that the tester cali-
brate the rotameter. The rotameter should be cleaned and main-
tained according to the manufacturer's instructions. For this
reason, it is recommended that the calibration curve and/or
rotameter markings be checked upon • receipt and then routinely
checked with the posttest meter system check. The rotameter may
be calibrated as follows:
1. Ensure that the rotameter has been cleaned as specified
by the manufacturer, and is not damaged.
2. Use the manufacturer's calibration curve and/or
markings on the rotameter for the initial calibration. Calibrate
the rotameter as described in the meter system calibration of
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 13 of 15
Subsection 2.1.2, and record the data on the calibration form
(Figure 2.4A or 2.4B).
3. Use the rotameter for testing if the pretest calculated
calibration is within 1.0 +0.05 £/min. If, however, the cali-
bration point is not within +5%, determine a new flow rate set-
ting, and recalibrate the system until the proper setting is
determined.
4. Check the rotameter calibration with each posttest
meter system check. If the rotameter check is within +10% of the
l-£/min setting, the rotameter can be acceptable with proper
maintenance. If, however, the check is not within +10% of the
flow setting, disassemble and clean the rotameter and perform a
full recalibration.
2.4 Barometer
The field barometer should be adjusted initially and before
each test series to agree within +2.5 mm (0.1 in.) Hg with a
mercury-in-glass barometer or with the pressure value reported
from a nearby National Weather Service Station and corrected for
elevation. The tester should be aware that the pressure readings
are normally corrected to sea level. The uncorrected readings
should be obtained. The correction for the elevation difference
between the weather station and the sampling point should be
applied at a rate of -2.5 mm Hg/30m (-0.1 in. Hg/100 ft)
elevation increase, or vice versa for elevation decrease.
The calibration checks should be recorded on the pretest
sampling form (Figure 2.5).
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 14 of 15
Date 9 //5 \1 ft Calibrated by
Meter box number r /K. ~ / AH@ /
Dry Gas Meter*
Pretest calibration factor = 0. ip (within ±2% of average
factor for each calibration run).
Impinger Thermometer
Was a pretest temperature correction used? yes _J/no
If yes, temperature correction (within ±1°C (2°F) of
reference values for calibration and within ±2°C (4°F) of
reference values for calibration check).
Dry Gas Meter Thermometer
Was a pretest temperature correction made? yes i/no
If yes, temperature correction (within ±3°C (5.4°F) of
reference values for calibration and within ±6°C (10.8°F) of
reference values for calibration check).
Barometer
Was the pretest field barometer reading correct? V yes no
(within ±2.5 mm (0.1 in) Hg of mercury-in-glass barometer)
Most significant items/parameters to be checked.
Figure 2.5. Pretest sampling checks
-------
Section No. 3.5.2
Revision No. 0
Date May 1, 1979
Page 15 of 15
Table 2.1. ACTIVITY MATRIX FOR CALIBRATION OF EQUIPMENT
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Wet test meter
Capacity of at least 2
JH/min and an accuracy
within +1.0%
Calibrate initially
and then yearly
by liquid displace-
ment
Adjust until
specifications
are met, or re-
turn to manu-
facturer
Dry gas meter
Y. = Y+0.02Y at a
flow rate of about
1 £/min
Calibrate vs. wet
test meter initially
and when the posttest
check is not within
Y+0.05
Repair and then
recalibrate, or
replace
Impinger ther-
mometer
Within ±1°C (2°F)
of true value
Calibrate each ini-
tially as a separate
component against a
mercury-in-glass
thermometer; after
train is assembled
before each field
test, compare with
mercury-in-glass
thermometer
Adjust, deter-
mine a constant
correction
factor, or
reject
Dry gas meter
thermometer
Within +3°C (5.4°F)
of true value
As above
As above
Rotameter
Clean and maintain ac-
cording to manufactur-
er's instructions
(required); calibrate
to +5% (recommended)
Initially and after
each field trip
Adjust and
recalibrate,
or reject
Barometer
Within +2.5 mm
(0.1 in.) Hg of mer-
cury-in-glass
barometer or of weather
station value
Calibrate initially
using a mercury-in-
glass barometer;
check before and
after each field test
Adjust to
agree with
certified
barometer
-------
Section No. 3.5.3
Revision No. 0
Date May 1, 1979
Page 1 of 6
3.0 PRESAMPLING OPERATIONS
The quality assurance activities for presampling preparation
are summarized in Table 3.1 at the end of this section. See
Section 3.0 of this Handbook for details on preliminary site
visits.
3.1 Apparatus Check and Calibration
Figure 3.1 or a similar form is recommended to aid the
tester in preparing an equipment checklist, status report form,
and packing list.
3.1.1 Sampling Train - The schematic of the S02 train is given
in Figure 1.1. Commercial models of this system are available.
Each individual or fabricated train must be in compliance with
the specifications in the Reference Method, Section 3.5.10.
3.1.2 Probe - The probe should be cleaned internally by
brushing first with tap water, then with deionized distilled
water, and finally with acetone. Allow probe to dry in the air.
In extreme cases, the glass or stainless steel liner can be
cleaned with stronger reagents; the objective is to leave the
liner free from contaminants. The probe's heating system should
be checked to see that it is operating properly. The probe must
be leak free when sealed at the inlet or tip and checked for
leaks at a vacuum of 250 mm (10 in. ) Hg with the meter box. Any
leaks should be corrected. The liner should be sealed inside the
metal sheath to prevent diluent air from entering the source
since most stacks are under negative pressure.
3.1.3 Midget Bubbler, Midget Impingers, and Glass Connectors -
All glassware should be cleaned with detergent and tap water,
and then with deionized distilled water. Any items that do not
pass a visual inspection for cracks or breakage must be repaired
or discarded.
-------
Section No. 3.5.3
Revision No. 0
Date May 1, 1979
Page 2 of 6
Apparatus check
Probe
Type liner
Glass v/
Stainless
steel
Other
Heated properly
Leak checked on
sampling train
Filter
Glass wool
Other
Glassware
Midget bubbler
Midget impinger
Size flddqtt
Type SfA?
Meter System
Leak- free pumps*
Rate meter*
Dry gas meter*
Reagents
Distilled water
H202, 30%
Isopropanol, 100%*
Silica gel
Other
Barometer
Drying tube
Acceptable
Yes
/
X
S
S
s
•X
iX
•X
s
•X"
wX
X
/
s
/
No
Quantity
required
3
^medl&ox
L
/&
Z.
Zy^
IJ&tVL
IK*-
5 w
I
10
Ready
Yes
^
X
^/
\s
s
\s
s
•X
*/
IX"
\/
No
Loaded
and packed
Yes
X
./
X
X
v/
J
s
s
/
/
S
No
* Most significant items/parameters to be checked.
Figure 3.1. Pretest preparations.
-------
Section No. 3.5.3
Revision No. 0
Date May 1, 1979
Page 3 of 6
3.1.4 Drying Tubes - Drying tubes should be packed with 6-to
16-mesh silica gel and sealed at both ends.
3.1.5 Valve and Rotameter - Prior to each field trip or at any
sign of erratic behavior, the flow control valve and rotameter
should be cleaned according to the maintenance procedure recom-
mended by the manufacturer.
3.1.6 Pump - The vacuum pump and oiler should be serviced as
recommended by the manufacturer, every 3 mo, or every 10th test
(whichever comes first), or upon erratic behavior (nonuniform or
insufficient pumping action).
3.1.7 Dry Gas Meter - A dry gas meter calibration check should
be made in accordance with the procedure in Section 3.5.2. An
acceptable posttest check from the previous test is sufficient.
3.1.8 Thermometers - The thermometers should be compared with
the mercury-in-glass thermometer at room temperature prior to
each field trip.
3.1.9 Barometer - The field barometer should be compared with
the mercury-in-glass barometer or with a National Weather Service
Station reading prior to each field trip.
3.2 Reagents and Equipment
3.2.1 Sampling - The midget bubbler solution is prepared by
mixing 80 ml of reagent grade or certified ACS isopropanol (100%)
with 20 ml of deionized distilled water. The midget impinger
absorbing reagent (3% hydrogen peroxide) is prepared by diluting
100 ml of 30% hydrogen peroxide to 1 £ with deionized distilled
water. All reagents must be prepared fresh for each test series,
using ACS reagent grade chemicals. Solutions containing isopro-
panol must be kept in sealed containers to prevent evaporation.
3.2.2 Sample Recovery - Deionized distilled water is required on
site for quantitative transfer of impinger solutions to storage
containers. This water and reagent grade isopropanol are used to
clean the midget bubbler after testing and prior to taking
another sample.
-------
Section No. 3.5.3
Revision No. 0
Date May 1, 1979
Page 4 of 6
3.3 Packaging Equipment for Shipment
Equipment should be packed in rigid containers to protect it
against rough handling during shipping and field operations (not
mandatory).
3.3.1 Probe - The inlet and outlet of the probe must be sealed
and protected from breakage. A suggested container is a wooden
case lined with polyethylene foam or other suitable packing
material; the case should have separate compartments for indi-
vidual devices. The case should be equipped with handles or eye
hooks that can withstand hoisting, and should be rigid to prevent
bending or twisting during shipping and handling.
3.3.2 Midget Bubblers, Impingers, Connectors, and Assorted
Glassware - All bubblers, impingers, and glassware should
be packed in a rigid container and protected by polyethylene foam
or other suitable packing material. Individual compartments for
glassware help to organize and protect each item. The impinger
train may be charged and assembled in the laboratory if sampling
is to be performed within 24 h.
3.3.3 Drying Tubes and Volumetric Glassware - A rigid container
lined with polyethylene foam material protects drying tubes and
assorted volumetric glassware.
3.3.4 Meter Box - The meter box—which contains the valve,
rotameter, vacuum pump, dry gas meter, and thermometers—should
be packed in a rigid shipping container unless its housing is
strong enough to protect components during travel. Additional
pump oil should be packed if oil is required for operation. It
is advisable to ship a spare meter box in case of equipment
failure.
3.3.5 Wash Bottles and Storage Containers - Storage containers
and miscellaneous glassware may be safely transported, if packed
in a rigid foam-lined container. Samples being transported in
the containers should be protected from extremely high ambient
temperatures (>50°C or about 120°F).
-------
Section No. 3.5.3
Revision No. 0
Date May 1, 1979
Page 5 of 6
Table 3.1 ACTIVITY MATRIX FOR PRESAMPLING OPERATIONS
Operation
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Apparatus
Probe
1. Probe liner free of
contaminants
2. Probe leak free
at 250 mm (10 in.) Hg
3. No moisture con-
densation
1. Clean probe in-
ternally by brushing
with tap water, then
deionized distilled
water, then acetone;
allow to dry in air
before test
2. Visual check be-
fore test
3. Check out heating
system initially and
when moisture appears
during testing
1. Retrace
cleaning pro-
cedure and
assembly
2. Replace
3. Repair or
replace
Midget bubbler,
midget impin-
ger, and
glass connec-
tors
Clean and free of
breaks, cracks, etc.
Clean with detergent,
tap water, and then
with deionized dis-
tilled water
Repair or
discard
Flow control
valve and
rotameter
Vacuum pump
Clean and without sign
of erratic behavior
(ball not moving freely.
Clean prior to each
field trip or upon
erratic behavior
Repair or
return to
manufacturer
Maintain sampling rate
of about 1 Vroin up to
250 mm (10 in.) Hg
Service every 3 mo or
upon erratic behav-
ior; check oiler
jars every 10th test
As above
Dry gas meter
Clean and within +2%
of calibration factor
Calibrate according
to Sec. 3.5.2; check
for excess oil if
oiler is used
As above
Reagents
Sampling
Requires all ACS grade
reagents
Prepare fresh daily
and store in sealed
containers
Prepare new
reagent
(continued)
-------
Section No. 3.5.3
Revision No. 0
Date May 1, 1979
Page 6 of 6
Table 3.1 (continued)
Operation
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sample recovery
Requires deionized dis-
tilled water on site
Use water and reagent
grade isopropanol to
clean midget bubbler
after test and before
sampling
Prepare new
reagent
Package Equip-
ment for Ship-
ment
Probe
Protect with poly-
ethylene foam
Prior to each ship-
ment
Repack
Midget bubbler,
impingers,
connectors,
and assorted
glassware
Pack in rigid con-
tainers with poly-
ethylene foam
As above
As above
Drying tubes,
volumetric
glassware
Sturdy container
lined with foam
As above
As above
Meter box
Meter box case and/or
container to protect
components; pack spare
meter box and oil
As above
As above
Wash bottles
and storage
containers
Pack in rigid foam-
lined container
As above
As above
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 1 of 12
4.0 ON-SITE MEASUREMENTS
On-site activities include transporting the equipment to the
test site, unpacking and assembling, sampling for sulfur dioxide,
and recording the data. The quality assurance activities are
summarized in Table 4.1 at the end of this section.
4.1 Transport of Equipment to the Sampling Site
The most efficient means of transporting the equipment from
ground level to the sampling site (often above ground level)
should be decided during the preliminary site visit or by prior
correspondence. Care should be taken to prevent damage to the
equipment or injury to test personnel during the moving. A
laboratory type area should be designated for preparation of the
absorbing reagents, for charging of the bubbler and impingers,
and for sample recovery.
4.2 Preliminary Measurements and Setup
The Reference Method outlines the procedure used to deter-
mine the concentration of sulfur dioxide in the gas stream. The
accuracy of the equipment that has been transported to the samp-
ling site and that may have been handled roughly can be deter-
mined by making a one-point check of the rotameter reading
against the dry gas meter reading at the test site. Use Equation
3 in Figure 2.4A or 2.4B and substitute dry gas meter readings in
place of wet test meter readings (i.e., V, = V ). Y . should be
Cl W -L, J_
between 0.9 and 1.1; if not, the meter box has lost its rate or
volume calibration. The tester can still use the meter box, but
the data should not be released for decision making until a post-
test recalibration has been made. If the dry gas meter calibra-
tion factor did change, the dry gas meter volumes may have to be
corrected. Record the test identification number on the sampling
data form, Figure 4.1.
4.3 Sampling
The on-site sampling includes the following steps:
-------
Plant name
//C/?7£ 'Poi^C/t
Sample location
Operator ."Jo £
/I/O • 3
///Q/77
Barometric pressure, mm
Probe material
Hg
Meter box number
city
Date
Sample number
Probe length m
Probe heater setting
Meter calibration factor (Y) /
X5"
Ambient temperature, °C (£&)
Initial leak check p. QQ V
Final leak check QQQ&
8
Sample point location /.3-S~/T) c*i A».
Sample purge time, min
Remarks T»La.v>. °X, D^u.
Sampling
time,
min
O
«T
/O
IS
ao
35"
Total
as-
Clock
time,
24 h
1100
1 lO-S"
II Id
m_r
n&r>
n 3>o
Sample
volume,
z (f*?l
izo. diO
;ar. -^0
JT.O-/0
j ^~ ao
JVC-iO
/v^-.ao
Total
A 500
Sample flow
rate setting,
£/min C&fe^/lKin)
;.o
1.0
/.o
1-0
1-0
Sample volume
mete red (AV ) ,
S- (&*)
5". /
^.2
r. i
s-.o
5-.0
AV
avl 5"-0
Percent
•a
deviation,
%
A
V
,2
0
0
Avg
dev /. 6
Dry gas
meter temp,
°c cs**}
—
ai
a.q
^o
•io
io
Avg
^9
Impinger
temp,
°C (^f
—
19
^A
»0
^0
AO
Max
temp SLO
Percent deviation =
AV - AV avg
m m 6
AV avg
100.
m
Figure 4.1. Field sampling data form for SO2
*T3 D Jd CO
0) p (D (D
^5 r+ < O
CD (D H- rt
CO H-
toS P- O
pj O 3
0^3
Hi 2|
H1^ O •
M U)
VD O •
vo
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 3 of 12
1. Preparation and/or addition of the absorbing reagents
to the midget bubbler and impingers.
2. Setup of the sampling train.
3. Connection to the electrical service.
4. Preparation of the probe (leak check of entire sampling
train and addition of particulate filter).
5. Insertion of the probe into the stack.
6. Sealing the port.
7. Checking the temperature of the probe.
8. Sampling.
9. Recording the data in Figure 4.1.
A final leak check of the train is always performed after samp-
ling.
4.3.1 Preparation and/or Addition of Absorbing Reagents
to Collection System - Absorbing reagents can be prepared
on site, if necessary, according to the directions in
Section 3.5.3.
1. Use a pipette or a graduated cylinder to introduce
15 ml of 80% isopropanol (IPA) into the midget bubbler or into a
graduated impinger bottle. Do not use the pipette or graduated
cylinder that was used to add the hydrogen peroxide solution.
Pipettes or graduated cylinders should be marked for use of H202
or IPA to minimize any possibility of introducing hydrogen perox-
ide into the isopropanol.
2. Add 15 ml of 3% hydrogen peroxide to each of the first
two midget impingers; leave the final midget impinger dry.
3. Pack glass wool into the top of the midget bubbler to
prevent sulfuric acid mist from entering the midget impingers and
causing a high bias for SO-.
4.3.2 Assembling the Sampling Train - After assembling the
sampling train as shown in Figure 1.1, perform the following:
1. Adjust probe heater to operating temperature. Place
crushed ice and water around the impingers.
2. Leak check the sampling train just prior to use at the
sampling site (not mandatory) by temporarily attaching a
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 4 of 12
3
rotameter (capacity of 0 to 40 cm /min) to the outlet of the dry
gas meter and placing a vacuum gauge at or near the probe inlet.
Plug the probe inlet, pull a vacuum of at least 250 mm (10 in.)
Hg, and note the flow rate indicated by the rotameter. A leakage
rate not <2% of the average sampling rate is acceptable. Note;
Carefully release the probe inlet plug before turning off the
pump. It is suggested (but not mandatory) that the pump be leak
checked separately, either prior to or after the sampling run.
If prior to the run, the pump leak check shall precede the leak
check of the sampling train. If after, the pump leak check shall
follow the train leak check. To leak check the pump, proceed as
follows: Disconnect the drying tube from the probe impinger
assembly. Place a vacuum gauge at the inlet to either the drying
tube or the pump. Pull a vacuum of 250 mm (10 in.) Hg. Plug or
pinch off the outlet of the flow meter and then turn off the
pump. The vacuum should remain stable for at least 30 s.
3. Place a loosely packed filter of glass wool in the end
of the probe, and connect the probe to the bubbler.
4.3.3 Sampling (Constant Rate) - Sampling is performed at a
constant rate of approximately 1.0 £/min as indicated by the
rotameter during the entire sampling run. The procedure is as
follows:
1. Record the initial dry gas meter readings, barometer
reading, and other data as indicated in Figure 4.1. Double check
the dry gas meter reading and be sure that no hydrogen peroxide
has been allowed to back up and wet the glass wool.
2. Position the tip of the probe at the sampling point,
connect the probe to the bubbler, and start the pump. Warning:
If the stack is under a negative pressure of >50 mm (2 in.) H^O
while disconnected from the impinger, the probe should be posi-
tioned at the sampling point, the sample pump turned on, and then
the probe immediately connected to the impinger to prevent the
impinger solutions from being siphoned backwards and contaminat-
ing the isopropanol.
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 5 of 12
3. Adjust the sample flow to a constant rate of approxi-
mately 1.0 £/min as indicated by the rotameter.
4. Maintain this constant rate within 10% during the
entire sampling run, and take readings (dry gas meter, tempera-
tures at dry gas meter and at impinger outlet, and rate meter) at
least every 5 min. Add more ice during the run to keep the
temperature of the gases leaving the last impinger at 20°C (68°F)
or less. Salt may be added to the ice bath to further reduce the
temperature.
5. Refer to emission standards for minimum sampling time
and/or volume. (For example, the Federal standard for fossil
fuel-fired steam generators specifies a minimum sampling time of
20 min and a minimum sampling volume of 20 £ corrected to stand-
ard conditions.) The total sample volume at meter conditions
should be approximately 28 8, (1 ft ). Make a quick calculation
near the end of the run to guarantee that sufficient sample
volume has been drawn; if the volume is insufficient, sample for
an additional 5 min.
6. Turn off the pump at the conclusion of each run, remove
probe from the stack, and record the final readings. Warning:
Again, if the stack is under a negative pressure, disconnect the
probe first, and turn off the pump immediately thereafter.
7. Conduct a leak check, as described in Subsection 4.3.2
(mandatory).
8. If the train passes the leak check, drain the ice bath
and purge the remainder of the train by drawing clean ambient air
through the system for 15 min at the sampling rate. To provide
clean ambient air, pass air through a charcoal filter or through
an extra midget impinger with 15 ml of 3% ^2O2' The tester may
opt to use ambient air without purification.
9. Calculate the sampling rate during the purging of the
sample. The sample volume (AV ) for each point should be within
+10% of the average sample volume for all points. If the average
of all points is within the specified limit, the sample rate is
acceptable. Noncompliance with the +10% of constant rate for a
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 6 of 12
single sample should not have a significant effect on the final
results of the test for noncyclic processes.
10. Change the particulate filter (glass-wool plug) at the
end of each test since particulate buildup on the probe filter
may result in a loss of SO_ due to reactions with \particulate
£ "•*
matter.
4.4 Sample Recovery
The Reference Method requires transfer of the impinger
contents and the connector washings to a polyethylene storage
container. This transfer should be done in the "laboratory" area
to prevent contamination of the test sample.
After completion of the purge, disconnect the impingers and
transport them to the cleanup area. The contents of the midget
bubbler (contains isopropanol) may be discarded. However, it is
usually advisable to retain this fraction until analysis is
performed on the H?02. Analysis of the isopropanol may be useful
in detecting cleanup or sampling errors. Cap off the midget
impinger section with the use of polyethylene or equivalent caps
before transport to the cleanup area. Transfer the contents of
the midget impingers into a labeled, leak-free polyethylene
sample bottle. Rinse the three midget impingers a couple of
times and the connecting tubes with 3 to 15 ml portions of dis-
tilled water. Add these washings to the same sample bottle, and
mark the fluid level on the side. The total rinse and sample
volume should be <100 ml; a 100-ml mark can be placed on the
outside of the polyethylene containers as a guide. Place about
100 ml of the absorbing reagent (3% H2O2) in a polyethylene
bottle and label it for use as a blank during sample analysis.
An example of a sample label is shown in Figure 4.2.
4.5 Sample Logistics (Data) and Packing Equipment
The sampling and sample recovery procedures are followed
until the required number of runs are completed. Log all data on
the Sample Recovery and Integrity Data Form, Figure 4.3. If the
bubbler, impingers, and connectors are to be used in the next
test, they should be rinsed with distilled water, and the bubbler
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 7 of 12
^™7^\ ^^"\^
Plant HCP1C TOUKfiiQtt-'t City /#tyfc//£*«y ^/^
Site £fo;/ft* My. 3 Sample type ^O^
Date 8/^0/77 Run number ,£#- /
Front rinse CH Front filter d Front solution CD
Back rinse CD Back filter d Back solution Or
Solution £/2,02. Level marked \^T J2
Volume: Initial ^Ot* L Final < /£O /kL. iS
Cleanup by (jl && iS
Figure 4.2. Example of a sample label.
-------
Plant
rl&n~t
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 8 of 12
fj . i A I ~f
Sample location £fc/'^" f'f ' $
Field Data Checks
Sample recovery personnel
Person with direct responsibility for recovered samples
Sample
number
1
2
3
4
5
6
Blank
Sample
identification
number
-«?-/
Date
of
recovery
&//0/77
Liquid
level
marked
Yes
Stored
in locked
container
Xrs
Remarks
loo
Signature of field sample trustee
>>»MY
Laboratory Data Checks
Lab person with direct responsibility for recovered samples^).
Date recovered samples received § /Ji
Analyst
Sample
number
1
2
3
4
5
6
Blank
Sample
identification
number
JZO-I
Date
of
analysis
8//Z/77
Liquid
at marked
level
y~
Sample
identified
Vet
Remarks
Signature of lab sample trustee JUt>Ov
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 9 of 12
should be rerinsed with isopropanol. A new drying tube should be
inserted into the sampling train. At the completion of the test:
1. Check all sample containers for proper labeling (time,
date, location, number of test, and any pertinent documentation).
Be sure that a blank has been taken.
2. Record all data collected during the field test in
duplicate by using carbon paper or by using data forms and a
field laboratory notebook. One set of data should be mailed to
the base laboratory, given to another team member or to the
Agency. Hand carrying the other set (not mandatory) can prevent
a very costly and embarrassing mistake.
3. Examine all sample containers and sampling equipment
for damage, and pack them for shipment to the base laboratory,
being carejful to label all shipping containers to prevent loss of
samples or equipment.
4. Make a quick check of the sampling and sample recovery
procedures using the data form, Figure 4.4.
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 10 of 12
Sampling
Bubbler and impinger contents properly selected, measured,
and placed in impinger?* ^/
Impinger Contents/Parameters*
1st: 15 ml of 80% isopropanol y
2nd: 15 ml of 3% H202
3rd: 15 ml of 3% H202 jX.
Final impinger dry? \/_
Probe heat at proper level? X
Crushed ice around impingers? y/
Pretest leak check at 250 mm (10 in.) Hg? .X
Leakage rate? 0.004
Probe placed at proper sampling point?
Flow rate constant at approximately 1.0 £/min?*
Posttest leak check at 250 mm (10 in.) Hg?*
Leakage rate? Q. 0&L, JLj(
Sample Recovery
System purged at least. 15 min at test sampling rate?*
Contents of impingers placed in polyethylene bottles?
Fluid level marked?* iX
Sample containers sealed and identified?*
Most significant items/parameters to be checked.
Figure 4.4 On-site measurements.
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 11 of 12
Table 4.1 ACTIVITY MATRIX FOR ON-SITE MEASUREMENT CHECKS
Activity
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Preparation
and/or addi-
tion of ab-
sorbing re-
agents
Add 15 ml of 80% iso-
propanol to midget
bubbler and 15 ml of
3% H20 to first two
midget impingers
Prepare 3% H^O fresh
daily; use pipette
or graduated cylinder
to add solutions
Reassemble col-
lection system
Assembling the
sampling
train
1. Assemble to speci-
fications in Fig. 1.1
2. A leakage rate <2%
of the average sampling
rate
1. Before each sam-
pling
2. Leak check before
sampling (recommended)
by attaching a rotame-
ter to dry gas meter
outlet, placing a
vacuum gauge at or
near probe inlet, and
pulling a vacuum of
>250 mm (10 in.) Hg
Sampling (con-
stant rate)
1. Within ±10% of a
constant rate
2. Minimum acceptable
time is 20 min and vol-
ume is 20 S, corrected
to STP or as specified
by regulation
3. Less than 2% leakage
rate at 250 mm (10 in.)
Hg
4. Purge remaining S0r
from isopropanol
1. Calculate % devi-
ation for each sample
using equation in
Fig. 4.1
2. Make a quick cal-
culation prior to
completion and an ex-
act calculation after
completion
3. Leak check after
sample run (manda-
tory) ; use same pro-
cedure as above
4. Drain ice and
purge 15 min with
clean air at the
sample rate
1. Reassemble
2. Correct the
leak
1. Repeat the
sampling , or
obtain accept-
ance from a
representative
of the
Administrator
2. As above
3. As above
4. As above
(continued)
-------
Section No. 3.5.4
Revision No. 0
Date May 1, 1979
Page 12 of 12
Table 4.1 (continued)
Activity
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sample logis-
tics (data)
and packing
of equipment
1. All data are re-
corded correctly
2. All equipment ex-
amined for damage and
labeled for shipment
3. All sample contain-
ers properly labeled
and packaged
1. Visually check
upon completion of
each run and before
packing
2. As above
3. Visually check
upon completion of
test
1. Complete
the data
form
2. Redo test
if damage
occurred during
testing
3. Correct when
possible
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 1 of 16
5.0 POSTSAMPLING OPERATIONS
Table 5.1 at the end of this section summarizes the quality
assurance activities for postsampling operations.
5.1 Apparatus Check
A posttest check—including a calibration check, the
cleaning, and/or the performance of routine maintenance—should
be made on most of the sampling apparatus. Cleaning and mainte-
nance of the sampling apparatus are discussed in Section 3.5.7.
Figure 5.1 should be used to record the posttest checks.
5.1.1 Metering System - The metering system has three components
that must be checked: dry gas meter thermometer(s), dry gas
meter, and rotameter.
The dry gas meter thermometer should be checked by compari-
son with the ASTM mercury-in-glass thermometer at room tempera-
ture. If the readings agree within 6°C (10.8°F), they are accept-
able. When the readings are outside this limit, the thermometer
must be recalibrated according to Section 2.5.2 after the post-
test check of the dry gas meter. For calculations, the dry gas
meter thermometer reading (field or recalibration) that would
give the higher temperature is used. That is, if the field read-
ing is higher, no correction of the data is necessary; if the
recalibration value is higher, the difference in the two readings
is added to the average dry gas meter temperature reading.
The posttest checks of the dry gas meter and rotameter are
similar to the initial calibration, as described in
Section 3.5.2, but they include the following exceptions:
1. The metering system should not have had any leaks
corrected prior to the posttest check.
2. Three or more revolutions of the dry gas meter are
sufficient.
3. Only two independent runs need be made. If the post-
test dry gas meter calibration factor (Y) does not deviate by >5%
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 2 of 16
Meter Box Number ^S "I
Dry Gas Meter*
Pretest calibration factor Y = /. 61
Posttest check Y, = / Qlj Y = /
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 3 of 16
from the initial calibration factor, the dry gas meter volumes
obtained during the test series are acceptable. If it deviates
by >5% recalibrate the metering system as in Section 3.5.2, using
the calibration factor (initial or recalibration) that yields the
lower gas volume for each test run. The lesser calibration
factor will give the lower gas volume.
The rotameter calibration factor (Y ) can also be determined
during the calibration of the dry gas meter. If Y does not
deviate by >10% from the initial calibration factor, the rotame-
ter operation is acceptable. If Y changes by >10%, the rotameter
should be cleaned and recalibrated. No corrections need be made
for any calculations.
5.1.2 Barometer - The field barometer readings are acceptable if
they agree within +5 mm (0.2 in.) Hg when compared with those of
the mercury-in-glass barometer. When the comparison is not
within this range, the lesser calibration value should be used
for the calculations. If the field barometer reads lower than
the mercury-in-glass barometer, the field data are acceptable;
but if the mercury-in-glass barometer gives the lower reading,
the barometric value adjusted for the difference in the two
readings should be used in the calculation.
5.2 Analysis (Base Laboratory)
Calibrations and standardizations are of the utmost import-
ance to a precise and accurate analysis. The analysis is based
on the insolubility of barium sulfate (BaSO4) and on the forma-
tion of a colored complex between excess barium ions and the
thorin indicator, l-(o-arsonophenylazo)-2-naphthol-3,6-disulfonic
acid, disodium salt. Aliquots from the impinger solution are
analyzed by titration with barium perchlorate to the pink end-
point. The barium ions react preferentially with sulfate ions in
solution to form a highly insoluble barium sulfate precipitate.
When the barium has reacted with all of the sulfate ions, the
excess barium then reacts with the thorin indicator to form a
metallic salt of the indicator and to give a color change as
shown in Equation 5-1.
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 4 of 16
Ba++ + S04 + thorin(x++) -> BaS04 + thorin(Ba++)
(yellow) (pink) Equation 5-1
Upon completion of each step of the standardization or of
each sample analysis, the data should be entered on the proper
data form. At the conclusion of the sample analysis, the data
form should be reviewed and signed by the laboratory person
with direct responsibility for the sample.
5.2.1 Reagents (Standardization and Analysis) - The following
reagents are required for the analysis of the samples:
1. Water. Deionized distilled water that conforms to ASTM
specification D1193-74, Type 3. At the option of the analyst,
the KMn04 test for oxidizable organic matter may be omitted when
high concentrations of organic matter are not expected. Note:
The water must meet the ASTM specifications since sulfate ions
and many other anions present in distilled water are not identi-
fied in the normal standardization of the acid by NaOH titration,
which measures the hydrogen ion concentration rather than the
sulfate ion concentration. This added sulfate concentration will
result in an erroneous standardization of the barium perchlorate
titration, which directly measures sulfate ion concentration and
not hydrogen ion concentration. A check on the acceptability of
the water is detailed in Subsection 5.2.4.
2. Isopropanol. 100%, ACS reagent grade. Check for per-
oxide impurities as described in Section 3.5.1.
3. Thorin indicator. Dissolve 0.20 +0.002 g of l-(o-ar-
sonophenylazo)-2-naphthol-3,6-disulfonic acid, disodium salt, or
the equivalent, in 100 ml of deionized distilled water. Measure
the distilled water in the 100-ml graduated cylinder (Class A).
4. Sulfuric acid standard, 0.0100N Either purchase
manufacturer-guaranteed or standardize the H2S04 to ±°-°02N
against 0.0100N NaOH that has been standardized against potassium
acid phthalate (primary standard grade) as described in Subsec-
tion 5.2.3. The 0.01N H2SC*4 may be prepared in the following
manner:
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 5 of 16
a. Prepare 0.5N H-SO. by adding approximately 1500 ml
of distilled ^ater to a 2-£ volumetric flask.
b. Cautiously add 28 ml of concentrated sulfuric acid
and mix.
c. Cool if necessary.
d. Dilute to 2 & with distilled water.
e. Prepare 0.01N H^SO. by first adding approximately
800 ml of distilled water to a l-£ volumetric
flask and then adding 20.0 ml of the 0.5N H2SO4.
f. Dilute to 1 S, with distilled water and mix thor-
oughly .
5. Barium perchlorate solution 0.0100N. Dissolve 1.95 g
of barium perchlorate trihydrate (Ba(C104)2 . 3H2
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 6 of 16
3. Weigh to the nearest 0.1 mg, three 40-mg portions of
the phthalate. Dissolve each portion in 100 ml of freshly boiled
deionized distilled water in a 250-ml Erlenmeyer flask.
4. Add two drops of phenolphthalein indicator, and titrate
the phthalate solutions with the NaOH solution. Observe titra-
tions against a white background to facilitate detection of the
pink endpoint. The endpoint is the first faint pink color that
persists for at least 30 s.
5. Compare the endpoint colors of the other two titrations
against the first. The normality is the average of the three
values calculated using the following equation.
N _ mg KHP
NaOH ml titrant x 204.23
where
NNaOH = calculated normality of sodium hydroxide,
mg KHP = weight of the phthalate, mg, and
ml titrant = volume of sodium hydroxide titrant, ml.
The chemical reaction for this standardization is shown in Equa-
tion 5-3. The sodium hydroxide is added to the potassium hydro-
gen phthalate and colorless phenolpthalein solution until there
is an excess of diluted hydroxyl ions which causes the phenolph-
thalein solution to change to a pink color.
NaOH + KHP + phenolphthalein -» KNaP + HOH + phenolphthalein.
(colorless) (pink) Eguation 5-3
5.2.3 Standardization of Sulfuric Acid - To standardize sulfuric
acid, proceed as follows:
1. Pipette 25 ml of the H2S04 into each of three 250-ml
Erlenmeyer flasks.
2. Add 25 ml of deionized distilled water to each.
3. Add two drops of phenolphthalein indicator, and titrate
with the standardized NaOH solution to a persistent pink end-
point, using a white background.
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 7 of 16
4. Titrate a blank of 25 ml of deionized distilled water,
using the same technique as step 3. The normality will be the
average of the three independent values calculated using the
following equation:
(ml NaOH . , - ml NaOH,, . ) x
NH „ = ^±d == ^^ Equation 5-4
O A
where
HpSO4 = calculated normality of sulfuric acid,
ml NaOH . , = volume of titrant used for H0SO,., ml,
acid £ **
ml NaOH,, , = volume of titrant used for blank, ml, and
blank
NXT r>cr = normality of sodium hydroxide.
.NclUri
5.2.4 Standardization of Barium Perchlorate (0.0100N) - To
standardize barium perchlorate, proceed as follows:
1. Pipette 25 ml of sulfuric acid standard (0.0100N) into
each of three 250-ml Erlenmeyer flasks.
2. Add 100 ml of reagent grade isopropanol and two to four
drops of thorin indicator, and titrate to a pink endpoint using
0.0100N barium perchlorate. Perform all thorin titrations
against a white background to facilitate the detection of the
pink endpoint color.
3. Prepare a blank by adding 100 ml of isopropanol to
25 ml of deionized distilled water. If a blank requires >0.5 ml
of titrant, the analyst should determine the source of contamina-
tion. If the distilled water contains high concentrations of
sulfate or other polyvalent anions, then all reagents made with
the distilled water will have to be remade using distilled water
that is acceptable.
4. Use the endpoint of the blank or the endpoint of the
first titration as a visual comparator for the succeeding titra-
tions .
5. Record data on analytical data form, Figure 5.2. The
normality of the barium perchlorate will be the average of the
three independent values calculated using Equation 5-5.
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 8 of 16
Plant
Sample location
A3P .
Volume and normality of barium
perchlorate
Date
Analyst fo
1 A«y. C3t ml 0.
N
2 aq.50 ml Q.o/oaQN
3 a«J.5O ml Q.
avg
Sample
number
1
2
3
4
5
6
Blank
Sample
identification
number
50- 1
Total
sample
volume
^soln''
ml
(00
N/A
Sample
aliquot
volume
ml
do
Volume of titrant (V ) , ml
1st
titration
n. ai
0
2nd
titration
n. »*
o
Average
H-30
Vtb=0
Volume for the blank must be the same as that of the sample aliquot.
1st titration _ or11st titration - 2nd titrationl <0.2 ml.
2nd titration | |-
Signature of analyst
Signature of reviewer or supervisor
/^-o— ^g-c-XU
Figure 5.2 Sulfur dioxide analytical data form.
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 9 of 16
NH2S04 X 25
NBa(C104)2 = ml Ba(C104)2 Equation 5-5
where
N
Ba(C104)2 = calculated normality of barium perchlorate,
H2S04 = normalitv of standardized sulfuric acid, and
ml Ba(C104)2 = volume of barium perchlorate titrant, ml.
The chemical reaction for this standardization was shown in
Equation 5-1. The standardized barium perchlorate should be
protected from evaporation of the isopropanol at all times.
Note: It is suggested that the analyst unfamiliar with this
titration carry out titrations on aliquots at low, medium, and
high concentrations in the following manner:
1. Pipette 2.0-, 10.0-, and 20.0-ml aliquots of 0.0100N
H2S04 into three 250-ml Erlenmeyer flasks.
2. Dilute to 25 ml with distilled water.
3. Add a 100-ml volume of 100% isopropanol and two to four
drops of thorin indicator to each.
4. Titrate with barium perchlorate to become familiar with
the endpoint.
5.2.5 Control Samples - The accuracy and precision of the sample
analysis should be checked. The accuracy of the analytical tech-
nique is determined by control samples. The precision is checked
by duplicate analyses of both the control and the field samples.
Acceptable accuracy and precision should be demonstrated on the
analysis of the control sample prior to the analysis of the
field samples.
The control sample should be prepared and analyzed in the
following manner:
1. Dry the primary standard grade ammonium sulfate
((NH4)2S04) for 1 to 2 h at 110°C (230°F), and cool in a desic-
cator.
2. Weigh to the nearest 0.5 mg, 1.3214 g of primary stand-
ard grade ammonium sulfate.
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 10 of 16
3. Dissolve the reagent in about 1800 ml of distilled
water in a 2-£ volumetric flask.
4. Dilute to the 2-H mark with distilled water. The
resulting solution is 0.0100N ammonium sulfate.
5. Enter all data on the form shown in Figure 5.3.
6. Pipette 25 ml of the control sample into each of three
250-ml Erlenmeyer flasks, and pipette a 25-ml blank of distilled
water into a fourth 250-ml Erlenmeyer flask. Note: Each control
sample will contain 16.5 mg of ammonium sulfate.
7. Add 100 ml of reagent grade isopropanol to each flask
and then two to four drops of thorin indicator.
8. Initially, titrate the blank to a faint pink endpoint
using the standardized barium perchlorate. The blank must con-
tain <0.5 ml of titrant, or the distilled water is unacceptable
for use in this method.
9. Titrate two of the control samples with the standard-
ized barium perchlorate to a faint pink endpoint using the blank
endpoint as a guide. The endpoint is the first faint pink end-
point that persists for at least 30 s. All titrations should be
done against a white background.
10. If the titrant volumes from the first two control
samples agree within 0.2 ml, the average of the two values can be
used to complete the calculations shown in Figure 5.3. If not
within 0.2 ml, titrate the third control sample. If the titra-
tion volume agrees within 0.2 ml of either of the first two
samples, use the two titrant volumes that are consistent for the
remaining calculations. If this criterion cannot be met with the
first set of two control samples, follow the same procedure on
a second set of two control samples.
11. If the criterion cannot be met for the second set of
control samples, the analyst should have the analytical tech-
nigues observed by a person knowledgeable in chemical analysis,
or should have all reagents checked.
12. After consistent titrant volumes are obtained, calcu-
late the analytical accuracy as shown in Figure 5.3. If the
measured value is within 5% of the stated value, the technique
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 11 of 16
Plant SulluV.c flc'J
Analyst ft. )
Date analyzed
N.
Ba(Cl04)2
Weight of ammonium sulfate is 1.3214 g?
Dissolved in 2 8, of distilled water?
0.0 10
P <.
Titration of blank Q.Q ml Ba(ClOA)0 (must be < 0.5-ml)
Control
sample
number
J
Time of
analysis,
24 h
0^30
•* *.
Titrant volume ,a ml
1st
*5. 0
2nd
35-0
3rd
Avg
9$. 0
Two titrant volumes must agree within 0.2 ml.
ml Ba(C104)2 x N , } = 25 ml x 0.01N
4 '2 (control sample) (control sample)
ml x Q.
N =
(must agree within +5%, i.e., 0.238 to 0.262)
Does value agree? tXyes _ no
Signature of analyst
Signature of reviewer
Figure 5.3. Control sample analytical data form
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 12 of 16
and standard reactions are acceptable, and the field samples may
be analyzed. When the 5% accuracy cannot be met, the barium
perchlorate must be restandardized or the control sample must be
checked until the accuracy criterion of the control sample
analysis can be obtained. The accuracy limit of ±5% for intra-
laboratory control samples is recommended based on the control
limit of ±7% for interlaboratory audit results discussed in
Section 3.6.8.
13. The recommended frequency for analysis of control
samples is the following:
a. Analyze two control samples each analysis day
immediately prior to analysis of the actual collected source
samples.
b. Analyze two control samples after the last collected
source sample is analyzed each analysis day.
14. Enter results from the control sample analyses on
Figure 5.3 and submit Figure 5.3 with the source test report
as documentation of the quality of the source test analysis.
5.2.6 S amp 1 e An a 1 y s is - Check the level of liquid in the con-
tainer to determine whether any sample was lost during shipment,
and note this on the data form, Figure 4.3. Figure 5.4 can be
used to check analytical procedures. If a noticeable amount of
leakage has occurred, follow the alternative method described
below. Approval should have been requested prior to testing in
case of subsequent leakage. The alternative method is as fol-
lows :
1. Mark the new level of the sample.
2. Transfer the sample to a 100-ml volumetric flask, and
dilute to exactly 100 ml with deionized distilled water.
3. Put water in the sample storage container to the ini-
tial sample mark, and measure the initial sample volume (vsojn )•
4. Put water in the sample storage container to the mark
of the transferred sample, and measure the final volume (vsoin )•
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 13 of 16
Reagents
Normality of sulfuric acid standard* U. Of 01 /V _
Date purchased /£>/36>/7£ Date standardized ////(,/'? 8
Normality of barium perchlorate titrant* 0. Oft 9 L
Date standardized ////k JlB
Normality of control sample* _ Q. O I OO A/
Date prepared /l/(*/7 8
Volume of burette 3D r~nt Graduations O. /
Sample Preparation
Has liquid level noticeably changed?*
Original volume Corrected volume
Samples diluted to 100 ml?* ^
Analysis
Volume of aliquot analyzed* X£/
Do replicate titrant volumes agree within 1% or 0.2 ml?
Number and normality of control samples analyzed 2.Q Q,t
Are replicate control samples within 0.2 ml?
Is accuracy of control sample analysis ±5%?*
All data recorded? I/ Reviewed by
Most significant items/parameters to be checked.
Figure 5.4. Posttest operations.
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 14 of 16
5. If vso-in is
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 15 of 16
5. Record all data on the data form, Figure 5.2. Average
the consistent titrant volumes, and use them as V. in subsequent
calculations. All analytical data must then be reviewed by a
person familiar with procedures, and this review should be noted
on the data form, Figure 5.2. Note; Protect the 0.0100N barium
perchlorate solution from evaporation at all times.
-------
Section No. 3.5.5
Revision No. 0
Date May 1, 1979
Page 16 of 16
Table 5.1. ACTIVITY MATRIX FOR POSTSAMPLING OPERATIONS
Activity
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sampling
Apparatus
Dry gas meter
Within ±5% of pretest
calibration factor
Make two independent
runs after each field
test
Recalibrate
and use cali-
bration factor
that gives
lower sample
volume
Rate meter
Within +10% of desired
flow rate (recommended)
Make two independent
runs during the check
of the rate meter
Recalibrate
Meter thermome-
ter
Within +6°C (10.8°F) at
ambient temperature
Compare with ASTM
mercury-in-glass
thermometer after
each field test
Recalibrate
and use
higher temper-
ture value for
calculations
Barometer
Within +5.0 mm (0.2 in.)
Hg at ambient pressure
Compare with mercury-
in-glass barometer
after each field test
Recalibrate
and use lower
barometric
value for
calculations
Analysis
Reagents
Prepare according to
requirements detailed
in Subsec. 5.2
Prepare and/or stand-
ardize within 24 h
of sample analysis
Prepare new
solutions
and/or re-
standardize
Control Sample
Titrants differ by <0.2
ml; analytical results
within +5% of stated
value
Before and after
analysis of field
samples
Prepare new
solutions and/
or restan-
dardize
Sample analysis
Titrant volumes differ
by <1% or <0.2 ml,
whichever is greater
Titrate until two or
more sample aliquots
agree within 1% or
0.2 ml, whichever is
greater; review all
analytical data
Void sample
if any two
titrations do
not meet
criterion
-------
Section No. 3.5.6
Revision No. 0
Date May 1, 1979
Page 1 of 6
6.0 CALCULATIONS
Calculation errors due to procedural or mathematical mis-
takes can be a part of total system error. Therefore, it is
recommended that each set of calculations be repeated or spot-
checked, preferably by a team member other than the one who
performed the original calculations. If a difference greater
than typical round-off error is detected, the calculations should
be checked step-by-step until the source of error is found and
corrected. A computer program is advantageous in reducing calcu-
lation errors. If a standardized computer program is used, the
original data entry should be included in the printout to be
checked; if differences are observed, a new computer run should
be made. Table 6.1 at the end of this section summarizes the
quality assurance activities for calculations.
Calculations should be carried out to at least one extra
decimal figure beyond that of the acquired data and should be
rounded off after final calculation to two significant digits for
each run or sample. All rounding off of numbers should be per-
formed in accordance with the ASTM 380-76 procedures. All calcu-
lations should then be recorded on a calculation form such as the
ones in Figures 6.1A and 6.IB, at the end of this section.
6.1 Nomenc1ature
The following nomenclature is used in the calculations.
CSO2 = concentrati°n of sulfur dioxide, dry basis
corrected to standard conditions, g/dscm
(Ib/dscf).
N = normality of barium perchlorate titrant,
meq/ml.
P, = barometric pressure at the exit orifice of the
dry gas meter, mm (in.) Hg.
P ., = standard absolute pressure, 760 mm (29.92
stct in.) Hg.
-------
Section No. 3.5.6
Revision No. 0
Date May 1, 1979
Page 2 of 6
T = dry gas meter average absolute temperature, K
/ O "T\ \
T ., = standard absolute temperature, 293K (528°R).
V = volume of sample aliquot titrated, ml.
a
V = dry gas volume measured by dry gas meter,
dcm (dcf).
, .j> = dry gas volume measured by dry gas meter,
* * t~*f*i V V" f\ /"^ "4" a n +• f^. f* ^ ^***w i^ —i *v» *3 ^-«^»ii^ ^ -i +- i ^™v»^ f* ^ r* S^Y*\ / /•
V
~n i c* ~r~ r\ i
corrected to standard conditions, dscm (dscf).
V , = total volume of solution in which the sulfur
dioxide sample is contained, 100 ml.
V. = volume of barium perchlorate titrant used for
the sample (average of replicate titrations), ml.
Vy^ = volume of barium perchlorate titrant used for
the blank, ml.
Y = dry gas meter calibration factor.
32.03 = equivalent weight of sulfur dioxide.
6 .2 C a,l cu 1 ajti ons
The following formulas for calculating the concentration of
sulfur dioxide are to be used along with example calculation
forms shown in Figures 6.1A and 6.IB.
6.2.1 Dry Sample Gas Volume, Corrected to Standard Conditions -
T P V P
v std bar „ v m bar Equation 6-1
Vm(std) = VmY Tm Pstd = K1Y Tm
where
K-, = 0.3858 K/mm Hg for metric units, or
= 17.64 °R/in. Hg for English units.
6.2.2 Sulfur Dioxide Concentration
/V - V ) N soln
V v f v -t-K ' V
^ ^P a Equation 6-2
-------
Section No. 3.5.6
Revision No. 0
Date May 1, 1979
Page 3 of 6
where
K2 = 32.03 mg/meq for metric units, or
= 7.061 x 10~5 Ib/meq for English units.
-------
Section No. 3.5.6
Revision No. 0
Date May 1, 1979
Page 4 of 6
Sample Volume
ft3, Tm = f^V.^OR, Pbar = *?•£ i. in. Hg, Y = /_.£ l_6_
_ -n c/i «• xx "i oar A / 9 A JT4.3
'm(std) - 17'64 InT-Sg- X T~^ =£•»"?. ft
Equation 6-1
S02 Concentration
N = --£ L 0 (g-eq)/ml, V = J /. Oml, V = _ £.O O ml
Vsoln = -'**'-*- ral' va = ^ -^
= 7.06 x 1C'5 t-tb= >0 x 1Q- cf
Vm(std)
Equation 6-2
Calculation form for data collected using Method 6
type equipment. The alternative use of Method 5 or
Method 8 equipment will change V and V /0^.,v to
TT _ f-t-^ m m^suu;
m(std) ' •
Figure 6.1A. Sulfur dioxide calculation form (English units).
-------
Sample Volume
Section No. 3.5.6
Revision No. 0
Date May 1, 1979
Page 5 of 6
V = ?; O.Q Q Si x 0.001 = Q.
m
m
= 1 £ 2- mm Hg, Y =
Vm(std) = °'3858
Equation 6-1
SO2 Concentration
N = .6/0 2.(g-eq)/ml, V. = / / .J O ml
_-___ -^ — _,^—
O. «O ml
v
soln = L « G-0 "I. va = >0_.0 ml
S0
= 32 . 03
m(std)
Equation 6-2
Calculation form for data collected using Method 6
type equipment. The alternative use of Method 5 or
Method 8 equipment will change V and vm/s+-d) to
Vm(std) = -• m •
Figure 6.IB. Sulfur dioxide calculation form (metric units)
-------
Section No. 3.5.6
Revision No. 0
Date May 1, 1979
Page 6 of 6
Table 6.1 ACTIVITY MATRIX FOR CALCULATION CHECKS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Analysis data
form
All data and calcula-
tions are shown
Visually check
Complete the
missing data
values
Calculations
Difference between
check and original cal-
culations should not
exceed round-off error
Repeat all calcula-
tions starting with
raw data for hand
calculations; check
all raw data input
for computer calcu-
lations; hand cal-
culate one sample per
test
Indicate
errors on
sulfur
dioxide cal-
culation form,
Fig. 6.1A or
6. IB
-------
Section No. 3.5.7
Revision No. 0
Date May 1, 1979
Page 1 of 3
7.0 MAINTENANCE
The normal use of emission-testing equipment subjects it to
corrosive gases, extremes in temperature, vibration, and shock.
Keeping the equipment in good operating order over an extended
period of time requires knowledge of the equipment and a program
of routine maintenance which is performed quarterly or after 2830
q
i (100 ft ) of operation, whichever is greater. In addition to
the quarterly maintenance, a yearly cleaning of the entire meter
box is recommended. Maintenance procedures for the various
components are summarized in Table 7.1 at the end of the section.
The following procedures are not required, but are recommended to
increase the reliability of the equipment.
7.1 Pump
In the present commercial sample train, several types of
pumps are used; the two most common are the fiber vane pump with
in-line oiler and the diaphragm pump. The fiber vane pump re-
quires a periodic check of the oiler jar. Its contents should be
translucent; the oil should be changed if not translucent. Use
the oil specified by the manufacturer. If none is specified, use
SAE-10 nondetergent oil. Whenever the fiber vane pump starts to
run erratically or during the yearly disassembly, the head should
be removed and the fiber vanes changed. Erratic operation of the
diaphragm pump is normally due to either a bad diaphragm (causing
leakage) or to malfunctions of the valves, which should be
cleaned annually by complete disassembly.
7.2 Dry Gas Meter
The dry gas meter should be checked for excess oil or corro-
sion of the components by removing the top plate every 3 mo. The
meter should be disassembled and all components cleaned and
checked whenever the rotation of the dials is erratic, whenever
the meter will not calibrate properly over the required flow rate
range, and during the yearly maintenance.
-------
Section No. 3.5.7
Revision No. 0
Date May 1, 1979
Page 2 of 3
7.3 Rotameter
The rotameter should be disassembled and cleaned according
to the manufacturer's instructions using only recommended clean-
ing fluids every 3 mo or upon erratic operation.
7.4 Sample Train
All remaining sample train components should be visually
checked every 3 mo and completely disassembled and cleaned or
replaced yearly. Many items, such as quick disconnects, should
be replaced whenever damaged rather than checked periodically.
Normally, the best procedure for maintenance in the field is to
use another entire unit such as a meter box, sample box, or
umbilical cord (the hose that connects the sample box and meter
box) rather than replacing individual components.
-------
Section No. 3.5.7
Revision No. 0
Date May 1, 1979
Page 3 of 3
Table 7.1. ACTIVITY MATRIX FOR EQUIPMENT MAINTENANCE CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurements
Action if
requirements
are not met
Routine main-
tenance
No erratic behavior
Routine maintenance
performed quarterly;
disassemble and
clean yearly
Replace parts
as needed
Fiber vane pump
In-line oiler free of
leaks
Periodically check
oiler jar; remove
head and change fiber
vanes
Replace as
needed
Diaphragm pump
Leak-free valves func-
tioning properly
Clean valves during
yearly disassembly
Replace when
leaking or
malfunctioning
Dry gas meter
No excess oil, corro-
sion, or erratic rota-
tion of the dial
Check every 3 mo
for excess oil or
corrosion by removing
the top plate; check
valves and diaphragm
whenever meter dial
runs erratically or
whenever meter will
not calibrate
Replace parts
as needed or
replace meter
Rotameter
Clean and no erratic
behavior
Clean every 3 mo or
whenever ball does
not move freely
Replace
Sample train
No damage
Visually check every
3 mo; completely dis-
assemble and clean
or replace yearly
If failure
noted, use
another entire
meter box,
sample box,
or umbilical
cord
-------
Section No. 3.5.8
Revision No. 0
Date May 1, 1979
Page 1 of 7
8.0 AUDITING PROCEDURE
An audit is an independent assessment of data quality.
Independence is achieved if the individual(s) performing the
audit and their standards and equipment are different from the
regular field crew and their standards and equipment. Routine
quality assurance checks by a field team are necessary in genera-
tion of good quality data, but they are not part of the auditing
procedure. Table 8.1 at the end of this section summarizes the
quality assurance functions for auditing.
234
Based on the results of collaborative tests ' ' of Method
6, two specific performance audits are recommended:
1. Audit of the analytical phase of Method 6.
2. Audit of data processing.
It is suggested that a systems audit be conducted as specified by
the quality assurance coordinator, in addition to these perform-
ance audits. The two performance audits and the systems audit
are described in detail in Subsections 8.1 and 8.2, respectively.
8.1 Performance Audits
Performance audits are made to quantitatively evaluate the
quality of data produced by the total measurement system (sample
collection, sample analysis, and data processing). It is recom-
mended that these audits be performed by the responsible control
agency once during every enforcement source test. A source test
for enforcement comprises a series of runs at one source. The
performance audit of the analytical phase is subdivided into two
steps: (1) a pretest audit which is optional and (2) an audit
during the actual analysis of the field samples which is re-
quired.
8.1.1 Pretest Audit of Analytical Phase Using Aqueous
Ammonium Sulfate (Optional) - The pretest audit described
in this subsection can be used to determine the proficiency of
the analyst and the standardization of solutions in the Method 6
-------
Section No. 3.5.8
Revision No. 0
Date May 1, 1979
Page 2 of 7
analysis and should be performed at the discretion of the agency
auditor. The analytical phase of Method 6 can be audited with
the use of aqueous ammonium sulfate samples provided to the
testing laboratory before the enforcement source test. Aqueous
ammonium sulfate samples may be prepared by the procedure de-
scribed in Section 3.5.5 on control sample preparation.
The pretest audit provides the opportunity for the testing
laboratory to check the accuracy of its analytical procedure.
This audit is especially recommended for a laboratory with little
or no experience with the Method 6 analysis procedure described
in this Handbook.
The testing laboratory should provide the agency/organiza-
tion requesting the performance test with a notification of the
intent to test 30 days prior to the enforcement source test. The
testing laboratory should also request that the agency/organiza-
tion provide the following performance audit samples: two
samples at a low concentration (500 to 1000 mg S02/dscm of
gas sampled or approximately 10 to 20 mg of ammonium sulfate per
sample) and two samples at a high concentration (1500 to 2500 mg
S02/dscm of gas sampled or about 30 to 50 mg of ammonium sulfate
per sample). At least 10 days prior to the enforcement source
test, the agency/organization should provide the four audit
samples. The concentration of the two low and the two high
audit samples should not be identical.
The testing laboratory will analyze one sample at the low
concentration and one at the high concentration, and submit their
results to the agency/organization prior to the enforcement
source test. (Note; The analyst performing this optional audit
must be the same analyst audited during the field sample analysis
described in Subsection 8.1.2).
The agency/organization determines the percent accuracy, %A,
between the measured SO2 concentration and the audit or known
values of concentration. The %A is a measure of the bias of the
analytical phase of Method 6. Calculate %A using Equation 8-1.
-------
Section No. 3.5.8
Revision No. 0
Date May 1, 1979
Page 3 of 7
- C
Equation 8-1
Cso2
where
C (M) = concentration measured by the lab analyst
2 mg/ml, and
C (A) = audit or known concentration of the audit
2 sample, mg/ml.
The recommended control limit for the pretest audit is the
90th percentile value for %A based on the results of three
audits (11/77, 5/78, and 10/78) performed by the Environmental
Monitoring and Support Laboratory, USEPA, Research Triangle Park,
North Carolina.13'14 By definition, 90% of the laboratory
participants in the audit obtained values of %A less than the
values tabulated below. The control limit is expected to be
exceeded by 10% of the laboratories to be audited, based on these
three audits. The 90th percentile values and the known audit con-
centrations are given below for each concentration range, 500 to
1000 mg S02/dscm and 1500 to 2500 mg SO2/dscm.
500 to 1000 mg SO2/dscm
Known audit
concentration 90th percentile for %A,
Audit date mg SO2/dscm %
5/78 686 4.1
10/78 572 6.4
1500 to 2500 mg SO2/dscm
Known audit
concentration 90th percentile for %A,
Audit date mg SO2/dscm 2a
11/77 1411 6.6
11/77 2593 4.0
5/78 2479 4.5
5/78 1907 4.5
10/78 2555 4.9
10/78 1754 5.2
-------
Section No. 3.5.8
Revision No. 0
Date May 1, 1979
Page 4 of 7
Based on the results of these audits, the recommended 90th per-
centile control limit for pretest audits is 7% for both con-
centration ranges.
If the results of the pretest audit exceed 7% the agency/
organization should provide the correct results to the testing
laboratory. After taking any necessary corrective action, the
testing laboratory should then analyze the two remaining samples
and report the results immediately to the agency/organization
before the enforcement source test analysis.
8.1.2 Audit of Analytical Phase Using Aqueous Ammonium
Sulfate (Required) - The agency should provide two
audit samples to be analyzed along with the field samples from
the enforcement source test. The purpose of this audit is to
assess the data quality at the time of the analysis. The
percent accuracy of the audit samples is determined using
Equation 8-1. The results of the calculated %A should be
included in the enforcement source test report as an
assessment of accuracy of the analytical phase of Method 8
during the actual enforcement source test.
8.1.3 Audit of Data Processing - Calculation errors are
prevalent in Method 8. Data-processing errors can be deter-
mined by auditing the data recorded on the field and
laboratory forms. The original and audit (check) calculation
should agree within roundoff; if not, all of the remaining
data should be checked. The data processing may also be
audited by providing the testing laboratory with specific data
sets (exactly as would occur in the field) and by requesting
that the data calculation be completed and that the results be
returned to the agency/organization. This audit is useful in
checking both computer programs and manual methods of data
processing.
8.2 Systems Audit
A systems audit is an on-site qualitative inspection and
review of the total measurement system (sample collection,
-------
Section No. 3.5.8
Revision No. 0
Date May 1, 1979
Page 5 of 7
sample analysis, data processing, etc.). Initially, a systems
audit is recommended for each enforcement source test, defined
here as a series of three runs at one source. After the test
team gains experience with the method, the frequency of audit
may be reduced—once for every four tests.
The auditor should have extensive background experience
in source sampling, specifically with the measurement system
being audited. The functions of the auditor are summarized in
the following:
1. Inform the testing team of the results of pretest
audits, specifying any area(s) that need special attention or
improvement.
2. Observe procedures and techniques of the field team
during sample collection.
3. Check/verify records of apparatus calibration checks
and quality control used in the laboratory analysis of control
samples from previous source tests, where applicable.
4. Record the results of the audit and forward them
with comments to the team management so that appropriate
corrective action may be initiated.
While on site, the auditor observes the source test team's
overall performance including the following specific
operations:
1. Setting up and leak testing the sampling train.
2. Preparing and adding the absorbing solution to the
impingers.
3. Checking for constant rate sampling.
4. Purging the sampling train.
Figure 8.1 is a suggested checklist for the auditor.
-------
Section No. 3.5.8
Revision No. 0
Date May 1, 1979
Page 6 of 7
Presampling Preparation
Yes No Comment
Q£ 1. Knowledge of process conditions
\S 2. Calibration of pertinent equipment, in particular,
the dry gas meter, prior to each field test
On-site Measurements
{/ 3. Leak testing of sampling train after sample run
4. Preparation and addition of absorbing solutions
to impingers
OK 5. Constant rate sampling
6. Purging of the sampling train and rinsing of the
impingers and connecting tubes to recover the
sample
7. Recording of pertinent process conditions during
sample collection
•^JtC 8. Maintaining the probe at a given temperature
Postsampling
9. Control sample analysis — accuracy and precision
Q/C 10. Sample aliquoting techniques
&t(. 11. Titration technique, particularly endpoint
precision
\s 12. Use of detection blanks in correcting field
sample results
13. Calculation procedure/check
14. Calibration checks
15. Standardized barium perchlorate solution
General Comments
3
t: fi*
Figure 8.1. Method 6 checklist to be used by auditors
-------
Section No. 3.5.8
Revision No. 0
Date May 1, 1979
Page 7 of 7
Table 8.1 ACTIVITY MATRIX FOR AUDITING PROCEDURE
Audit
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Analytical
phase using
aqueous
ammonium sul-
fate
Measured %A of the
pretest audit sample
should be less than the
90th percentile value,
7%
Frequency: Once dur-
ing every enforcement
source test
Method: Measure ref-
erence samples and
compare with true
values
Review oper-
ating tech-
nique
Data-processing
errors
The original and check
calculations within
round-off error
Frequency: Once dur-
ing every enforcement
source test
Method: Independent
calculations, starting
with recorded data
Check and
correct all
data for the
source test
Systems audit
Operation technique
described in this
section of the Hand-
book
Frequency: Once dur-
ing every enforcement
test until experience
gained, then every
fourth test
Method: Observation
of techniques, assist-
ed by audit checklist,
Fig. 8.1
Explain to
team the
deviations
from recom-
mended tech-
niques; note
on Fig. 8.1
-------
Section No. 3.5.9
Revision No. 0
Date May 1, 1979
Page 1 of 1
9.0 RECOMMENDED STANDARDS FOR ESTABLISHING TRACEABILITY
To achieve data of desired quality, two considerations are
essential: the measurement process must be in a state of statis-
tical control at the time of the measurement, and the systematic
errors, when combined with the random variation (errors of meas-
urement), must result in an acceptable uncertainty. To ensure
good quality data, it is necessary to perform quality control
checks and independent audits of the measurement process; to
document these data by means of a quality control chart as appro-
priate; and to use materials, instruments, and measurement proce-
dures that can be traced to an appropriate standard of reference.
Data must be routinely obtained by repeat measurements of
control standard samples and working standards. The working
calibration standards should be traceable to standards that are
considered primary, such as those listed below.
1. Dry gas meter must be calibrated against a wet test
meter that has been verified by an independent liquid displace-
ment method (Section 3.5.2) or by use of a spirometer.
2. The barium perchlorate is standardized against sulfuric
acid. The sulfuric acid should have been standardized with
primary standard grade potassium acid phthalate. The standard-
ized barium perchlorate should then be validated with an aqueous
solution of primary standard grade ammonium sulfate. This makes
the titrant solution traceable to two primary standard grade
reagents.
-------
Section No. 3.5.10
Revision No. 0
Date May 1, 1979
Page 1 of 3
10.0 REFERENCE METHOD*
METHOD 6—DETF.RMIVMION OF SI'LFI R )MOVIE
EMISSIONS i'XUM tiTATIO.VAKl bulKiL?)
1. Principle and Applicability
1.1 Principle A gas sample is eKrai'led from the
sampling point in tbe stack. The sulfuric aud misl
including sulfur tnoxlde) and the sulfur dioxide are
separated. Tbe sulfur dioxide fraction is measured by
tbe barium-lborm tltrdtlou method.
1.2 Apphcal'ibiy. Tins method is applicable for the
determination of sulfur dioxide emissions from stationary
sources. The minimum detectable limit of the method
has been determined to be 3.4 milligrams (mgi of SOi'm'
I2I2X10-' Ib'fl'). Although no upixr limit has been
established, tests have shown that concentrations as
high as 80,000 mg'tu* of SO: cnn be collected clliclcutly
ID two midget impingers, each containing 15 milljiter^
of 3 percent h\drogen peronde. at a rate of 1 0 1pm for
20 minutes Based on theoretical calculations, the upper
concentration limit in a 20-liter sample is about &3.31A)
Possible interforents are free ammonia, water-soluble
cations, and fluorides. TUe cations and fluorides are
remove J by glass wool tillers and an isopropanol bubbler.
and hence do not affect the SO: analysis. W hen samples
are being taken from a gas stream with high concentra-
tions of ver» line metallic fumes (such as in inlets to
eontiol devices), a high-elnciency glass fiber filter must
be used in place of the glass wool plug u.e., the one in
the probed to remove the cation mtcrCutnts.
Free anuuonia interferes by reacting with SO, to form
paniculate sulnte and by reacting with the indicator
If free ammonia is present (this can be determined by
knowledge of the process and noticing wbite paniculate
niatt«r tn the probe and isoprojttnol bubbler 1, alterna-
tive methods, subject to the approval of tbe Admimslra
tor, U.S. Environmental Trotei lion
required.
2.
Agency, an
.densatlon ana a tuter tenner in-stacs: or neatea om-
:k) to remove paniculate matter, Including sulfuric
1 mist. A plug of glass wool Is a satisfactory filter.
.1.2 Bubbler and Implngers. One midget bubbler,
2.1 Sampling. The sampling train Is shown In Figure
J-l, and component parts are discussed below. The
tetter has the option of substituting sampling equip-
ment described In Method 8 In place of tbe midget Im-
pinger equipment of Method 6. However, the Method 8
train must be modified to Include a heated filter between
the probe and Isopropanol Implnger, and the operation
of the sampling train and sample analysis must be at
tbe flow rates and solution volumes defined in Method 8.
The tester also has the option of determining SOi
simultaneously with paniculate matter and moisture
determinations by (1) replacing the water In a Method 5
Impinger system with 3 percent perioxide solution, or
(2) by replacing tbe Method 5 water Impinger system
with a Method 8 isopropanol-filUr-peroxlde system. The
analysis for SOt must be consistent with the procedure
In Method 8.
2.1.1 Probe. BorosUlcate glass, or stainless steel (other
materials of construction may be used, subject to the
approval of tbe Administrator), approximately fvmra
Inside diameter, with a heating system to prevent water
condensation and a filter (either in-slack or heated out-
stack) ' '
acid m
2 1 2 __ _
wit'h'medium-coarse glass'frit and borosilicate or quarts
glass wool packed In top (see Figure 6-1) to prevent
sulfuric acid mist carryover, and three 30-ml midget
tmpingera. Tbe bubbler and midget Implngers must be
connected In series with leak-free glass connectors. 8111-
eone srease may be nsed, if necessary, to prevent leakage.
At the option of tbe tester, a midget Implnger may be
used In place of the midget bubbler.
Other collection absorbers and flow rates may be used,
but are subject to the approval of the Administrator.
Also, collection efficiency must be shown to be at least
90 percent for each test run and must be documented in
the report. If tbe efficiency Is found to be acceptable after
a series of three tests, further documentation Is not
required. To conduct the efficiency test, an extra ab-
sorber must be added and analysed separately. This
extra absorber must not contain more than 1 percent of
the totaled.
2.14 Glass Wool. Borosilicate or quarts.
1.1.4 Stopcock Grease. Acetone-Insoluble, beat-
stable tlllcone grease may be used. If necessary.
1.1.5 Temperature Gauge, Dial thermometer, or
equivalent, to measure temperature of gas leaving Im-
plnger train to within 1* C (2* F.)
11 .e Drying Tube. Tube packed with 6-to 16-meih
Indicating type silica gel, or equivalent, to dry the gas
sample and to protect the meter and pump. If the tUlac
gel has been used previously, dry at 175* C (350* F) for
2 hours. New silica gel may be used si received. Alterna-
tively, other types of deslccants (equivalent or better)
may be used, subject to approval of the Administrator.
2.1.7 Value. Needle value, to regulate sample gas flow
rate
2.1.8 Pump. Leak-tree diaphragm pump, or equiv-
alent, to pull gas through the train. Install a small tank
between the pump and rate meter to eliminate the
pulsation effect of the diaphragm pump on the rotameter.
2.1.9 Rate Meter. Rotameter, or equivalent, capable
of measuring flow rate to within 2 percent r< thj selected
flOTr rate of about 1000 cc/mlu.
2.1.10 Volume Meter. Dry gas meter, sufficiently
accurate to measure the sample volume within 2 percent,
calibrated at the selected flow rate and conditions
actually encountered during sampling, and equipped
with a temperature gauge (dial thermometer, or equiv-
alent) capable of measuring temperature to within
3"C <5.4°F ).
2.1.11 Barometer. Mercury, amerold, or other barom-
eter capable of measuring atmospheric pressure to within
2.1 mm Hg (0 1 In. Hg). In many cases, the barometric
reading may be obtained from a nearby national weather
service station, In which case, the station value (which
Is the absolute barometric pressure) shall be requested
and an adjustment for elevation difference* between
the weather station and sampling point shall be applied
atarateofmmus2.5mmHg(0.1ln. Hg) per30m (100ft)
elevation Increase or vice versa for elevation decrease
2.1.17 Vacuum Gauge. At least 760 mm Hg (30 in.
Hg) gauge, to be used for leak check of the sampling
train.
2.2 Sample Recovery.
2.2.1 Wash bottles. Polyethylene or (lass, MO ml,
two.
2.2.2 Storage Bottles. Polyethylene, 100 ml, to store
Impinger samples (one per sample).
2.3 Analysis
2.3.1 Pipettes. Volumetric type, 5-ml, 20-ml (one per
sample), and 25-ml sizes.
2.3.2 Volumetric Flasks. 100-ml slse (one per sample)
and 100-ml site.
2.3.3 Burettes. 5- and 50>ml slses.
2.3.4 Erlenmeyer Flasks. 260 mi-else (on* for each
sample, blank, and standard).
2.3.5 Dropping Bottle. 125-ml site, to add Indicator.
2.3.6 Graduated Cylinder. 100-ml site.
2.3.7 Bpectropbotometer. To measure absorbance at
862 nanometers
3. Ragentt
Unless otherwise Indicated, all reagents must conform
to the speclfuatlons established by the Committee on
Analytical Reagents of the American Chemical Society.
Where such specifications are not available, use tbe best
available grade.
3.1 Sampling.
3.1.1 WaterTDelonited, distilled to conform to ASTM
specification D1193-74, Type 3. At the option of tbe
analyst, the KMnO4 test for oxldizable organic marur
may be omitted when high concentrations of org&nu
matter are not expected to M present.
a.l 2 Isopropanol. 80 percent. Mn 80 ml of isopropanol
with 30ml of deionited, distilled water. Check each lot of
Isopropanol for peroxide Impurities as follows: sbakr 10
ml of isopropanol with 10 ml of freshly prepared 10
percent potassium Iodide solution. Prepare a blank by
similarly treating 10 ml of distilled water. After 1 minute.
read the absorbance at 342 nanometers on a spectra-
photometer. If absorbance exceeds 0 1, reject alcohol for
use.
Peroxides may be removed from isopropanol by redis-
tilling or by passage through a column of activated
alumina; however, reagent grade Isopropanol "with
suitably low peroxide levels may be obtained from com-
mercial sources Rejection of contaminated lots may,
therefore, be a more efficient procedure.
8.1 3 Hydrogen Peroxide, S Percent. Dilute 80percent
hydrogen peroxide 1:9 Wv) with deionued, distilled
water (80 ml Is needed per sample). Prepare fresh daily
814 Potassium Iodide Solution, 10 Percent. Dissolve
10.0 grams Kl in detonited, distilled water and dlluu- to
100 ml. Prepare when needed.
8.2 Sample Recovery.
8.2.1 Water. Deioniied, distilled, as in 3 1 1.
8.2.2 Isopropanol. 80 Percent. Mil 80 ml of isopropanol
with 20 ml of deioniied, distilled water.
8 3.1 Water9Delonited, distilled, as In 3.1.1.
8.8.2 Isopropanol, 100 percent.
8.33 Thorin Indicator i-(o-arsonophenylato)-2-
naphthol-3,6-disulfonlc acid, dlsodlum salt, or equiva-
lent. Dissolve 0.20 g In 100 ml of delonited, distilled
water.
3.8.4 Barium Ferchlorate Solution, 0.0100 N. Di«-
solve 1.991 of barium percblorate trthydrats |Ba(flO.)r
SHiO] In 200 ml distilled water and dilute to 1 liter with
sopropanol. Alternatively, 1 22 g of (BaClr2H>O) ma\
be used Instead of tbe perchlorate. Standardise as in
Section 5.5.
3.3 5 Sulfuric Acid Standard, 00100 N. Purchase or
standardise to •0.0002 N against 0 0100 N NaOH which
has previously been standardized against potassium
acid phthalate (primary standard grade).
4. Pmudurt.
4.1 Sampling. , .
4.1.1 Preparation of collection train. Measure 15 ml of
80 percent isopropanol Into the midget bubbler and 15
ml of 3 percent hydrogen peroxide into each of the first
two midget Implngera. Leave the final midget Implnger
dry Assemble the train as shown In Figure 6-1. Adjust
probe heater to a temperature sufficient to prevent w ater
condensation. Place crushed ice and water around the
implngers
4 1 - Leak-check procedure A leak check prior to the
sampling run is optional, however, a leak check after the
sampling run is mandatory. The leak-check procedure is
as follows:
With the probe disconnected, place a vacuum gauge at
the inlet to the bubbler and pull a vacuum of 250 mm
(10 In ; Hg: plug or pinch olf the outlet of the flow meter,
and then turn off the pump. The vacuum shall remain
stable for at least 30 seconds. Carefully release the
vacuum gauge before releasing the flow meter end to
prevent back flow of the tmpinger fluid.
Other leak check procedures may be used, subject to
the approval of the Administrator, U S Environmental
Protection Agency. The procedure used in Method 5 Is
not suitable for diaphragm pump*:
4 1 3 Sample collection Record the initial dry gas
meter reading and barometric pressure To begin sam-
pling, position the tip of the probe at the sampling point,
\onnect the probe to the bubbler, and start the pump
Adjust the sample flow to a constant rate of ap-
proximately 1 0 liter'mm as Indicated by the rotameter
Nfaintam this constant rate (*10 percent) during the
entire sampling run Take reading? • (dry gas meter.
temperatures at dry gas meter and at impinger outlet
and rate meter) at least every 5 minutes. Add more ice
during the run to keep the temperature of the gases
leaving the last impinger at 20° C (68« F) or less At the
conclusion of each run, turn off the pump, remove probe
from the stack, and record the final readings. Conduct a
leak check as in Section 412 (This leak check is manda-
tory ) If a leak Is found, void the test run. Drain the Ice
bath, and purge the remaining part of the train by draw-
ing clean ambient air through the system for 15 minutes
at the sampling rate
Clean ambient air can be provided by passing air
through a charcoal filter or through an extra midget
Impinger with 15 ml of 3 percent H:0i. The tester may
opt to simply use ambient air, without purification.
4 2 Sample Recovery. Disconnect the Implngers alter
purging. Discard the contents of the midget bubbler Pour
the contents of the midget impingers Into a leak-free
polyethylene bottle for shipment. Rinse the three midget
impingers and the connecting tubes with delonited
distilled water, and add the washings to the same storage
container. Mark the fluid level. Seal and Identify the
sample container.
4 8 Sample Analysis. Note level of liquid in container,
and confirm whether any sample was lost during ship-
ment; note this on analytical data sheet. If a noticeable
amount of leakage has occurred, either void the sample
or use methods, subject to the approval of the Adminis-
trator, to correct the final results.
Transfer the contents of the storage container to a
100-ml volumetric flask and dilute to exactly 100 ml
with deionlted, distilled water. Pipette a 20-ml aliquot of
this solution into a 250-ml Erlenmeyer flask, add 80 ml
of 100 percent Isopropanol and two to four drops of thorin
indicator, and titrate to a pink endpoint using 0 0100 N
barium perchlorate. Repeat and average the titration
volumes. Bun a blank with each series of samples. Repli-
cate tltrations must agree within 1 percent or 0.2 ml,
whichever Is larger.
(NOTi.—Protect the 0.0100 N barium perchlorate
solution from evaporation at all times.)
5. CUftrolfm
5.1 Metering System.
5 1.1 Initial Calibration. Before Its Initial use in the
field, first leak check the metering system (drying tube,
needle valve, pump, rotameter, and dry gas meter) as
follows: place a vacuum gaute at the inlet to the drying
tube and pull a vacuum of 250 mm (10 In.) Hg; plug or
pinch on the outlet or the flow meter, and then turn off
the pump. The vacuum shall remain stable'for at least
30 seconds. Carefully release the vacuum gaute befor*
releasing the flow meter end.
Next, calibrate the meterinf system (at the sampling
flow rate specified by the method) as follows: connect
an appropriately sited wet test meter (e.g., 1 liter per
revolution) to the Inlet of the drying tube. Make three
Independent calibration runs, using at least five revolu-
tions of the dry gas meter per run. Calculate tbe calibra-
tion factor, y (wet test meter calibration volume divided
by the dry gas meter volume, both volumes adjusted to
the same reference temperature and pressure), for each
run, and average the results. If any r value deviates by
more than 2 percent from tbe average, the metering
system Is unacceptable for use. Otherwise, use the aver*
age as the calibration factor tor subsequent test runs.
5.1.2 Post-Test Calibration Cheek. After each field
test series, conduct a calibration cheek as In Section 5.11
above, except for the following variations: (a) tbe leak
check Is not to be conducted, (b) three, or more revela-
tions of the dry gas meter may be used, and (c) only two
independent runs need be made. If the calibration factor
does not deviate by more than 5 percent from the Initial
calibration factor (determined In Section 9.1.1), then the
dry gas meter volumes obtained during the test series
are acceptable. If the calibration factor deviates by more
than 5 percent, recalibrate the metering system as la
Section 5.1.1, and for the calculations, use the calibration
factor (initial or recalibratlon) that yields the lower gas
volume ,'jr each test run.
*40 CFR 60, Ju,ly 1, 1978
-------
Section No. 3.5.10
Revision No. 0
Date May 1, 1979
Page 2 of 3
5 '1 Thermometers. Calibrate Hgalnst mereurj-ln-
Sl&ss thermometers.
5 3 Rotametrr. The rot unetcr need not be calibrated
but should be cleaned and maintained according to the
manufacturer's Instruction.
5.4 Barometer. Calibrate against a mercury barom-
eter.
5.5 Barium Perchlorate Solution. Standardize the
barium perchlorate solution against 25 ml of standard
sulfuric acid to which 100 ml ot 100 percent Isopropanol
has been added.
«. Caleubamt
Carry out calculations, retaining at least one extra
decimal figure beyond that of the acquired data. Round
on figures after final calculation.
8.1 Nomenclature.
C"»-Concentration ot nlfur dioxide, dry basis
* corrected to standard conditions, mg/dsem
(Ib/dscf).
.V-Normality of barium perchlorate tltrant,
mlUlequivalents/ml.
Fb.,-Barometric pressure at the exit orifice of the
dry gas meter, mm Hg (in. Hg).
Au* Standard absolute pressure, 760 mm Hg
(29.92 In. Hg).
7".-Average dry gas meter absolute Umperatnre,
r.u-Standard absolute temperature, 283* K
V.-Volume of sample aliquot titrated, ml.
V,»Dry fas Tolnme as measured by the dry ge»
meter, dcm(dcf).
V\.(.id) — Dry gas votunje measured by the firy gu
meter, corrected to standard conditions,
dscm (dscf).
VMiB»Total volume of solution In which the sulfur
dioxide sample Is contained, 100ml.
Vi»Volume of barium perchlorate titrant used
for the sample, ml (average of replicate
titretlons).
Vit»Volume of barium perchlorate tltrant used
for the blank, ml.
V- Dry gas meter calibration factor.
32.03- Equivalent weight ot sulfur dioxide.
6.2 Dry sample gas volume, corrected to standard
conditions.*
Equation t-i
when:
Ki-O.XS» *K/nun Hg for metric units.
-17.M °R/ln. Hg for English units.
«J Sulfur dioxide concentration.
where:
Xi-32.03 mg/meq. for metric units.
-7.M1X10-* Ib/meq. for English units.
Equation 8-2
1. Atmospheric Emissions from Kulfuric Acid Manu-
facturing Prowsws. U.S. D11EW, PHS. Division cT Air
Pollution. Public Health Service Publication No.
K99-AP-13. Cinciruiatl, Ohio. 196S.
2. Corbett, P. F. The Determination of SOi and SOi
In Flue Oases. Journal ot the Institute of Fuel. 14: 237-
243,1M1.
3. Matty, R. E. and E. K. Dlehl. Measuring Flue-Gas
SOi and SO*. Power. 101:94-67. November 1957.
4. Fatten, W. F. and I. A. Brink, Jr. New Equipment
and Techniques for Sampling Chemical Process Ut&es.
1. Air Pollution Control Association. 13:182. 1903.
5. Rom, 1.}. Maintenance. Calibration,and Operation
ot Isokinetie Source-Sampling Equipment. Office of
Air Programs, Environment^ Protection Agency.
Research Triangle Park, N.C. APTD-0578. March 1972.
S. Hamll, H. F. and D. E. Camann. Collaborative
Study of Method for the Determination of Bulfur Dioxide
Emissions from Stationary Sources (Fossil-Fuel Fired
Steam Generators). Environmental Protection Agency,
Research Triangle Park, N.C. EPA-«M/«-;t-024.
December 1973.
7. Annual Book of ASTM Standards. Part 31; Water,
Atmospheric Analysis. American Society for Testing
and Materials. Philadelphia, Pa. 1974. pp. 40-42.
8. Knoll, JTf E. and M. R. Mldgett. The Application of
EPA Method a to High SuUur Dioxide Concentrations.
Environmental Protection Agency. Research TrUnglo
Pwk. N.C. EPA-WO/4-78-038. July 1976.
THERMOMETER
PROBE (END PACKED'
WITH QUARTZ OR
PYREX WOOL)
A
WM
' STACK WALL
/MID
GLASS WOOL
\
MIDGET IMPINGERS
MIDGET BUBBLER
SILICA GEL
DRYING TUBE
KfcTEHETER NEEDLE VALVE
PUMP
Figure 6-1. S02 sampling train.
SURGE TANK
-------
Amendments to Reference Method 8; Correction*
In Method 6 of Appendix A, Sections
2.1. 2.1.6. 211.7. 2.1.8. 2.1.11. 2.1.12.
2.3.2. 3.3.4. 4.1JZ, 4.L3. and 5.1.1 are
amended as follow*:
1. In Section 2.1, the word "periox-
ide" in the fourth line of the second
paragraph is corrected to read "perox-
ide."
2. In Section 2.1.6, the word "siliac"
in the third line Is corrected to read
"silica."
3. In Section .2.1.7. the word "value".
which appears twice is corrected to
read "valve,"
4. In Section 2.1.8, the word "disph-
ragm" is corrected to read "dia-
phragm" and the word "surge" is In-
serted between the words "small" and
"tank."
5. In Section 2.1.11, the word "amer-
oid" is corrected to read "aneroid."
6. In Section 2.1.12, the phrase "and
Rotameter." is inserted after the
phrase "Vacuum Gauge" and the
phrase "and 0-40 oc/min rotameter" Is
inserted between the words -"gauge"
and ". to."
7. In Section 2.3.2. the phrase "and
100-ml size" is corrected to read "and
1000-ml size."
8. In Section 3.3.4. the word "sopro-
panol" in the fourth line is corrected
to read "isopropanol."
fl. In Section 4.1.2, delete the last
sentence of the last paragraph. Also
delete the second paragraph and re-
place it with the following paragraphs:
Temporarily attach a suitable (e.g., 0-40
cc/mta) rotameter to the outlet of the dry
gas meter and place a vacuum gauge at or
•near the probe inlet. Plug the probe Inlet,
pull a vacuum of at least 250 mm Hg (10 in.
Hg>, and note the flow rate as indicated fay
the rotameter. A leakage rate not in excess
of 2 percent of the average sampling rate Is
acceptable.
NOTE Carefully release the probe Inlet
plug before turning off the pump.
It is suggested (not mandatory) that the
pump be leak-checked separately, either
prior to or after the sampling run. If done
prior to the sampling run, the pump teak-
check shall precede the leak check of the
sampling train described immediately above;
if done after the sampling run. the pump
leak-check shall follow the train leak-check.
To leak check the pump, proceed as follows:
Disconnect the drying tube from the probe-
imptnger assembly. Place a vacuum gauge at
the inlet to either the drying tube or the
tpump, pull a vacuum of 250 """ (10 in.) Hg.
plug or pinch off the outlet of the flow
meter and then turn off the pump. Trie
vacuum should remain stable for at least 30
seconds.
10. In Section 4.1.3, the sentence "If
a leak is found, void the test run" on
the sixteenth line is corrected to read
"If a leak Is found, void the test run. or use
procedures acceptable to the Administrator
to adjust the wimple volume tor the leak-
age."
11. In Section 5.1.1, the word "or" on
the sixth line is corrected to read "of."
Section No. 3.5.10
Revision No. 0
Date May 1, 1979
Page 3 of 3
*Federal Register, Vol. 43, No. 57-March 23, 1978
-------
Section No. 3.5.11
Revision No. 0
Date May 1, 1979
Page 1 of 2
11.0 REFERENCES
1. 40 Code of Federal Regulations 60. July 1, 1978.
2. Hamil, F. Laboratory and Field Evaluations of EPA
Methods 2, 6, and 7. Report No. EPA- 650/4-74-026.
Southwest Research Institute, San Antonio, Tex. 1974.
3. Hamil, F., and David E. Camann. Collaborative Study of
Method for the Determination of Sulfur Dioxide Emis-
sions from Stationary Sources. Report No. EPA-650/4-
74-024. National Environmental Research Center, Envi-
ronmental Protection Agency, Research Triangle Park,
N.C. December 1973.
4. Hamil, F., David E. Camann, and Richard E. Thomas.
The Collaborative Study of EPA Methods 5, 6, and 7 in
Fossil Fuel-Fired Steam Generators. Final Report No.
EPA-650/4-74-013. Southwest Research Institute, San
Antonio, Tex. September 1974.
5. Quality Assurance Handbook for Air Pollution Measure-
ment Systems, Vol. I, Principles. EPA-600/9-76-005.
Environmental Protection Agency, Research Triangle
Park, N.C. March 1976.
6. Guidelines for Development of a Quality Assurance
Program: Volume V - Determination of Sulfur Dioxide
Emissions from Stationary Sources. EPA-650/4-74-005.
Research Triangle Institute, Research Triangle Park,
N.C. November 1975.
7. McCoy, Richard A., David E. Camann, and Herbert C. McKee.
Collaborative Study. Reference Method for Determin-
ation of Sulfur Dioxide in the Atmosphere (Pararos-
aniline Method). EPA-650/4-74-027. December 1973.
8. Smith, Franklin, and Carl Nelson, Jr. Guidelines for
Development of a Quality Assurance Program. EPA-R4-73-
028d. August 1973.
9. Fuerst, Robert G. Improved Temperature Stability of
Sulfur Dioxide Samples Collected by the Federal Refer-
ence Method. EPA-600/4-78-018, April 1978.
-------
Section No. 3.5.11
Revision No. 0
Date May 1, 1979
Page 2 of 2
10. Knoll, Joseph E., and Midgett, M. Rodney. The Applica-
tion of EPA Method 6 to High Sulfur Dioxide Concentra-
tions. EPA-600/4-76-038. July 1976.
11. Osborne, Michael C., and Midgett, M. Rodney. Survey of
Continuous Source Emission Monitors: Survey No. 1 NO
and S02. EPA-600/4-77-022. April 1977.
12. Buchanan, J. N., and Wagoner, D. E. Guidelines for
Development of a Quality Assurance Program: Volume
VII - Determination of Sulfuric Acid Mist and Sulfur
Dioxide Emissions from Stationary Sources. EPA-650/4-
74-005g. March 1976.
13. Fuerst, R. G., R. L. Denny, and M. R. Midgett. A
Summary of Interlaboratory Source Performance Surveys
for EPA Reference Methods 6 and 7 - 1977. Available
from U.S. Environmental Protection Agency, Environmental
Monitoring and Support Laboratory (MD-77), Research
Triangle Park, N.C. 27711.
14. Fuerst, R. G., and M. R. Midgett. A Summary of Inter-
laboratory Source Performance Surveys for EPA Reference
Methods 6 and 7 - 1978. Report in preparation by U.S.
Environmental Protection Agency, Environmental Monitoring
and Support Laboratory (MD-77), Research Triangle Park,
N.C. 27711.
-------
Section No. 3.5.12
Revision No. 0
Date May 1, 1979
Page 1 of 13
12.0 DATA FORMS
Blank data forms are provided on the following pages for the
convenience of the Handbook user. Each blank form has the cus-
tomary descriptive title centered at the top of the page. How-
ever, the section-page documentation in the top right-hand corner
of each page of other sections has been replaced with a number in
the lower right-hand corner that will enable the user to identify
and refer to a similar filled-in form in a text section. For
example, Form M6-1.2 indicates that the form is Figure 1.2 in
Section 3.5.1 of the Method 6 Handbook. Future revisions of
these forms, if any, can be documented as 1.2A, 1.2B, etc. Thir-
teen of the blank forms listed below are included in this sec-
tion. Five are in the Method Highlights subsection as shown by
the MH following the form number.
Form Title
1.2 Procurement Log
2.2 Wet Test Meter Calibration Log
2.4A and 2.4B Dry Gas Meter Sample Calibration Data
(English and metric units)
2.5 (MH) Pretest Sampling Checks
3.1 (MH) Pretest Preparations
4.1 Sampling Data Form for SO2
4.2 Sample Label
4.3 Sample Recovery and Integrity Data
4.4 (MH) On-Site Measurements
5.1 (MH) Posttest Sampling Checks
5.2 Sulfur Dioxide Analytical Data
5.3 Control Sample Analytical Data
5.4 (MH) Posttest Operations
-------
Section No. 3.5.12
Revision No. 0
Date May 1, 1979
Page 2 of 13
6.1A and 6.IB Sulfur Dioxide Calculation Forms
(English and metric units)
8.1 Method 6 Checklist To Be Used by
Auditors
-------
PROCUREMENT LOG
Item description
Qty.
Purchase
order
number
Vendor
Date
Ord.
Rec.
Cost
Dispo-
sition
Comments
Quality Assurance Handbook M6-1.2
-------
WET TEST METER CALIBRATION LOG
Wet test meter serial number
Date
Range of wet test meter flow rate
Volume of test flask V =
s
Satisfactory leak check?
Ambient temperature of equilibrate liquid in wet test meter and reservoir
Test
number
1
2
3
Manometer
reading,
mm H,,O
Final
volume (Vf),
£
Initial
volume (V. ) ,
& x
Total ,
volume (V ) ,
£ m
Flask
volume (V ),
£ s
Percent
error,
°/
/o
Must be less than 10 mm (0.4 in.)
Calculations:
b Vm = Vf - V
% error = 100 (vm -
(+1%).
Signature of calibration person
Quality Assurance Handbook M6-2.2
-------
DRY GAS METER SAMPLE CALIBRATION DATA
(English units)
Date
Calibrated by
Meter box number
Barometer pressure. P =
m
Dry test meter temperature correction factor
in. Hg Wet test meter number
°F
Wet test
meter
pressure
drop (Dm),£
in. H20
Rota-
meter
setting
(Rs),
ft /min
Wet test
meter gas
volume
b
ft3
Dry test meter
gas volume
(vd),bft3
Initial
Final
Wet test
meter
gas temp
>
°FX
Dry test meter
Outlet
gas temp
(t,),
o
°F
Average
gas temp
(td),C
°F
Time
of run
(6) d
min
Average
ratio
(Y^,6
(Y )/
i
D expressed as negative number.
Volume passing through meter. Dry gas volume is minimum for at least five revolutions of the meter.
The average of
and t if using two thermometers; the actual reading if using one thermometer.
The time it takes to complete the calibration run.
With Y defined as the average ratio of volumes for the wet test and the dry test meters, Y. = Y +0.02 Y for
Y +0.05 Y for the posttest checks, thus, X
calibration and Y.
i
TT fmM
V (t, + 460 F) P + (D /13.6)
w d m m
V.
w
460UF) (pm)
(Eq. 1)
Y =
« |^ « |^ -IT
(Eq. 2)
With Y defined as the average ratio of volumetric measurement by wet test meter to rotameter.
Tolerance Yr = 1 +0.05 for calibration and Y +0.1 for posttest checks
V
w
460°F)
(Dm/13.6)| (60)
0 (t + 460°F) (P ) (0.035)
iw HI
(Eq. 3)
Y =
(Eq. 4)
Quality Assurance Handbook M6-2.4A
-------
DRY GAS METER SAMPLE CALIBRATION DATA
(metric units)
Date
Calibrated by
Meter box number
Barometer pressure, P =
Dry test meter temperature correction factor
mm Hg Wet test meter number
°C
Wet test
meter
pressure
drop (Dm),a
mm H20
Rota-
meter
setting
bji
Initial
Final
Wet test
meter
gas temp
< v .
°c
Dry test meter
Inlet
gas temp
v
°C
Outlet
gas temp
-------
SAMPLING DATA FORM FOR SO,
Plant name
Sample location
Operator
City
Date
Sample number
Barometric pressure, mm (in.) Hg
Probe material
Meter box number
Ambient temperature, °C (°F)
Initial leak check
Final leak check
Probe length m (ft)
Probe heater setting
Meter calibration factor (Y)
Sample point location
Sample purge time, min
Remarks
Sampling
time,
min
Total
Clock
time,
24 h
Sample
volume,
SL (ft3)
Total
Sample flow
rate setting,
3
£/min (ft /min)
Sample volume
metered (AV ) ,
3 m
si (ff3)
AV
m
avg
Percent
0
deviation,
%
Avg
dev
Dry gas
meter temp,
°C (°F)
Avg
Impinger
temp,
°C (°F)
Max
temp
Percent deviation =
AV - AV avg
m m 6
AV avg
100.
m
Quality Assurance Handbook M6-4.1
-------
SAMPLE LABEL
Plant City
Site Sample type
Date Run number
Front rinse LJ Front filter 0 Front solution CH
Back rinse LJ Back f ilter CH Back solution [H
Solution Level marked d «
x
Volume: Initial Final ^
Cleanup by I
ul
Quality Assurance Handbook M6-4.2
-------
Plant
SAMPLE RECOVERY AND INTEGRITY DATA
Sample location
Field Data Checks
Sample recovery personnel
Person with direct responsibility for recovered samples
Sample
number
1
2
3
4
5
6
Blank
Sample
identification
number
Date
of
recovery
Liquid
level
marked
Stored
in locked
container
Remarks
Signature of field sample trustee
Laboratory Data Checks
Lab person with direct responsibility for recovered samples
Date recovered samples received
Analyst
Sample
number
1
2
3
4
5
6
Blank
Sample
identification
number
Date
of
analysis
Liquid
at marked
level
Sample
identified
Remarks
Signature of lab sample trustee
Quality Assurance Handbook M6-4.3
-------
SULFUR DIOXIDE ANALYTICAL DATA
Plant
Date
location
and normality of barium
hlorate
Analyst
1
2
3
ml
ml
ml
N
N
N
N, avg
Sample
number
1
2
3
4
5
6
Blank
Sample
identification
number
Total
sample
volume
(V.oln>'
ml
N/A
Sample
aliquot
volume
(va)?
ml
Volume of titrant (V ) , ml
1st
titration
2nd
titration
Average
V^ =
Volume for the blank must be the same as that of the sample aliquot.
1st titration
2nd titration
= 0.99 to 1.01 orjlst titration - 2nd titration|<0.2 ml.
Signature of analyst
Signature of reviewer or supervisor
Quality Assurance Handbook M6-5.2
-------
CONTROL SAMPLE ANALYTICAL DATA FORM
Plant
Date analyzed
Analyst
N.
Ba(Cl04)2
Weight of ammonium sulfate is 1.3214 g?
Dissolved in 2 S, of distilled water?
Titration of blank
ml Ba(ClO4)2 (must be < 0.5-ml)
Control
sample
number
Time of
analysis,
24 h
Titrant volume ,a ml
1st
2nd
3rd
Avg
Two titrant volumes must agree within 0.2 ml.
ml Ba(C10 ) x N
t
25 ml x 0.01N
(Control sample) (control sample)
ml x
N =
(must agree within +5%, i_e., 0.238 to 0.262)
Does value agree? yes no
Signature of analyst
Signature of reviewer
Quality Assurance Handbook M6-5.3
-------
SULFUR DIOXIDE CALCULATION FORM
(English units)
Sample Volume3
vm = _• ft3, Tm = ._ °R, Pbar = __.__ in. Hg, Y = _.
O Y V P
V = 17 64 R m
17'64
m(std) ' in. Hg T
m
Equation 6-1
SO- Concentration
N = _. (g-eq)/ml, V. = . ml, V., = . ml
t ~~~ ^ "~" ~~ "CD — — —. —.
Vsoln = --- -_ _ ml, Va = _ _ ._ ml
= 7.06 x 1(T5 t tb ^ x 1Q- lb/dgcf
Vm(std)
Equation 6-2
Calculation form for data collected using Method 6
type equipment. The alternative use of Method 5 or
Method 8 equipment will change V and V , .,. to
TI _ -r.3 m m(std)
m(std) ~ ' rt •
Quality Assurance Handbook M6-6.1A
-------
SULFUR DIOXIDE CALCULATION FORM
(metric units)
Sample Volume
V = . H x 0.001 = . m
in —• — — — ___ __
Tm = •- K' pbar = . mm Hg, Y = _.
Y V P
. _oco K m bar 3
Vm(std) = °-3858 = 'm
Equation 6-1
SO2 Concentration
N = . (g-eq)/ml, V = . ml, V , = . ml
V , = . ml, V = .ml
soln a
N (V - V ) (V , /V )
r =32.03 ^ J* §£ln__a_ = _ _. mg/dscm
S02 Vm(std)
Equation 6-2
Calculation form for data collected using Method 6
type equipment. The alternative use of Method 5 or
Method 8 equipment wi^l change Vm and vm(st(j) to
V ,.,.
m(std)
Quality Assurance Handbook M6-6.1B
-------
METHOD 6 CHECKLIST TO BE USED BY AUDITORS
Presampling Preparation
Yes No Comment
___ 1. Knowledge of process conditions
2. Calibration of pertinent equipment, in particular,
the dry gas meter, prior to each field test
On-site Measurements
3. Leak testing of sampling train after sample run
4. Preparation and addition of absorbing solutions
to impingers
5. Isokinetic sampling
6. Purging of the sampling train and rinsing of the
impingers and connecting tubes to recover the
sample
7. Recording of pertinent process conditions during
sample collection
8. Maintaining the probe at a given temperature
Postsampling
9. Control sample analyses—accuracy and precision
10. Sample aliquoting techniques
11. Titration technique, particularly endpoint
precision
12. Use of detection blanks in correcting field
sample results
13. Calculation procedure/check
14. Calibration checks
15. Standardized barium perchlorate solution
General Comments
Quality Assurance Handbook M6-8.1
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 1 of 11
Section 3.6
METHOD 7--DETERMINATION OF NITROGEN OXIDE
EMISSIONS FROM STATIONARY SOURCES
OUTLINE
Section
SUMMARY
METHOD HIGHLIGHTS
METHOD DESCRIPTION
1. PROCUREMENT OF APPARATUS
AND SUPPLIES
2. CALIBRATION OF APPARATUS
3. PRESAMPLING OPERATIONS
4. ON-SITE MEASUREMENTS
5. POSTSAMPLING OPERATIONS
6. CALCULATIONS
7. MAINTENANCE
8. AUDITING PROCEDURE
9. RECOMMENDED STANDARDS FOR
ESTABLISHING TRACEABILITY
10. REFERENCE METHOD
11. REFERENCES
12. DATA FORMS
Number
Documentation of Pages
3.6
3.6
3.6.1
2
8
13
3.6.2
3.6.3
3.6.4
3.6.5
3.6.6
3.6.7
3.6.8
3.6.9
3.6.10
3.6.11
3.6.12
7
9
11
14
6
2
8
1
3
2
16
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 2 of 11
SUMMARY
A gas sample is extracted from the sampling point in the
stack. The sample is collected in an evacuated 2-H round bottom
borosilicate flask containing 25 ml of dilute sulfuric acid-
hydrogen peroxide absorbing solution. The nitrogen oxides,
except nitrous oxide, are measured colorimetrically using the
phenoldisulfonic acid (PDS) method for analysis.
If the gas being sampled contains insufficient oxygen for
the conversion of NO to N02 , then oxygen should be introduced
into the flask to permit this conversion. Oxygen may be intro-
duced into the flask by one of three methods: (1) Before
evacuating the sampling flask, flush with pure cylinder oxygen,
and then evacuate flask to 75 mm (3.0 in.) Hg absolute pressure
or less; or (2) inject oxygen into the flask after sampling; or
(3) terminate sampling with a minimum of 50 mm (2.0 in.) Hg
vacuum remaining in the flask, record this final pressure, and
then open the flask to the atmosphere until the flask pressure is
almost equal to atmospheric pressure. The chemical reactions
that occur during sampling absorption are:
NO sample: NO + H2O? -> NO2 + H20 -> 2NO2 + H2O2 •* 2HNO3
NO2 sample: 2NO2 + H2O2 -* 2HNO3
NO sample: (2NO) gaseous + O2 -* 2NO2 + H2O2 -> 2HNO3
Method 7 is applicable to the measurement of nitrogen oxides
emitted from stationary sources. The range of the method has
been determined to be 2 to 400 mg NO , expressed as N09 per dry
J\ £*
standard cubic meter without having to dilute the sample.
The precision of the method (as measured by repeatability
and reproducibility of the measurements) in the collaborative
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 3 of 11
studies varies from 6.6% to 15% (repeatability) and from 9.5% to
19% (reproducibility). See Appendixes A and K, Volume I of this
Handbook for definition and discussion of these measures of data
quality.
The method description given herein draws heavily on the
o
corresponding guideline document, the collaborative test re-
ports,3'4'5 and the Reference Method from the 40 CFR 60, July 1,
1978. Section 3.6.10 contains a complete copy of the Reference
Method. Blank data forms are provided in Section 3.6.12 for
the convenience of the Handbook user.
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 4 of 11
METHOD HIGHLIGHTS
Section 3.6 provides the procedures for collecting and
analyzing a grab sample of oxides of nitrogen (NO ). The results
A
are expressed as concentrations of nitrogen dioxide (NO-). The
applicable regulation should be consulted to determine any addi-
tional requirements (i.e., velocity traverse or O_ grab sample).
Method 7 requires less experience and manpower to collect the
sample than most of the other reference methods. However, based
on the wide variations in the collaborative results of analyses
on aqueous ammonia nitrate audit samples, it is imperative that
the analyst be familiar with the analytical techniques described
in the Reference Method in Section 3.6.10. A larger number of
samples (normally 12) is also required to be taken because the
method collects a grab sample not an integrated sample over an
extended time.
The four blank data forms at the end of this section may be
removed from the Handbook and used in the pretest, test, and
posttest operations. Each form has a subtitle (e.g., Method 7,
Figure 3.1) for helping the user find a similiar filled-in form
in the method description (Section 3.6.3). On the blank and
filled-in forms, the items/parameters that can cause the most
significant errors are starred.
1. Procurement of Equipment
Section 3.6.1 (Procurement of Apparatus and Supplies) gives
the specifications, criteria, and design features of the equip-
ment and material required to perform Method 7 tests with the
evacuated flask sampling train. This section is designed to
guide the tester in the procurement and initial check of equip-
ment and supplies. The activity matrix (Table 1.1) at the end of
Section 3.6.1 can be used as a quick reference and is a summary
of the corresponding written description.
2. Pretest Preparations
Section 3.6.2 (Calibration of Apparatus) provides a step-by-
step description of the calibration procedures along with the
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 5 of 11
required accuracy for each component. The optimum wavelength
should be determined every 6 mo, and the calibration factor
should be determined each time the spectrophotometer is used to
analyze NO samples. The volume of each collection flask must be
X
determined with stopcock in place. This volume measurement is
required only on the initial calibration, provided the stopcock
is not changed. The calibration section may be removed along
with the corresponding sections from the other methods and made
into a separate quality assurance reference manual for use by
calibration personnel.
Section 3.6.3 (Presampling Operations) provides the tester
with a guide for equipment and supplies preparation for the field
test. The calibration data should be summarized on a pretest
checklist (Figure 3.1, Section 3.6.3) or similar form. A pretest
preparation form (Figure 3.2, Section 3.6.3) can be used as an
equipment checkout and packing list. The flasks may be charged
with the absorbing reagent in the base laboratory. The method of
packing and the use of the described packing containers should
help protect the equipment, but neither is required by the
Reference Method.
3. On-Site Measurements
Section 3.6.4 (On-Site Measurements) contains step-by-step
procedures for the sample collection and for the sample recovery.
The on-site checklist (Figure 4.3, Section 3.6.4) provides the
tester with a quick method of checking the requirements. When
high negative stack pressures are present, extra care should be
taken to purge the leak-tested sample system and to be sure the
flask is <_75 mm (3 in. ) Hg absolute pressure prior to testing.
Also the 16-h sample residence time in the flask must be observed.
4. Posttest Operations
Section 3.6.5 (Postsampling Operations) gives the posttest
equipment procedures and a step-by-step analytical procedure for
determination of NO , expressed as NO-. Posttest calibration is
X £+
not required on any of the sampling equipment. The posttest
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 6 of 11
operation forms (Figure 5.3, Section 3.6.5) provide some key
parameters to be checked by the tester and laboratory personnel.
The step-by-step analytical procedure description can be removed
and made into a separate quality assurance analytical reference
manual for the laboratory personnel. Analysis of a control
sample is required prior to the analysis of the field samples.
This analysis of an independently prepared known standard will
provide the laboratory with quality control checks on the
accuracy and precision of the analytical techniques. Strict
adherence to the Reference Method analytical procedures must be
observed; for example in the evaporation of the sample, the
substitution of a hot plate for the steam bath is not acceptable.
Section 3.6.6 (Calculations) provides the tester with the
required equations, nomenclature, and significant digits. It is
suggested that a calculator be used if available to reduce the
chance of calculation error.
Section 3.6.7 (Maintenance) provides the tester with a guide
for a maintenance program. This program is not required, but
should reduce equipment malfunctions.
5. Auditing Procedure
Section 3.6.8 (Auditing Procedure) provides a description
of necessary activities for conducting performance and system
audits. The performance audit of the analytical phase can be
conducted using an aqueous ammonium nitrate solution. Perform-
ance audits for the analytical phase and the data processing are
described in Section 3.6.8. A checklist for a systems audit is
also included in this section.
Section 3.6.9 (Recommended Standards for Establishing Trace-
ability) provides the primary standards to which the data should
be traceable. The analysis of NO is traceable to primary stand-
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 7 of 11
Section 3.6.11 (References) is a listing of the references
that were used in this method description.
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 8 of 11
PRETEST SAMPLING CHECKS
(Method 7, Figure 3.1)
Date Calibrated by
Flask Volume
Flask volumes measured with valves? yes no
Volume measured within ±10 ml of actual volume? yes no
Temperature Gauge
Was a pretest temperature correction used? yes no
If yes, temperature correction (within +1°C (2°F) of
reference values for calibration and within ±2°C (4°F) of
reference values for calibration check)
Vacuum Gauge
Was gauge calibrated against a U-tube mercury manometer
(If it was a mechanical gauge)? yes no not
applicable?
Barometer
Was the pretest field barometer reading within +2.5 mm (0.1 in.)
Hg of the mercury-in-glass barometer? yes no
Most significant items/parameters to be checked.
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 9 of 11
PRETEST PREPARATIONS
(Method 7, Figure 3.2)
Apparatus check
Probe
Glass liner
clean
Heated properly
Leak checked
Collection Flask
Clean
Leak checked
Temperature
gauge
Evacuation System
Leak- free pumps
Manifold and
tubing
U-tube manometer
Barometer
Reagents
Distilled water
Absorbing solu-
tion*
Sodium hydrox-
ide, IN
pH paper
Sample Recovery
Dropper or
burette
Sample bottles
Pipette, 25 ml
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Loaded
and packed
Yes
No
* Most significant items/parameters to be checked.
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 10 of 11
ON-SITE MEASUREMENTS
(Method 7, Figure 4.3)
Sampling
Volume of 25 ml of absorbing solution placed in flask?
Flask valve stopper in purge position?
Sampling train properly assembled?
Leak free?* Stopcock grease used?
Type?
Flask evacuated to 75 mm (3 in.) Hg pressure?
Leakage from manometer observation?*
(e.g., maximum change in manometer of <_IQ mm (0.4 in.)
Hg/min)
Initial pressure of flask recorded?*
Initial temperature of flask recorded?
Probe purged before sampling?
Sample collected properly?*
Flask shaken for 5 min after collection and disassembly
from train?*
Oxygen introduced to flask? Method used?
Samples properly labeled and sealed and stored for shipment?
Sample Recovery
Samples allowed to remain in flasks for minimum of 16 h?*
Final flask temperature and pressure recorded?*
Sample transferred to leak-free polyethylene bottle?
Flask rinsed twice with 5-ml portions of distilled water
and rinse added to bottle containing sample?
pH adjusted to between 9 and 12?*
* Most significant items/parameters to be checked.
-------
Section No. 3.6
Revision No. 0
Date May 1, 1979
Page 11 of 11
POSTTEST OPERATIONS
(Method 7, Figure 5.3)
Reagents
Phenoldisulfonic acid stored in dark stoppered bottle?
Sulfuric acid, concentrated, 95% minimum assay reagent
grade?
Ammonium hydroxide, concentrated reagent grade?
Sample Preparation
Has liquid level noticeably changed?*
Original volume Corrected volume
Analysis
Spectrophotometer calibrated?*
Setting for maximum absorbance of standard nm
Control sample prepared?*
Any solids in sample removed through Whatman No. 41 filter
paper?
Absorbance measured at optimum wavelength used for the stand-
ards, using the blank solution as a zero reference?
All analytical data recorded on checklist and laboratory form?
* Most significant items/parameters to be checked.
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 1 of 13
1.0 PROCUREMENT OF APPARATUS AND SUPPLIES
The activity matrix for apparatus is given in Table 1.1 at
the end of this section. The required apparatus for a Method 7
sampling train is shown in Figure 1.1. Additional specifica-
tions, criteria, and/or design features as applicable are given
here to aid in the selection of equipment to ensure the collec-
tion of good quality data. All new items of equipment are to be
inspected visually for identification and damage before accept-
ance. Also, if applicable, new equipment is to be calibrated
according to Section 3.6.2, as part of the acceptance check.
During the procurement of equipment and supplies, it is
suggested that a procurement log be used to record the descrip-
tive title of the equipment, identification number (if applica-
ble), and the results of acceptance checks. An example of a
procurement log is shown in Figure 1.2. A blank copy of this
form is given in Section 3.6.12 for the Handbook user. Calibra-
tion data generated in the acceptance check are to be recorded in
the calibration log book. Alternative grab sampling systems or
equipment capable of measuring sample volume to within +2% and
collecting a sufficient sample volume to allow analytical re-
peatability to within +5% is acceptable, subject to approval.
The following equipment is specified in the Reference Method.
1.1 Sampling
1.1.1 Sampling Probe - The sampling probe should be made of
glass (borosilicate) encased in a stainless steel sheath and
equipped with a heating system capable of preventing water con-
densation and with a filter (either in-stack or heated out of
stack) to remove particulate matter. A plug of glass wool in the
sample probe is satisfactory for the in-stack filter. Stainless
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 2 of 13
10
14
+1
•H
E
<0
10
.*
W
-------
Item description
Sptc4 rooWtoinetef
Qty.
1
Purchase
order
number
IOVS"
Vendor
G>CMA-?,M lo»*b
Date
Ord.
*lnhl
Rec.
>)if/77
Cost
ifrS-00
Dispo-
sition
ok.
Comments
rt
H-
O
Figure 1.2. Example of a procurement log.
*Tj C3 S*0 C/3
D) 0) (D (D
iQ rt<3 O
fl> (D H
CO
u> S H
0) O 3
O K 3
H, Z
M2 O
I-1- O •
u> •
I-1 (jo
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 4 of 13
p
steel or Teflon tubing may also be used for the probe liner.
Heating is not required if the probe remains dry during the
purging period, but it is recommended that the probe have pro-
vision for heating. The in-stack end of the probe should have an
expanded diameter for about the first 4 cm to be used for the
glass-wool filter. A probe of approximately 1.2 m (4 ft) total
length is usually sufficient for sampling. However, the probe
tip can be no closer than 1 m (3.28 ft) from the inner wall of
stacks >2 m in diameter. When stack gas temperatures exceed
480°C (900°F), a probe fabricated from quartz (Vycor) should be
used along with quartz wool for filter material. The main crite-
rion in selecting a probe material is that it be nonreactive with
the gas constituents and therefore not introduce a bias into the
analysis.
A new probe should be checked visually for specifications
(i.e., the length and composition ordered). It should be checked
for cracks, breaks, and leaks on a sampling train. The probe
heating system should be checked as follows:
1. Connect the probe (without filter) to the inlet of the
pump.
2. Electrically connect and turn on the probe heater for 2
or 3 min. If functioning properly, it will become warm to the
touch.
3. Start the pump and adjust for a flow rate of about
1.0 A/min.
4. Check the probe. It should remain warm to the touch.
The heater must be capable of maintaining the exit air tempera-
ture at a minimum of 100°C (212°F) under the above conditions.
If it cannot, the probe should be replaced. Any probe not
satisfying the acceptance check should be repaired if possible,
or returned to the supplier.
1.1.2 Collection Flask - A 2-8, borosilicate round bottom flask,
with a short neck and 24/40 standard taper opening is required.
Ti
Trade name.
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 5 of 13
The collection flask should be protected from implosion or break-
age by using (1) tape, (2) a commercial unit encased in foam, or
(3) a fabricated closed-cell foam enclosure. Once the flask has
been connected to the flask valve, both should be marked as a set
and neither should be used at random with other flasks as this
will cause volume fluctuations with the sample.
1.1.3 Flask Valve - A T-bore stopcock is connected to a 24/40
standard taper joint. Bores should be numbered but not switched
to prevent leakage problems. The T-bore should be marked to
avoid turning the stopcock in the wrong direction when sampling.
The flask valve should be marked to identify its matched flask.
1.1.4 Temperature Gauge - A temperature gauge should consist of
a dial-type thermometer, or equivalent, capable of measuring 1°C
(2°F) intervals from -5° to 50°C (25° to 125°F). Dial-type
thermometers are easily damaged, so each new thermometer must be
checked visually for damage, such as a dented or bent stem. Each
thermometer should read within +1°C (2°F) of the true value when
checked in an ice water bath and at room temperature against a
mercury-in-glass thermometer that conforms to ASTM E-l No. 63C or
63F. Damaged thermometers that cannot be calibrated must be
replaced.
1.1.5 Vacuum Line - The vacuum line should be of a nonreactive,
thick wall type and should be leak checked at 75 mm (3 in.) Hg of
absolute pressure while connected to the sampling train. The
tubing should be flexible and approximately 1 to 1.6 m (3 to
5 ft) in total length. If the tubing is found to leak, it
should be rejected.
1.1.6 Vacuum Gauge - A U-tube manometer should be about 1 m
(36 in.) in length with 1-mm (0.1 in.) divisions, or the equiva-
lent, capable of measuring pressure to within +2.5 mm (0.1 in.)
Hg. If a U-tube manometer is used, no calibration is required.
Upon receipt, the user should verify by reading the instructions
that the manometer was designed to use mercury. If the manometer
is acceptable, it must then be leak checked. When a mechanical
vacuum gauge is used, it must be calibrated upon receipt by the
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 6 of 13
procedures described in Section 3.6.2. If it fails to calibrate,
it should be replaced.
The vacuum gauge should be leak checked as follows: (1)
connect vacuum line to the manometer at the end that connects to
the sampling train, as shown in Figure 1.1 (2) pull a vacuum of
75 mm (3 in.) Hg or less, (3) shut off the valve between the
manometer and the pump, (4) shut off the pump, (5) observe the
vacuum registered on the manometer for any deviation over a 1-min
period. If there is no deviation, the vacuum gauge is accept-
able; if there is a deviation, the gauge is unacceptable and
should be corrected or replaced.
1.1.7 Vacuum Pump - The vacuum pump should be capable of produc-
ing a vacuum of 75 mm (3 in.) Hg or less. The pump must be leak
free when running and when pulling a vacuum (inlet plugged) of 75
mm (3 in.) Hg. Two types of vacuum pumps are commonly used—a
modified sliding fiber vane pump or a diaphragm pump. For safety
reasons, the pump should be equipped with a three-wire electrical
cord. To check the pump for leaks, install a vacuum gauge in the
pump inlet line. Plug the inlet line and run the pump until the
vacuum gauge reads 75 mm (3 in. ) Hg of vacuum. The vacuum read-
ing should remain stable for 30 seconds.
1-1.8 Squeeze Bulb - A one-way, hard rubber bulb with about a
50-ml capacity is needed to purge the sampling system.
1.1.9 Volumetric Pipette - A 25-ml volumetric glass pipette
(Class A) is needed for addition of reagent to the collection
flask.
1.1.10 Stopcock Grease - An inert, high-vacuum, high-temperature
chlorofluorocarbon grease should be used. Halocarbon 25 - 55 has
been found to be effective.
1.1.11 Barometer - Mercury, aneroid, or other barometers capable
of measuring atmospheric pressure to within 2.5 mm (0.1 in.) Hg
are required. In many cases, the barometric reading may be
obtained from a nearby National Weather Service Station, in which
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 7 of 13
case the station value (which is the absolute barometric pres-
sure) should be requested and an adjustment for elevation differ-
ences between the weather station and the sampling point should
be applied at a rate of -2.5 mm Hg/30 m (0.1 in. Hg/100 ft)
of elevation increase, or vice versa for elevation decrease.
Upon receipt, check the barometer against a mercury-in-glass
barometer. Replace it if it cannot be calibrated to read cor-
rectly.
1.2 Sample Recovery
1.2.1 Graduated Cylinder - A 50-ml glass or polyethylene gradu-
ated cylinder with 1-ml divisions is required.
1.2.2 Storage Bottles - A minimum of 12 leak-free polyethylene
bottles for recovery of samples are needed. The bottles should
be packed in a cushioned, locked container (box or footlocker)
for shipment. The leak-free seal can be initially checked by
putting water in each, sealing, and then shaking the container
upside down.
1.2.3 Wash Bottle - Glass or polyethylene wash bottles are
needed for rinsing (transferral) of the sample solution to stor-
age bottles.
1.2.4 Stirring Rod - A stirring rod (glass or polyethylene) is
required to check the pH of the absorbing reagent.
1.2.5 pH Indicating Paper - pH paper with the range of 7 - 14 is
required to test the alkalinity of the samples.
1.3 Analysis
1.3.1 Pipettes - Several volumetric pipettes are required (two 1
ml, two 2 ml, one 3 ml, one 4 ml, two 10 ml, and one 25 ml); one
transfer pipette (10 ml with 0.1-ml divisions) is required.
1.3.2 Volumetric Flasks - One 100-ml volumetric flask, is needed
for each sample and each standard. Two 1000-ml volumetric
flasks are required for the blank and the standard nitrate.
Additional volumetric flasks (50 ml) are required for aliquots
for analysis and for dilution of samples that fall outside the
calibration range (absorbance >400-(jg standard).
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 8 of 13
1.3.3 Evaporating Dishes - Several 175- to 250-ml capacity
porcelain dishes with lip for pouring are needed, one for each
sample and one for each standard. The Coors No. 45006 (shallow,
195 ml) has been found to be satisfactory. Alternatively,
polymethyl-pentene beakers (Nalge No. 1203, 150 ml) or glass
beakers (150 ml) may be used. When glass beakers are used,
etching of the beakers may cause solid matter to be present in
the analytical step; the solids should be removed by filtration.
For this reason, glass beakers should be used only if necessary.
1-3.4 Steam Bath - A steam bath is required to evaporate the
absorbing solution. Low-temperature ovens or thermostatically
controlled hot plates kept below 70°C (160°F) are acceptable
alternatives.
1.3.5 Polyethylene Policeman - One stirring rod (polyethylene
policeman) is required for each sample and standard. A glass
stirring rod is not recommended.
1.3.6 Graduated Cylinder - A 100-ml graduated glass cylinder
(Class A) with 1-ml divisions is required for additions of dis-
tilled water.
1.3.7 Spectrophotometer - A Spectrophotometer capable of measur-
ing the absorption at 410 nm (or the maximum peak), a set of
neutral density filters, and a filter for wavelength calibration
are required.
1.3.8 pH Paper - The paper should cover the pH range of 7 - 14
with intervals of 1-pH unit.
1.3.9 Analytical Balance - One analytical balance that weighs to
0.1 mg and a set of Class-S calibration weights to check the
accuracy of the balance (+0.3 mg) upon receipt are needed. The
balance should be serviced by or returned to the manufacturer if
agreement cannot be met.
1.3.10 Dropping Pipette or Dropper - A dropping pipette, or a
dropper, or its equivalent for addition of ammonium hydroxide to
the evaporation dish is needed.
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 9 of 13
1.4 Reagents
Unless otherwise indicated, it is intended that all reagents
conform to the specifications established by the Committee on
Analytical Reagents of the American Chemical Society (ACS), where
such specifications are available; otherwise, use the best avail-
able grade.
1.4.1 Sampling - To prepare the absorbing solution, cautiously
add 2.8 ml of concentrated H2S04 to 1 8, of deionized distilled
water and mix well. Add 6 ml of 3% hydrogen peroxide, freshly
prepared from 30% hydrogen peroxide (ACS reagent grade) solution.
The absorbing solution must be used within 1 week of its prepara-
tion and if possible within 24 h. Store in a dark-colored bot-
tle. Do not expose to extreme heat or direct sunlight. Note:
The 30% hydrogen should be stored in the refrigerator.
1.4.2 Sample Recovery - Two reagents are required for sample
recovery.
Sodium hydroxide (IN) - Dissolve 40 g of NaOH ACS reagent
grade in deionized distilled water and dilute to 1 £.
Water - Use deionized distilled to conform to ASTM speci-
fication D1193-74, Type 3. At the option of the analyst, the
KMnC- test for oxidizable organic matter may be omitted whenever
high concentrations of organic matter are not expected to be
present.
1.4.3 Analysis - For the analysis, the following reagents are
required.
Fuming sulfuric acid - Use 15% to 18% by weight of free sul-
fur trioxide, ACS reagent grade. Note: Handle with caution.
Phenol - Use white solid, ACS reagent grade.
Sulfuric acid - Use concentrated, 95% minimum assay, ACS
reagent grade. Note; Handle with caution.
Potassium nitrate - Dry at 105° to 110°C (220° to 230°F) for
a minimum of 2 h just prior to preparation of standard solution,
ACS reagent grade.
Standard KNO., solution - Dissolve exactly 2.198 g of dried
potassium nitrate (KNO3) in deionized distilled water and dilute
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 10 of 13
to 1 H with deionized distilled water. One ml of the working
standard solution is equivalent to 100 |jg of nitrogen dioxide
(N02).
Water - Deionized distilled as in Subsection 1.4.2.
Phenoldisulfonic acid solution - Dissolve 25 g of pure white
phenol in 150 ml of concentrated sulfuric acid on a steam bath.
Cool; add 75 ml of fuming sulfuric acid; and heat at 100 °C
(212°F) for 2 h. Store in a dark, stoppered bottle. Alterna-
tively, this solution may be purchased prepared, if it meets the
American Public Health Association specification for nitrate-
nitrogen in water.
Ammonium hydroxide - Use concentrated, ACS reagent grade.
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 11 of 13
Table 1.1.
ACTIVITY MATRIX FOR PROCUREMENT OF APPARATUS
AND SUPPLIES
Apparatus/
reagents
Probe
Collection
flask
Acceptance limits
Borosilicate glass tub-
ing, stainless steel or
Teflon capable of re-
moving particulate and
preventing moisture
condensation
Two-liter borosilcate
glass round bottom,
short neck w/24/40
standard taper opening
Frequency and method
of measurement
Upon receipt, visual-
ly check for cracks
or flaws and heating
capability
Upon receipt visual-
ly check and leak
check
Action if
requirements
are not met
Return to
supplier and
note in pro-
curement log
As above
Flask valve
Borosilicate glass T-
bore stopcock w/24/40
standard taper male
joint (joint connection
to be made by glass-
blower)
Visually check upon
receipt
As above
Temperature
gauge
Dial-type, capable of
measuring from -5° to
+50°C within 1°C
Visually check upon
receipt, and compare
against Hg-in-glass
thermometer
As above
Vacuum line
tubing
Capable of withstanding
75 mm absolute pres-
sure
Upon receipt visual-
ly check and leak
check
As above
Vacuum gauge
U-tube manometer, open
end, 1 m with 1-mm div-
isions
Visually check upon
receipt
As above
Vacuum pump
Pump capable of pulling
vacuum of 75 mm Hg or
less
Upon receipt check
with suitable pres-
sure gauge
As above
Squeeze bulb
Rubber, one-way
Visually check upon
receipt
As above
Volumetric
pipettes
1-, 2-, 3-, 4-, 10-,
25-ml glass (Class A)
As above
As above
(continued)
-------
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 12 of 13
Table 1.1 (continued)
Apparatus/
reagents
Stopcock grease
Barometer (or
consult local
weather sta-
tion
Storage bottle
Wash bottle
Glass stirring
rod
pH paper
Volumetric
flasks
Evaporating
dishes
Steam bath
Polyethylene
policeman
Graduated cyl-
inders
Acceptance limits
High vacuum, high temp-
perature chlorof luoro-
carbon grease
Capable of reading at-
mospheric pressure to
+2.5 mm Hg
Polyethylene, 100-ml,
or greater capacity,
screw cap
Polyethylene or glass
As above
Sensitive in pH range
7-14
50-, 100- , 1000-ml
glass (Class A)
Porcelain evaporating
dishes or polymethyl-
pentene beakers
Evaporate the sample
solution at a low
controlled temperature
Polyethylene stirring
rod
50, 100 ml (Class A)
with 1-ml divisions
Frequency and method
of measurement
As above
Visually check; cali-
brate against
mercury-in-glass
barometer
Visually check upon
receipt
Visually check label
upon receipt
As above
As above
As above
As above
As above
As above
As above
Action if
requirements
are not met
As above
As above
Return to
supplier and
note in pro-
curement
log
As above
As above
Return to
supplier
As above
Discard when
the bottoms
become etched
Return to
supplier
As above
As above
(continued)
-------
T~
Section No. 3.6.1
Revision No. 0
Date May 1, 1979
Page 13 of 13
Table 1.1 (continued)
Apparatus/
reagents
Spectrophotome-
ter
Dropping
pipette or
dropper
Sulfuric acid
Hydrogen perox-
ide
Sodium hydrox-
ide
Sulfuric acid
Phenol
Potassium ni-
trate
Acceptance limits
Capable of measuring
absorbance at 410 run
(such as Bausch & Lomb
Spectronic 70)
Able to add reagents
dropwise
Concentrated, ACS rea-
gent grade
30% aqueous solution,
ACS reagent grade
ACS reagent grade pel-
lets
Fuming, 15-18% free
sulfur trioxide
White solid, ACS rea-
gent grade
ACS reagent grade
Frequency and method
of measurement
Upon receipt, either
check wavelength
with filters or en-
sure optimum wave-
length is between
400 and 415 nm
Visually check upon
receipt
Visually check upon
receipt; check speci-
fications
As above
Visually check upon
receipt; check speci-
fications
As above
As above
As above
Action if
requirements
are not met
Adjust, re-
calibrate as
per manu-
facturer* s
instructions ,
and note in
procurement
log
Return to
supplier
As above
As above
Return to
supplier
As above
As above
As above
-------
Section No. 3.6.2
Revision No. 0
Date May 1, 1979
Page 1 of 7
2.0 CALIBRATION OF APPARATUS
Calibration of the apparatus is one of the most important
functions in maintaining data quality. The detailed calibration
procedures included in this section are designed for the equip-
ment specified by Method 7 and described in the previous section.
Table 2.1 at the end of this section summarizes the quality
assurance functions for calibration. All calibrations should be
recorded on standardized record forms and retained in a calibra-
tion log book.
2.1 Collection Flask
Assemble the clean flasks and valves and fill with water
(room temperature) to the stopcock. Measure the volume to +10 ml
by transferring the water to a 500-ml glass (Class A) graduated
cylinder. Do duplicate volume determinations, and use the mean
value. Number and record the volume mean value on the flask or
foam encasement and in the laboratory log book. This volume
measurement is required only on the initial calibration if the
flask valves are not switched.
2.2 Spectrophotometer
2.2.1 Determination of Optimum Wavelength - Calibrate the wave-
length scale of the spectrophotometer every 6 mo. The calibra-
tion may be accomplished by using an energy source with an in-
tense line emission such as a mercury lamp, or by using a series
of glass filters spanning the measuring range of the spectropho-
tometer. Calibration materials are available commercially and
from the National Bureau of Standards. Specific details on the
uses of such materials should be supplied by the vendor.
In general, when using glass filters, each filter is in-
serted into the light path and the wavelength dial is rotated
until the instrument response is greatest. Then the reading on
the dial is noted and can be compared with the true value. When
using an alternate light source, the instrument lamp is replaced
-------
Section No. 3.6.2
Revision No. 0
Date May 1, 1979
Page 2 of 7
by the alternate lamp. The wavelength dial is rotated, and the
dial reading is noted at each peak for comparison with the true
value. The wavelength scale of the spectrophotometer must read
correctly within +5 nm of the true wavelength at all calibration
points; otherwise, the spectrophotometer should be repaired and
recalibrated. Once the wavelength scale of the spectrophotometer
is properly calibrated, use 410 nm as the optimum wavelength for
the measurement of the absorbance of the standards and samples.
Alternatively, a scanning procedure may be employed to
determine the optimum wavelength. If the instrument is a double-
beam spectrophotometer, scan the spectrum between 400 and 415 nm
using a 200 ng NO2 standard solution in the sample cell and a
blank solution in the reference cell. If a peak does not occur,
the spectrophotometer is probably malfunctioning and should be
repaired. If a peak is obtained within the 400- to 415-nm range,
the wavelength at which this peak occurs should be the optimum
wavelength for the measurement of absorbance of both the stand-
ards and the samples. For a single-beam spectrophotometer,
follow the scanning procedure described, but scan the blank and
the standard solutions separately. The optimum wavelength should
be the one at which the maximum difference in absorbance between
the standard and the blank occurs. The data obtained for this
alternative optimum wavelength determination should be recorded
on the data form as shown in Figure 2.1.
2.2.2 Determination of Calibration Factor - K - The calibration
" " C
factor (KC) must be determined in the verification of the analyt-
ical technique and solution preparation prior to sample analysis
with the control sample. After the analytical technique and
solutions have been verified as to their accuracy and precision,
a new calibration factor should be determined simultaneously with
the field sample analysis. Since a detailed discussion of this
procedure is included in the sample analysis Section 3.6.5, it is
omitted here.
2.3 Barometer
The field barometer should be adjusted initially and before
each test series to agree within 2.5 mm (0.1 in.) Hg of the
-------
Section No. 3.6.2
Revision No. 0
Date May 1, 1979
Page 3 of 7
Spectrophotometer number
Calibrated by & •
Date
Reviewed by
Spectrophotometer
setting, run
399
400
401
402
403
404
405
406
407
408
409
410
411
412
413
414
415
416
Absorbance
of standard
ODa
.955
. 93V-
. 92.0
.
.873
. 8Y4
. 8 3o
. 8«
.8;/
'. 765"
.777
Absorbance
of blank
./85
.1 51
. i *L
. i 1 (o
.OQ7
• Ofck
. 080
. OTi
. Ob(p
• os-b
.057
.ova
.03k
O2>J
'.0X8
.0/5-
.009
.000
Actual
absorbance of
ODC
.lib
. 777
• 784
. 7&8
. 8/O
. 8/3
. gz./
. 8/k
. B^/
. T?'/
. 69Z
.783
. 13 I
. 11k
. "777
Absorbance of the 200 pg N0? standard in a single beam
spectrophotometer.
Absorbance of the blank in a single-beam spectrophotometer.
£•
For a single-beam spectrophotometer — absorbance of the standard
minus absorbance of the blank. For a double beam spectrophoto-
meter — absorbance of the 200 pg NO,, standard with the blank
in the reference cell.
Spectrophotometer setting for maximum actual absorbance of
standard Vo run.
If the maximum actual absorbance occurs at a spectrophotometer
setting of O99 or >_416 nm, the spectrophotometer must be
repaired or recalibrated.
Figure 2.1. Optimun wavelength determination data form.
-------
Section No. 3.6.2
Revision No. 0
Date May 1, 1979
Page 4 of 7
mercury-in-glass barometer or with the pressure value reported
from a nearby National Weather Service Station and corrected
for elevation. The correction for elevation difference between
the station and sampling point should be applied at a rate of
-2.5 mm Hg/30 m (-0.1 in Hg/100 ft) elevation increase, or vice
versa for elevation decrease.
2.4 Thermometer
The thermometers used to measure the temperature of the
sample flask should be initially compared with a mercury-in-glass
thermometer that meets ASTM E-l No. 63C or 63F specifications as
follows:
1. Place both the mercury-in-glass and the dial-type or an
equivalent thermometer in an ice bath. Compare readings after
the bath stabilizes.
2. Allow both thermometers to come to room temperature.
Compare readings after both stabilize.
3. The dial-type or equivalent thermometer is acceptable
if values agree within 1°C (2°F) at both room and ice bath temp-
eratures. If the difference is greater than +1°C (2°F), the
thermometer should be either adjusted and recalibrated until the
above criteria are met, or replaced.
4. Prior to each field trip the temperatures should then
be compared at room temperature with the thermometer in the
equipment. If the value is not within +2°C (4°F) of the mercury-
in-glass thermometer value, the meter thermometer should be
replaced or recalibrated.
2.5 Vacuum Gauge
When a mercury U-tube manometer is used, no calibration is
required. The U-tube manometer should be checked initially to
ensure that it is leak free.
When a mechanical gauge is used, it must be calibrated
against a mercury U-tube manometer before the field test unless
otherwise specified by the administrator. The mechanical gauge
should be calibrated in the following manner:
-------
Section No. 3.6.2
Revision No. 0
Date May 1, 1979
Page 5 of 7
I. Connect the mechanical gauge and the U-tube manometer
in parallel with the vacuum pump. This can be accomplished with
a T-connection. One line should be placed on the vacuum side of
the pump, and the other two lines should be placed on the vacuum
side of the gauge and manometer.
2. Turn the pump on, and pull a vacuum of about 25 to 50
mm (1 to 2 in.) Hg. Shut off main pump valve and then shut off
pump.
3. Observe the U-tube manometer to be sure that the system
is leak free. Any variation >10 mm (0.4 in.) Hg over a 1-min
period is not acceptable. The manometer and gauge readings must
agree within +2.5 mm (0.1 in.) Hg, or the gauge should be re-
paired or replaced.
4. Turn the pump on, and pull the maximum vacuum for which
the pump is capable (must be within 75 mm (3 in.) Hg of absolute
pressure). Shut off the main valve, and then the pump.
5. Be sure that the system is leak free and again compare
readings.
6. The gauge must agree within 2.5 mm (0.1 in.) Hg at both
vacuums, or the gauge is not acceptable.
2.6 Analytical Balance
The analytical balance should always be zeroed and cali-
brated against a standard Class-S weight(s) just before the
potassium nitrate (KNO») is weighed for the formulation of the
working standard. This calibration should be done in the fol-
lowing manner:
1. Zero the balance.
2. Place a 5-g and then a 10-g standard weight on the
balance.
3. Be sure the balance readings of the standardized weights
agree within +2 mg of the standard weights.
4. Enter the data on the calibration form, Figure 2.2.
5. The weight of the weighing boat and the potassium
nitrate should be <10 g; if not, heavier standard weights should
be used to calibrate the balance.
-------
Section No. 3.6.2
Revision No. 0
Date May 1, 1979
Page 6 of 7
Balance name
Classification of standard weights
Number
"s"
Date
6/n/i*
0.5000 g
0. *00*f
1.0000 g
o.w^r
10.000 g
/O.OOO7.
50.0000 g
^O.OOOG
100.0000 g
/oo. 0004
Analyst
&JL3
Figure 2.2. Analytical balance calibration form.
-------
Section No. 3.6.2
Revision No. 0
Date May 1, 1979
Page 7 of 7
Table 2.1. ACTIVITY MATRIX FOR CALIBRATION OF EQUIPMENT
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Collection
flask
Measure volume within
+10 ml
On receipt, measure
with graduated cyl-
inder
Recalibrate
Spectropho-
tometer
1. ^Calibrate wave-
length scale
2. ^Determine optimum
wavelength within 399
to 416 nm
1. Upon receipt and
every 6 mo, use glass
filters or light
source
2. Upon receipt and
every 6 mo scan be-
tween 400 and 415 nm
with 200 mg NO stand-
ard solution
1. Return
to manufac-
turer for
repair
2. As above
Barometer
Reading agrees within
+2.5 mm (0.1 in.) Hg
of mercury-in-glass
barometer
Upon receipt and be-
fore each field test
Repair or
return
Thermometer
Reading agrees within
+1°C (2°F) of mercury-
in-glass thermometer
As above
As above
Vacuum gauge
(mechanical
only)
Reading agrees within
+2.5 mm (0.1 in.) Hg
of mercury U-tube man-
ometer
As above
As above
Analytical bal-
ance
Weight within +2 mg of
standard weights (Class
S)
Use standard weight
before preparation
of working solution
Repair or
return to
manufacturer
The tester may opt to perform either step 1 or 2, both are not
required.
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 1 of 9
3.0 PRESAMPLING OPERATIONS
The quality assurance functions for presampling operations
are summarized in Table 3.1 at the end of this section. See
Section 3.0.1, Planning the Test Program, of this Handbook for
details on preliminary site visits.
3.1 Apparatus Check and Calibration
Previously used equipment should be visually checked for
damage and/or excessive wear before each field test. Items
should be repaired or replaced (as applicable) if judged to be
unsuitable for use. A pretest checklist (Figure 3.1) summarizes
equipment calibration. The pretest operations form (Figure 3.2)
can be used as an equipment check and packing list. The com-
pleted form should be dated, signed by the field crew supervisor,
and filed in the operational log book. The replacement of worn
or damaged items of equipment should be initiated. Procedures
for performing the checks are given herein; a check is placed in
the proper row and column as the check/operation is completed.
Each team will have to construct its own checklist according to
the type of sampling train and equipment it uses.
3.1.1 Probe (Filter) - Clean the probe internally by brushing
first using tap water, then with distilled deionized water, next
with acetone, and finally allow it to dry in the air. In extreme
cases, the glass liner can be cleaned with stronger reagents.
Note: Do not use nitric acid to clean the probe unless a thor-
ough cleaning is performed to remove all the nitrates. In either
case, the object is to leave the glass liner chemically inert to
oxides of nitrogen. If the probe is equipped with a heating
system, check to see whether it is operating properly. The probe
should be sealed on the filter side and checked for leaks at an
absolute pressure of <380 mm (15 in.) Hg. The probe must be leak
free under these conditions. This leak check may be performed
following the leak check of the sample flask and using the same
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 2 of 9
Date X//^"/77 Calibrated by
/ "
Flask Volume
Flask volumes measured with valves? v yes
no
Volume measured within ±10 ml? yes no
Temperature Gauge
Was a pretest temperature correction used? yes I/no
If yes, temperature correction (within +1°C (2°F) of
reference values for calibration and within ±2°C (4°F) of
reference values for calibration check).
Vacuum Gauge
Was gauge calibrated against a U-tube mercury manometer
(If it was a mechanical gauge)? yes no \S not
applicable?
Barometer
Was the pretest field barometer reading within +2.5 mm (0.1 in.)
Hg of the mercury-in-glass barometer? \/ yes no
*
Most significant items/parameters to be checked.
Figure 3.1. Pretest sampling checks,
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 3 of 9
Apparatus check
Probe
Glass liner
clean
Heated properly
Leak checked
Collection Flask
Clean
Leak checked
Temperature
gauge
Evacuation System
Leak- free pumps
Manifold and
tubing
U-tube manometer
Barometer
Reagents
Distilled water
Absorbing solu-
tion*
Sodium hydrox-
ide, 1 N
pH paper
Samp_le_ Recovery
Dropper or
burette
Sample bottles
Pipette, 25 ml
Acceptable
Yes
V
*
•
s
s
^
^
yS
^s
t/
•
*f
^s
I/
V/
No
Quantity
required
3
rt
a
3
i
i .,-*«,
1 i;fcr
1 l/'te*'
1 pk<).
i4
>
Ready
Yes
•
^
^
I/
•
s
I/
-
v/
^
^
^
No
Loaded
and packed
Yes
^
^
-
^
i^
•
k
s
}/
f
/
V
No
* Most significant items/parameters to be checked.
Figure 3.2. Pretest preparations.
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 4 of 9
setup as described below in Subsection 3.1.2. The glass liner
should be sealed inside the metal sheath to prevent ambient air
from entering the duct.
3.1.2 Collection Flask, Flask Valve, and Evacuation System - The
collection flask and valve in contact with sample gas should be
cleaned with a strong detergent and hot water, and rinsed with
tap water and deionized distilled water. Periodically, the
glassware can be cleaned with a grease remover such as decahydro-
napthalene (C,_H,0), followed with acetone, and then with the
J.U J.O
cleaning agents named above. An alternate procedure is to use
dichromate cleaning solution. Do not use solutions containing
nitrogen. Vapor degreaser can be used to remove the stale vacuum
grease.
Stopcocks and joints should be lubricated with a chemically
inert lubricant. An inert hydrogen-free chlorofluorocarbon
lubricant can be used.
The evacuation system (Figure 1.1) is assembled, and a
minimum vacuum of 75 mm (3 in.) Hg absolute pressure is produced
in each flask with the flask valve in the "evacuation" position.
The vacuum should be held for at least 1 min with the pump valve
in the "vent" position without appreciable fluctuation (£10 mm
(0.4 in.) Hg); if this is not possible, check for leaks.
If the leak check of the probe is to be performed using the
same setup, the probe tip should be plugged with a rubber stop-
per. Immediately after the sample flask has been determined to
be leak free, turn the flask valve to the "purge" position. The
vacuum will initially drop. After the vacuum stabilizes there
should not be any appreciable fluctuation—that is £10 mm (0.4
in.) Hg over a 1-min period. If stabilization is not obtained,
check for leaks and correct.
3.2 Reagents
Unless otherwise indicated, it is intended that all reagents
conform to the specifications established by the Committee on
Analytical Reagents of the American Chemical Society (ACS), where
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 5 of 9
such specifications are available; otherwise, use the best avail-
able grade.
Chloride is an interference in the phenoldisulfonic acid
method because even rather low concentrations of chloride result
in nitrate losses. It is important that the chloride content be
reduced to a minimum, preferably below 10 mg/2.
3.2.1 Sampling - The absorbing reagent is prepared by adding 2.8
ml of concentrated sulfuric acid (H2S04) to 1 SL of deionized
distilled water. Mix well, and add 6 ml of 3% hydrogen peroxide
(H2O2). Prepare a fresh absorbing solution weekly, store in a
dark-colored pyrex container, and do not expose to extreme heat
or direct sunlight. If the reagent must be shipped to the field
site, it is advisable that the absorbing reagent be prepared
fresh on site.
3.2.2 Sample Recovery - A sodium hydroxide solution (NaOH) is
prepared by dissolving 40 g NaOH in distilled water and diluting
to 1 £. This solution can be transferred to a polyethylene
1000-ml (32-oz) jar for shipment. Deionized distilled water and
pH paper are required to test for basicity and for transferral of
samples.
3.2.3 Analysis - The following reagents are needed for analysis
and standardization:
Fuming sulfuric acid - 15% to 18% (by weight) free sulfur
trioxide (SO3).
Phenol - White solid ACS reagent grade.
Sulfuric acid - Concentrated reagent, 95% minimum assay,
ACS reagent grade.
Standard solution - Dissolve 2.198 g of dried potassium
nitrate (KN03) ACS reagent grade in distilled water, and dilute
to 1 £ in a volumetric flask. For the working standard solution,
pipette 10 ml of the resulting solution into a 100-ml volumetric
flask and dilute to the mark. Note: One ml of the working
standard solution is equivalent to 100 pg of nitrogen dioxide.
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 6 of 9
Water - Deionized distilled.
Phenoldisulfonic acid solution - Dissolve 25 g of pure white
phenol (no discoloration) in 150 ml of concentrated sulfuric acid
on a steam bath. Cool. Add 75 ml of fuming sulfuric acid, and
heat at 100°C (212°F) on a steam bath for 2 h. Store in a dark
stoppered bottle. This acid may also be purchased if it meets
the American Public Health Association specification for nitrate-
nitrogen in water.
3.3 Packing Equipment for Shipment
Equipment should be packed in rigid containers to protect it
against rough handling during shipping and field operations (not
mandatory).
3.3.1 Probe - Pack the probe in a case protected by polyethylene
foam or other suitable packing material. An ideal container is a
wooden case (or the equivalent) lined with foam material in which
separate compartments are cut to hold the individual devices.
This case can also contain a Pitot tube for velocity determina-
tions. The case should have handles that can withstand hoisting
and should be rigid enough to prevent bending or twisting of the
devices during shipping and handling.
3.3.2 Collection Flask and Valve - The collection flasks and
valves should be packed securely in a suitable shipping con-
tainer. An ideal container is a case or footlocker of approxi-
mately the following dimensions: 30 in. x 15 in. x 15 in. This
container, when lined with foam, will accommodate eight collec-
tion flasks with the appropriate mated flask valves.
3.3.3 Evacuation System, Temperature Gauges, Vacuum Lines,and
Reagents - A sturdy case lined with foam material can
contain the evacuation manifold, squeeze bulb, manometer, and
reagents for sample recovery. Special care should be taken with
mercury U-tube manometers to avoid any spillages.
3.3.4 Evacuation Pump - The vacuum pump should be packed in a
shipping container unless its housing is sufficient for travel.
Additional pump oil and oiler jar should be packed with the pump
if oil is required for its operation.
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 7 of 9
3.3.5 Glass Storage Containers - All glass storage containers
must be packed with cushion material at the top and bottom of the
case, and with some form of dividers to separate the components.
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 8 of 9
Table 3.1. ACTIVITY MATRIX FOR PRESAMPLING PREPARATION
Characteristic
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Apparatus Check
Probe
1. Clean; glass liner
inert to oxides of ni-
trogen
2. Heating properly if
equipped with heating
system
3. Leak free
1. Before each test
2. As above
3. Pressure <380 mm
(15 in.) Hg
Must be re-
placed
Collection
flask
Clean; volume within
+10 ml
Before each test,
clean with strong de-
tergent and hot wa-
ter and rinse with
tap and deionized dis-
tilled water; periodi-
cally clean with
grease remover
Repeat cleans-
ing of flask
and/or measure
volume
Evacuation
system
Vacuum of 75 mm (3 in.)
Hg absolute pressure
in each flask; leakage
rate <10 mm (0.4 in.)
Hg/min
Before each test,
check for leaks using
Hg-filled U-tube man-
ometer
Correct leaks
Absorbing
Reagents
Sulfuric acid,
concentrated
2.8 ml/1
Prepare fresh absorb-
ing solution weekly;
use graduated pipette
Make up new
solution
Hydrogen perox-
ide, 3%
As above
As above
(continued)
-------
Section No. 3.6.3
Revision No. 0
Date May 1, 1979
Page 9 of 9
Table 3.1. (continued)
Characteristic
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sample Recovery
Reagents
Sodium hydrox-
ide
40 g ACS reagent grade
NaOH in a l-i
volumetric flask
(Class A)
On makeup of solution,
use triple-beam bal-
ance and Class A
volumetric flask
As above
Water
Deionized distilled
to ASTM specifications
Dll 93-82, Type 3
Prepare
fresh for
each analy-
sis period
Analytical
Reagent
Potassium
nitrate
2.198 +0.001 g KN03
ACS reagent grade
into a 1-Jd volumetric
flask (Class A)
On makeup of solution,
use analytical bal-
ance
Purchase new
solution
Phenoldisul-
fonic acid
solution
25 g white phenol
ACS reagent grade in
150-ml concentrated
cylinder (Class A)
75 ml fuming sul-
furic acid
On makeup of solution,
use triple-beam bal-
ance and graduated
cylinder
On makeup of solution,
graduated cylinder
(Class A)
Make up new
solution.
As above
-------
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 1 of 11
4.0 ON-SITE MEASUREMENTS
The on-site measurement activities include transporting the
equipment to the test site, unpacking and assembling the equip-
ment, confirming duct measurements and traverse points (if volu-
metric flow rate is to be determined), velocity traverse, molec-
ular weight determination of the stack gas, moisture content,
sampling for oxides of nitrogen, and data recording. Table 4.1
at the end of this section summarizes the quality assurance
activities relative to on-site measurements.
4.1 Transport of Equipment to the Sampling Site
The most efficient means of transporting or moving the
equipment from ground level to the sampling site (as decided
during the preliminary site visit) should be used to place the
equipment on site. Care should always be exercised against
damage to the test equipment or injury to test personnel during
the moving phase. A "laboratory" type area should be designated
for preparation of absorbing reagent and charging of the flasks.
An acceptable alternative is to charge the flasks in the home
laboratory. Utilization of plant personnel or equipment (winches
and forklifts) in movement of the sampling gear is highly recom-
mended .
4.2 Preliminary Measurements and Setup
The Reference Method outlines the determination of the
concentration of oxides of nitrogen in the gas stream. The
volumetric flow rate must be determined utilizing Method 2,
Section 3.1, and Method 4, Section 3.3 of this Handbook so that
mass emission rate may be determined.
4.3 Sampling
The on-site sampling includes preparation and/or addition of
the absorbing reagent to collection flasks (if not performed at
home laboratory), setup of the evacuation system, connection
-------
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 2 of 11
of the electric service, preparation of the probe (leak check and
addition of particulate filter), insertion of probe into the
stack, purging of the probe, sealing of the port, evacuation of
flasks, sampling and recording of the data, and a final leak
check. In addition, EPA Reference Methods 1, 2, 3, and/or 4 may
have to be performed simultaneously with Method 7. This will be
specified by the applicable regulation, and the applicable refer-
ence method should be followed.
4.3.1 Preparation and/or Addition of Absorbing Reagent
to Collection Flasks - If preparation of absorbing reagent
is necessary on site, follow directions given in Section 3.6.3.
Pipette exactly 25 ml of absorbing reagent into the sample flask.
Place a properly lubricated flask valve into the collection flask
with the valve turned in the "purge" position. Lubrication of
joints is intended to prevent leaks and should not seal the bore
of the stopcock or contaminate the sample.
4.3.2 Assembling Sampling Train - Assemble the sampling train as
shown in Figure 1.1 and perform the following:
1. Visually check probe for liner separation (cracks,
etc.).
2. Place a loosely packed filter of glass or quartz wool
in the inlet end of the probe to trap any particulates.
3. Insert the probe into the stack to the sampling point,
and seal the opening around the probe.
4.3.3 Evacuation, Purge, and Sampling - A sample is taken as
follows:
1. Turn the pump and flask valves to the "evacuate" posi-
tions and evacuate to a minimum of 75 mm (3 in. ) Hg absolute
pressure or until the apparent boiling point is reached (bubbling
of absorbing solution).
2. Turn the pump valve to the "vent" position, turn off
the pump and check the manometer for fluctuations. The manometer
should stay stable (maximum deviation £10 mm (0.4 in.) Hg) for at
least 1 minute. If the mercury level changes, check for leaks
-------
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 3 of 11
and eliminate the problem. Pressure in the flask should be
£75 mm (3 in.) Hg absolute when sampling is commenced.
3. Record the volume of the flask and valve (V..,), the
r
flask temperature (t..), and the barometric pressure (P, ) on a
i car
data form (see Figure 4.1A or 4.IB) or in a field laboratory
notebook.
4. Turn the flask valve counterclockwise to the "purge"
position.
5. Turn the pump valve to the "purge" position.
6. Purge the probe and the vacuum line using the one-way
squeeze bulb.
7. If condensation occurs in the probe or the flask valve,
heat the probe until (upon purging) the condensation disappears.
8. Turn the pump valve to the "vent" position.
9. Turn the flask valve clockwise to its "evacuate" posi-
tion, and record the difference in the mercury levels in the
manometer. The absolute internal pressure in the flask (P.) is
equal to the barometric pressure less the manometer reading (Leg
A and Leg B).
10. Immediately turn the flask valve to the sample posi-
tion, and permit the gas to enter the flask until pressures in
the flask and sample line (i.e., duct, stack) are equal. This
will usually require about 15 s; a longer period indicates a
"plug" in the probe, which must be corrected before sampling is
continued.
11. After collecting the sample, turn the flask valve to
its "purge" position.
12. Disconnect the flask and valve from the sampling train
and shake the flask for at least 5 min.
4.3.4 Chemical Reactions of Sample Collection - If the gas being
sampled contains insufficient oxygen for the conversion of NO to
NO_ (e.g., an applicable subpart of the standard may require
taking a sample of a calibration gas mixture of NO in N2), then
oxygen should be introduced into the flask to permit this
-------
o
V
Sri
A.
2
g
•H
4-1
rt
u
o
co
Operator Barometric pressure (P,_ .) .19.8*/ in. Hg
a
Initial temperature
Initial pressure
in. Hg
/•-s
•r)
H
•H
t«
O
nt
•H
PM
•H
PQ
00
(U
60
0)
A
#£*
a) co
e «j o
rH U-( rH H
O cd S
> M-l >
O
1
0)
co n) a»
CD > ,0
rH B
Probe
temperature,
F
to t
r r r
"* « ?
• • '
^ <*> rK
^ r r
•
K) O aP
J 1?
"
0 0 o
r* rt rt
m m —
rO ^ Q
r- r- cP
o o O
— o o
tit
pQ f)O O
OL ^1 ^T
<
\^
I
^
a
PH
II
o
o
•H
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 4 of 11
en
-P
•H
x:
en
•H
rH
w
o
M-l
(U
-H
0)
T3
-H
X
o
fi
(0
tn
O
M
4J
•H
<:
r-l
•
•f
(U
tn
•H
-------
ff
cu
o
no
w
4->
cd
CJ
O
<0
J-l
3
CO
CO
a)
a
•H
4J
a)
>v
4J 4J
•H cd cd
O P M
o
4J
cd
4-1
cd S co
rH Cd P-
PH CO O
0)
(-1
4J
cd
M
0)
I-
0)
4J
cd
4J
1-1
c
0)
3
co
co
^^
•H
EH
oW
/~iH
4J
SwX
CJ
O
cd
•H
P^
•H
PQ
00
3
•rl
<3
00
3
/**\
s
o *o
ti
cd
*|M
co cd o)
cd > £
*! C
oT
3
0) 4->
O M CJ
H Q)O
P . p^
0)
4-1
0)
i-l (I) VJ
Cd 4-> Sf
CO CS
a
cy 4J o
rH C -rl
O. -H 4J
S O cd
CO d. CJ
CO O
r-H
a) t-i
rH
^ *
tf)
Oi
r
r
"~
«0 /V) IO
d
rO
0
l^
^ta
*
(X
O
0
??
O
~
(^
-
(i
^•B
(O
0
0
f\
*
0
7
a
o
9
^
r
O
o
T*
'
(°
/J «
0-(
v^
ri
r
CO
0
0
JL
f
£%J
1
^
0
o
o
00
O
o
^"*
1
^
^o
i.
+
-------
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 6 of 11
conversion. Oxygen may be introduced into the flask by one of
three methods: (1) Before evacuating the sampling flask, flush
with pure cylinder oxygen, and then evacuate flask to 75 mm (3.0
in.) Hg absolute pressure or less; or (2) inject oxygen into the
flask after sampling; or (3) terminate sampling with a minimum of
50 mm (2.0 in.) Hg vacuum remaining in the flask, record this
final pressure, and then vent the flask to the atmosphere until
the flask pressure is almost equal to atmospheric pressure.
Chemical reactions which occur during sampling adsorbtion
are:
NO sample: NO + ^2O2 "* N02 + H2° * 2N02 + H2°2 ~" 2HN03 •
NO2 sample: 2NO2+ H2°2 "* 2HN03 •
NO sample: (2NO) gaseous + 02 -> 2NO2 + H2O2 •* 2HN03.
4.4 Sample Recovery
The Reference Method requires a minimum sample absorption
period of 16 h in the flask. If the laboratory is close by, the
sample may be left in the flasks for return to the laboratory.
Otherwise, the appropriate data may be taken in the field, solu-
tions made alkaline and transferred to leak-free polyethylene
bottles after the required absorption period.
4.4.1 Flask Pressure, Temperature, and Barometric Pressure
After the absorption period is completed (>16 h), record the
barometric pressure and the room temperature (final temperature
(tf) on the integrity data forms (Figures 4.2A or 4.2B.)
1. Shake the flask and contents for 2 min.
2. Connect the flask to a mercury-filled U-tube manometer.
3. Open the valve from the flask to the manometer and
record the flask temperature (tf), the barometric pressure, and
the difference between the mercury levels in the manometer (Leg A
and Leg B). The absolute internal pressure in the flask (P^) is
the barometric pressure less the manometer reading.
4. Transfer the contents of the flask to a leak-free
polyethylene bottle.
-------
Plant
0 *.-•*»<*
9loiw-V
Date
) 2> I
~
Sample recovery personnel 3. *Hift ye/*.^
Person with direct responsibility for recovered samples
Barometric pressure, (P, )
in. Hg
P.
Sample
number
ftP-1
ftp- 3-
ftP-:>
Final pressure,
in. Hg
Leg Af
).&
;•*
d..O
Leg Bf
0-fe
o.-?
?-0
>£a
a-7.fcf
?-7-->f
*SW
Final temperature,
°F (tf)
13.
"7^
-13
°R (Tf ) b
533
5"3»
5-32.
Sample
recovery
time,
24-h
I'iaS^
;i^&
IH i^r
PH
adjusted
9 to 12
i^
*X
*/
Liquid
level
marked
^
•^
t/
Samples
stored
in locked
container
tX
t-X
^
Pf = Pbar - (Af
V"
Tf = tf + 460 F .
Lab person with direct responsibility for recovered samples ^?.
Date recovered samples received 3>/»ll"j Analyst 3". "Vn^e^t
All samples identifiable? >jgs
Remarks
Signature of lab sample trustee _
All liquids at marked level ? g &
Figure 4.2A. NO sample recovery and integrity data form
(English units).
h3 D » CO
p) p) (D (D
iQ rt < O
(D 0) H-rt
W H-
-J 31 H-O
fU O 3
hh
2 O
O '
vo o
-------
Plant
f Wvy-V
Date
Stl&t I
"?"?
. Barometric pressure, (pbar)
Person with direct responsibility for recovered samples p . fc. Q
Sample recovery personnel^
ftP-3
Final pressure,
mm Hg
Leg Af
HO- 1
30.6"
SO- *
Leg Bf
15--31
^o.'i
as- *f
pf
-?oSi
101
b-W
Final temperature,
°C (tf)
&a.~i
^a-*
£.a.."7
K (Tf)
St^-T. 1
^^5-.^
S^^. "7
Sample
recovery
time,
24-h
1 %»»
)-»>2»0
^H 1
PH
adjusted
9 to 12
•^
X"
Analyst ~^T.
All samples identifiable ? -y ef»
Remarks
Signature of lab sample trustee
All liquids at marked level ?
Figure 4.2B. NO sample recovery and integrity data form
(metric units).
••d D » cn
pj qj ro a)
iQ ft < O
(D (C (-•- rt
en H-
oo g H- O
pj O 3
O ^< 3
t-h 2
H 2 O
M- O •
I-1
vo
•-J
vo
U)
•
(Ti
-------
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 9 of 11
5. Rinse the flask three times with 5-ml portions of
deionized distilled water, and add the rinse water to the bottle.
6. Adjust the pH to between 9 and 12 by adding sodium
hydroxide (IN) dropwise (about 25 to 35 drops). Check the pH by
dipping a stirring rod into the solution and then touching the
rod to the pH test paper. Remove as little material as possible
during this step. The pH adjustment is mandatory. The NaOH
changes the sample, which is in the form of HNO3/ to NaN03. If
the pH is not adjusted, the HNO3 will be liberated during the
evaporation phase of analysis.
4.5 Sample Logistics (Data) and Packing of Equipment
The above procedures are followed until the required number
of runs are completed. Log all data on the form shown in Figure
4.2 A or 4.2.B
1. Check all sample containers for proper labeling (time,
date, location, number of test, and any pertinent documentation).
Be sure that a blank has been taken.
2. Record all data collected during the field test and
duplicate by the best means available. One set of data should be
mailed to the base laboratory, or given to another team member or
to the Agency; the original data should be hand carried.
3. Examine all sample containers and sampling equipment for
damage, and pack them properly for shipment to the base labora-
tory. All shipping containers should be properly labeled to
prevent loss of samples or equipment.
4. The sampling procedures can be reviewed after testing or
during the testing using an on site measurement checklist (Figure
4.3).
-------
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 10 of 11
Sampling
Volume of 25 ml of absorbing solution placed in flask?
Flask valve stopper in purge position?
Sampling train properly assembled?
Leak free?* Stopcock grease used? tX"
Type? £ - 73 W
Flask evacuated to 75 mm (3 in.) Hg pressure? iX"
Leakage from manometer observation?* ^
(e.g., maximum change in manometer of £10 mm (0.4 in.)
Hg/min)
Initial pressure of flask recorded?* _
Initial temperature of flask recorded?
Probe purged before sampling?
Sample collected properly?*
Flask shaken for 5 min after collection and disassembly
from train?*
Oxygen introduced to flask? A'/W Method used? _
Samples properly labeled and sealed and stored for shipment?
Sample Recovery
Samples allowed to remain in flasks for minimum of 16 h?*
Final flask temperature and pressure recorded?*
Sample transferred to leak-free polyethylene bottle?
Flask rinsed twice with 5-ml portions of distilled water
and rinse added to bottle containing sample? _ «*•*•"
pH adjusted to between 9 and 12?*
* Most significant items/parameters to be checked.
Figure 4.3. On-site measurements.
-------
Section No. 3.6.4
Revision No. 0
Date May 1, 1979
Page 11 of 11
Table 4.1. ACTIVITY MATRIX FOR ON-SITE MEASUREMENTS
Characteristic
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Apparatus
assembly
Operational
check
Assemble using Fig.
1.1; no leakage
Maximum vacuum of
75 mm (3 in.) Hg abso-
lute pressure
Leakage rate £10 mm
(0.4 in.) Hg/min
Before sample collec-
tion, visually and
physically inspect
all connections
Before sample
collection, use Hg-
filled U-tube man-
ometer
As above
Sample recovery
Shake flask for 5 min
Let flask set for a
minimum of 16 h
During each sample
collection, use
manometer, centigrade
thermometer, and pH
paper
Shake flask for 2 min
Determine flask pres-
sure and temperature
Adjust pH of sample to
9-12 with NaOH
Mark sample level on
container
Record data on data
form (Fig. 4.2)
Check for
leaks; repair
system; repair
test
Check system
for leaks;
check vacuum
pump
Check all
joints and
valves for
source of
leakage
Reject
sample, re-
run test
Sample logis-
tics
Properly label all
containers, etc
Record all data on
field data forms
(Fig. 4.1 and Fig.
4.2)
Visually check
each sample
As above
Complete the
labeling
Complete the
data records
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 1 of 10
5.0 POSTSAMPLING OPERATIONS
Table 5.1 at the end of this section summarizes the quality
assurance activities for sample analysis. If the laboratory
receives the samples in the sample flask, laboratory personnel
will have to complete the sample recovery procedures previously
explained in Section 3.6.4.
5.1 Procedures For Operating a Spectrophotometer
The correct manipulations of blanks and sample cells are
critical. Careless technique is unacceptable. The following
points are recommended and should be adhered to.
1. Designate the cuvettes as either a blank or a sample
cell. Do not interchange the cells during an analysis because
they are not always matched.
2. Do not touch the bottom of the cuvette with your fin-
gers.
3. Rinse the cuvette at least twice with the solution you
are about to measure.
4. Remove lint, liquid, and so forth with a lens tissue or
its equivalent.
5.2 Base Laboratory (Analysis)
5.2.1 Check of Field Sample Integrity - If the field samples
have been shipped in sample containers, be sure that all samples
are identifiable and that the liquid level of each is at its
mark. If a sample is not identifiable or if a loss of liquid is
detected, note it on the data form, as shown in Figures 4.2A and
4.2B. When a noticeable amount of leakage has occurred, use an
alternative method, subject to the approval of the administrator,
to correct the final value; approval should have been requested
prior to testing. An alternative method is as follows:
1. Mark the new level of the sample.
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 2 of 10
2. Transfer the sample to a 50-ml volumetric flask, along
with two 5-ml deionized distilled water rinsings of the con-
tainer.
3 . Add water to the sample storage container to the init-
ial sample mark, and measure the initial sample volume (V •, )
in ml. 1
4. Add water to the sample storage container to the mark
of the transferred sample, and measure the final volume (V , )
in ml.
5. If (v_0nn )
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 3 of 10
sample analysis and thus prevent having to invalidate the field
samples and to require a complete retest of the source.
The control samples and the standard KN03 solution should be
prepared using the following procedure.
1. Dry the potassium nitrate (KN03) ACS reagent grade at
105° to 110°C for a minimum of 2 h prior to the preparation of
the control sample and the standard solution.
2. Place a 2 g Class-S weight on the balance. The
balance must agree within ±2 mg of the Class-S standard weight.
3. Cool and store KN03 in desiccator. Weigh and then
dissolve 2.198 ±0.002 g of dried KNO3 in about 800 ml of
deionized distilled water in a 1-A volumetric flask (Class A).
4. Dilute to the mark with deionized distilled water, and
label and date the solution.
5. Dilute 10.0 ml of the standard solution to the mark in
a 100-ml volumetric flask with deionized distilled water, and
label as "control sample" for analysis.
6. Weigh and then dissolve 2.198 ±0.002 g of dried KNO3
in about 800 ml of deionized distilled water in a l-£ volu-
metric flask (Class A).
7. Dilute to the mark with distilled deionized water, and
label and date as the standard KN03 solution.
8. Dilute 10.0 ml of the standard KNO3 solution to the
mark in a 100-ml volumetric flask with deionized distilled water,
and label as "working standard KNO3 solution" for analysis.
9. Pipette 0.0, 2.0, 4.0, 6.0, and 8.0 ml of the working
standard KNO3 solution into five 50-ml volumetric flasks.
10. Pipette 2.0, 4.0, and 6.0 ml of the control sample
into another set of 50-ml volumetric flasks.
11. Add 25 ml of absorbing solution, 10 ml of deionized
distilled water, and then sodium hydroxide (IN) dropwise to each
of the eight flasks until the pH is between 9 and 12 (about 25 to
35 drops each). Check for alkalinity by touching a glass rod
first to the solution and then to pH paper. Note: The pH check
is mandatory.
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 4 of 10
12. Dilute to the mark with deionized distilled water, and
mix thoroughly.
5.2.3 Analysis of Control Samples, Standard Solutions, and
Field Samples - The analysis of the samples has a time-dependent
color change. To provide an estimate of the accuracy and preci-
sion of the analysis, the control sample is analyzed at the same
time as the field sample. The standard solutions, field samples,
and control samples should be analyzed in the following manner.
1. Pipette a 25-ml aliquot of each solution into a separ-
ate porcelain evaporating dish.
2. Evaporate the solutions (standards, field samples, and
control samples) to dryness on a steam bath and then cool. Note;
Do not evaporate on a hot plate or in an oven unless it is
thermostatically controlled below 70°C (160°F). Remove samples
from steam bath just before complete dryness is reached (the
bottom of the dish should be covered with a smooth film), so
that the last droplet evaporates as the dishes cool.
3. Add 2.0 ml of phenoldisulfonic acid reagent to each
dried residue and either mix thoroughly with a polyethylene
policeman or let the solution stand for 5 min.
4. Add 1.0 ml of deionized distilled water and four drops
of concentrated sulfuric acid, and then heat the solution on a
steam bath for 3 min with occasional stirring.
5. Cool. Add 20 ml of deionized distilled water, and mix
well by stirring.
6. Add concentrated ammonium hydroxide dropwise (a 50-ml
burette is suggested) with constant stirring until the pH is 10,
as determined either by pH paper or by the first yellow color
that does not fade.
7. Transfer directly to a 100-ml volumetric flask if the
sample does not contain solids. Rinse the evaporating dish with
at least three 5-ml portions of deionized distilled water, and
then add the washings to the contents of the flask.
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 5 of 10
8. Remove any solids from the sample by filtering the
sample through a Whatman No. 41 filter paper into a 100-ml volu-
metric flask; rinse each evaporating dish with three 5-ml por-
tions of deionized distilled water; filter these
three rinses. Wash the filter with at least three 15-ml portions
of deionized distilled water, and then add the filter washings to
the contents of the volumetric flask.
9. Dilute to the 100-ml mark with deionized distilled
water and mix the contents of the flask thoroughly.
10. Measure the absorbance of the standard solutions at
the optimum wavelength, using the blank solution as a zero
reference. Note; The flasks should not sit in warm or light
areas for very long before analysis because precipitates may
form.
11. Record the standard solutions and control sample data
on Figure 5.1 or similar form.
12. Read the absorbance of the field samples from Run 1 and
then one of the control samples; Run 2 and another control
sample; and Run 3 and the last control sample.
13. If the absorbance reading of any field sample is
greater than the absorbance reading of the standard sample A.
(the absorbance of the 400 (jg NC>2 standard), then dilute the
sample and the blank with equal volumes of deionized distilled
water using pipettes to get ratios of 25/5, 25/10, and so forth.
14. Record all field sample analysis data as shown in
Figure 5.2, and calculate the mass (m) of NO for each sample as
J\
|jg of NO2.
15. Perform the calculations and the accuracy checks of the
three control samples as shown in Figure 5.1. It is recommended
that the agreement for each control sample be within ±15%. The
standard solution and control sample analytical form should be
included in the emission test report as a documentation of the
analytical accuracy. This accuracy limit of ±15% for intra-
laboratory control samples is recommended based on the control
limit of ±20% for interlaboratory audit results discussed in
Section 3.6.8.
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 6 of 10
Date 3-3-77
Analyst J~.
Optimum wavelength
Blank used as reference?
om
Sample
number
Al
A2
A3
A4
SI
S2
S3
Sample,
(Jg
100
200
300
400
100
200
300
Working
solution
X
X
X
X
Control
sample
X
X
X
Measured,
absorbance,
OD
o. /7>L
0 • 3 £>o
n £TiaO
£-77O
o.tfo
o.SBl
o.sio
Calculated
absorbance,
OD
_
-
-
-
0./9/
O.3&I
Q.sni
Absorbance
comparison
error, %
_
-
-
-
- 0. 5"
o.o
-0.2.
Av8C O. 2.
OD = (|Jg)/K ; i.e., SI calculated absorbance = 100/K .
K = 100
c
Aj + 2A2 + 3A3 + 4A4'
k^
,4,
^i-
>»i
Absorbance comparison errors:
I(measured absorbance, OD) - (calculated absorbance, OD)|.
% = 100 x
L
calculated absorbance, OD
Average of absolute values.
Figure 5.1. Standard solution and control sample
analytical data form.
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 7 of 10
Plant
Date samples received -3/Z/77
Aliquot factor >C
Blank absorbance USt& f\S
Calibration factor (K )
c
Run number(s) A P-/
Date analyzed 3/3/77
Samples analyzed by J\
Date reviewed by 7J
Date of review ..
Sample
number
AP-I
#P~Z,
*P-3
Sample
absorbance ,
A
0- 745
0- L>2> l
b. *V s~o
Dilution
factor,
F
/.*>
/.o
Z..O
Total mass of NO
as NO, in sample,
z m
1 8"J
blol*
9iTO
m = 2 K AF, Note; If other than a 25 ml aliquot is used for
analysis, the factor 2 must be replaced by a corresponding
factor.
Figure 5.2 NO laboratory data form.
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 8 of 10
16. When the above criteria cannot be met, it is recom-
mended that the analytical techniques be checked and then the
field sample and control sample analysis be repeated using a
20.0-ml aliquot of the remaining field samples.
17. The main parameters of the analytical procedures may
be checked during or after the analysis, using a posttest
operations form (Figure 5.3).
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 9 of 10
Reagents
Phenoldisulfonic acid stored in dark stoppered bottle? \S
Sulfuric acid, concentrated, 95% minimum assay reagent
grade?
Ammonium hydroxide, concentrated reagent grade?
Sample Preparation
Has liquid level noticeably changed?* fVO
Original volume Corrected volume
Analysis
Spectrophotometer calibrated?* \s
Setting for maximum absorbance of standard yD Q nm
Control sample prepared?* i/
Any solids in sample removed through Whatman,Nq^ 41 filter
paper?
an ,No.
///ft
Absorbance measured at optimum wavelength used for the stand-
ards, using the blank solution as a zero reference?
All analytical data recorded on checklist and laboratory form?
* Most significant items/parameters to be checked.
Figure 5.3. Posttest operations.
-------
Section No. 3.6.5
Revision No. 0
Date May 1, 1979
Page 10 of 10
Table 5.1. ACTIVITY MATRIX FOR SAMPLE ANALYSIS
Characteristic
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Control sample
analysis
(recommended)
Agree within 15% of
the working standards
for each sample
Compare control sample
analysis to working
standards analysis
Redo field
and control
samples and/
or seek
assistance
with analyti-
cal technique
Field sample
analysis
No sample volume lost,
or final results
corrected
Working standard
analyzed simultaneous-
ly with field sample
No absorbance readings
outside working
standard solution
concentration
Compare liquid level
to mark before
analysis
Use same solutions
and techniques used
for control samples
Dilute sample and
blank with equal
amounts of deionized
distilled water
Void sample
As above
Dilute and
reanalyze
Data recording
All pertinent data
recorded on Figs. 5.1
and 5.2
Visually check
Supply missing
data
-------
Section No. 3.6.6
Revision No. 0
Date May 1, 1979
Page 1 of 6
6.0 CALCULATIONS
Calculation errors due to procedural or mathematical mis-
takes can be a large component of total system error. Therefore,
it is recommended that each set of calculations be repeated or
spot-checked, preferably by a team member other than the one who
performed the original calculations. If a difference greater
than typical round-off error is detected, the calculations should
be checked step-by-step until the source of error is found and
corrected. A computer program is advantageous in reducing calcu-
lation errors. If a standardized computer program is used, the
original data entry should be checked, and if differences are
observed, a new computer run should be made. Table 6.1 at the
end of this section summarizes the quality assurance activities
for calculations.
Calculations should be carried out at least one extra deci-
mal figure beyond that of the acquired data and should be rounded
after final calculation to two significant digits for each run or
sample. All rounding of numbers should be performed in accord-
ance with the ASTM 380-76 procedures. All calculations are then
recorded on a form such as the one in Figure 6.1A or 6. IB, fol-
lowing the nomenclature list.
6.1 Nomenclature
The following nomenclature is used in the calculations.
A = Absorbance of sample.
C = Concentration of NO as NO-, dry basis, corrected
to standard conditions, mg/dscm (Ib/dscf).
F = Dilution factor (i.e., 25/5, 25/10, etc.) required
only if sample dilution was needed to reduce the
absorbance to the range of calibration.
K = Spectrophotometer calibration factor.
o
m = Mass of NO as NO- in gas sample, pg.
a £.1
-------
Section No. 3.6.6
Revision No. 0
Date May 1, 1979
Page 2 of 6
Pf = Final absolute pressure of flask, mm (in.) Hg.
P. = Initial absolute pressure of flask, mm (in.) Hg.
P , , = Standard absolute pressure, 760 mm (29.92 in.) Hg
Tf = Final absolute temperature of flask, K (°R).
T^ = Initial absolute temperature of flask, K (°R).
T td = Standard absolute temperature, 293K (528°R).
V = Sample volume at standard conditions, dry basis,
ml.
Vf = Volume of flask and valve, ml.
V = Volume of absorbing solution, 25 ml.
a
6.2 Calculations
The following are the equations used with example calcula-
tion forms Figures 6. 1A and 6.IB to calculate the concentration
of nitrogen oxides.
6.2.1 Sample Volume - Calculate the sample volume on a dry basis
at standard conditions (760 mm (29.92 in.) Hg and 293K (528°R))
by using the following equation.
v - ^td'V V £f-!A
op1 P \T T /
sc *std W Ii/
/P p \
- K iv ?«; mi\ (_£ ~ _i| Equation 6-1
- ^T f * \T^ T^)
where
V
K-, = 0.3858 :=— for metric units, or
1 mm Hg
o
r>
K, = 17.64 5— for English units.
l in. Hg
-------
Section No. 3.6.6
Revision No. 0
Date May 1, 1979
Page 3 of 6
6.2.2 Total pg of NO^ Per Sample - Calculate the total pg of N02
per sample by using Equation 6-2.
m = 2 K AF . Equation 6-2
c
where
2 = 50/25, the aliquot factor (if other than a
25-ml aliquot was used for analysis, the
corresponding factor must be substituted) .
6.2.3 Sample Concentration - Calculate the sample concentration
on a dry basis at standard conditions using Equation 6-3.
_ _ „ m ] Equation 6-3
" 2 [Vsc
where
3 3
K2 = 10 L?g/mT for metric units, or
K2 = 6.243 x io~5 for English units.
-------
Section No. 3.6.6
Revision No. 0
Date May 1, 1979
Page 4 of 6
Sample Volume
v = ^ 0 I 3 ml, p = Z. T.k £ in. Hg,
pi = _ -
. Hg,
. °R
V
sc
= 17.64 (Vf - 25)
Ti
= L 1 8 Q ml Equation 6-1
Total pg NO2 Per Sample
=6.7^30D, F= /.CO
^— — —^ "•"• ^™" ^^ ~"~
Equation 6.2
m = 2Kc AF =
_ H 03. fjg Of NO,
Sample Concentration
C = 6.243 x 10
-5
j = 2.7 5" x
10~5 Ib/dscf
Figure 6.1A. Nitrogen oxide calculation form
(English units).
-------
Section No. 3.6.6
Revision No. 0
Date May 1, 1979
Page 5 of 6
Sample Volume
= Zoi3. ml, P. = 7 £ 2.O mm Hg, T. = 2. 9 6 .2 K
— — — — — — — — — —
mm
Hg, T± = Z 9 5-6 K
V = 0.3858 (V,, - 25)
SO X
Ti
= • ml
Equation 6-1
Total |jg N02 Per Sample
K = _ ^"Z f.,A = 0.2 4. 3 OD, F =
C """"
m = 2K AF = _ 7 0*t' Hg of N09.
C ^
Equation 6-2
Sample Concentration
C = 10'
x 1C) mg/dscf.
Equation 6-3
Figure 6.IB. Nitrogen oxide calculation form
(metric units).
-------
Section No. 3.6.6
Revision No. 0
Date May 1, 1979
Page 6 of 6
Table 6.1 ACTIVITY MATRIX FOR CALCULATIONS
Characteristic
Sample volume
calculation
Sample mass
calculation
Sample concen-
tration
Calculation
check
Document and
report re-
sults
Acceptance limits
All data available;
calculations correct
within round-off error
As above
As above
Original and check
calculations agree
within round-off error
All data available;
calculations correct
within round-off error
Frequency and method
of measurement
For each sample, exam-
ine the data form
As above
As above
For each sample, per-
form independent cal-
culation using data
on Figs. 4.1, 4.2, and
4.3
For each sample, exam-
ine the data form
Action if
requirements
are not met
Complete the
data or void
the sample
As above
As above
Check and
correct
all data
Complete the
data or void
the sample
-------
Section No. 3.6.7
Revision No. 0
Date May 1, 1979
Page 1 of 2
7.0 MAINTENANCE
The normal use of emission-testing equipment subjects it to
corrosive gases, extremes in temperature, vibration, and shock.
Keeping the equipment in good operating order over an extended
period of time requires knowledge of the equipment and a routine
maintenance program which should be performed quarterly or upon
improper functioning of the apparatus. It is suggested that the
vacuum pump be disassembled and cleaned yearly. A summary of
the components with maintenance procedures is presented in
Table 7.1 at the end of this section. The following procedures
are not required, but are recommended to increase the reliability
of the equipment.
7.1 Pumps
Several types of pumps are used in the present commercial
sampling trains. The two most common are the fiber vane pump
with in-line oiler and the diaphragm pump. The fiber vane pump
requires a periodic check of the oiler jar. The oil should be
translucent. During the yearly disassembly or if the fiber vane
pump starts to run erratically, the head should be removed and
the fiber vanes changed. The diaphragm pump will show a leak
when the diaphragm needs changing. If the diaphragm pump runs
erratically, it is usually due to a bad diaphragm (causing leak-
age) or to malfunctions in the valves. The valves should be
cleaned annually by complete disassembly of the pump.
7.2 Shipping Containers
Since the majority of the sampling train is glassware, the
shipping containers are very important for protection and safety.
All shipping containers should be inspected quarterly for their
condition, and repaired or modified to assure the safety of the
equipment.
-------
Section No. 3.6.7
Revision No. 0
Date May 1, 1979
Page 2 of 2
Table 7.1 ACTIVITY MATRIX FOR MAINTENANCE
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Routine main-
tenance
Proper functioning
Perform routine main-
tenance quarterly;
disassemble and clean
yearly
Replace parts
as needed
Fiber vane pump
Oil translucent pump
leakless and capable
of pulling a vacuum of
less than 75 mm (3 in.)
Hg absolute pressure
Check of oiler jar
periodically; remove
head and change fiber
vanes
Replace as
needed
Diaphragm pump
Leak free, valves func-
tioning properly, and
capable of pulling a
vacuum of <75 mm
(3 in.) Hg absolute
pressure
Clean valves during
disassembly; replace
diaphragm as needed
Replace when
leaking or
malfunctioning
Shipping con-
tainer
Protect equipment
from damage
Inspect quarterly;
repair as needed
Replace
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 1 of 8
8.0 AUDITING PROCEDURE
An audit is an independent assessment of data quality.
Independence is achieved if the individual(s) performing the
audit and their standards and equipment are different from the
regular field crew and their standards and equipment. Routine
quality assurance checks by a field team are necessary in genera-
tion of good quality data, but they are not part of the auditing
procedure. Table 8.1 at the end of this section summarizes the
quality assurance functions for auditing.
345
Based on the results of collaborative tests ' ' of Method
7, two specific performance audits are recommended:
1. Audit of the analytical phase of Method 7.
2. Audit of data processing.
It is suggested that a systems audit be conducted as specified by
the quality assurance coordinator, in addition to these perform-
ance audits. The two performance audits and the systems audit
are described in detail in Subsections 8.1 and 8.2, respectively.
8.1 Performance Audits
Performance audits are made to quantitatively evaluate the
quality of data produced by the total measurement system (sample
collection, sample analysis, and data processing). It is recom-
\
mended that these audits be performed by the responsible control
agency once during every enforcement source test. A source test
for enforcement comprises a series of runs at one source. The
performance audit of the analytical phase is subdivided into two
steps: (1) a pretest audit which is optional, and (2) an audit
during the actual analysis of the field samples which is re-
quired.
8.1.1 Pretest Audit of Analytical Phase Using Aqueous
Potassium Nitrate (Optional) - The pretest audit described
in this subsection can be used to determine the proficiency of
the analyst and the standardization of solutions in the Method 7
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 2 of 8
analysis and should be performed at the discretion of the agency
auditor. The analytical phase of Method 7 can be audited with
the use of aqueous potassium nitrate samples provided to the
testing laboratory before the enforcement source test. Aqueous
potassium nitrate samples may be prepared by the procedure de-
scribed in Section 3.6.5 on control samples preparation.
The pretest audit provides the opportunity for the testing
laboratory to check the accuracy of its analytical procedure.
This audit is especially recommended for a laboratory with little
or no experience with the Method 7 analysis procedure as de-
scribed in this Handbook.
The testing laboratory should provide the agency/organi-
zation requesting the performance test with a notification of the
intent to test 30 days prior to the enforcement source test. The
testing laboratory should also request that the agency/organiza-
tion provide the following performance audit samples: two
samples at a low concentration (250 to 500 mg NO^/dscm of gas
sampled) and two samples at a high concentration (600 to 1000 mg
NO2/dscm of gas sampled). At least 10 days prior to the
enforcement source test, the agency/organization should provide
the four audit samples. The concentrations of the two low and
two high samples should not be identical.
The testing laboratory will analyze one sample at the low
concentration and one at the high concentration, and submit their
results to the agency/organization prior to the enforcement
source test. Note: The analyst performing this optional audit
must be the same analyst audited during the field sample
analysis described in Subsection 8.1.2.
The agency/organization determines the percent accuracy, %A,
between the measured N02 concentration and the audit or known
values of concentration. This %A is a measure of the bias of the
analytical phase of Method 7. Calculate %A using Equation 8-1.
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 3 of 8
- CN09
%A = =-= ,.. x 100 Equation 8-1
where
CM_ (M) = concentration measured by the lab analyst
WU2 mg/ml, and
CN_ (A) = audit or known concentration of the audit
2 sample, mg/ml.
The recommended control limit for the pretest audit is the
80th percentile value for %A based on the results of three
audits (11/77, 5/78, and 10/78) performed by the Environmental
Monitoring and Support Laboratory, USEPA, Research Triangle Park,
12 13
North Carolina. ' The 80th percentile values and the known
audit concentrations are given below for each concentration
range, 250 to 500 mg NO /dscm and 600 to 1000 mg NO /dscm. By
X X
definition, 80% of the laboratory participants in the audit
obtained values of %A less than the 80th percentile values tabu-
lated below. The 80th percentile is recommended for NO instead
of the 90th percentile as used for SO2 in Method 6, Section
3.5.8, even though it is recognized that about one out of five
laboratories audited would be expected to exceed the 80th per-
centile limits for the pretest audits.
250 to 500 mg NO /dscm
Known audit
concentration 80th percentile for %A,
Audit date mg NO../dscm %
11/77 421 16.2
5/78 516 13.6
5/78 328 14.9
10/78 246 15.6
10/78 458 17.2
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 4 of 8
600 to 1000 mg NO
Audit date mg NO /dscm
X
Known audit
concentration 80th percentile for %A,
11/77 804 16.4
5/78 703 19.7
5/78 938 21.3
10/78 731 17.5
10/78 880 18.7
Based on the results in the previous tables, a control limit
of 20% is suggested for both concentrations levels.
If the results of the pretest audit exceed 20% the agency/
organization should provide the correct results to the testing
laboratory. After taking any necessary corrective action, the
testing laboratory should then proceed to analyze the two re-
maining samples and report the results immediately to the
agency/organization before the enforcement source test analysis.
8.1.2 Audit of Analytical Phase Using Aqueous Potassium
Nitrate (Required) - The agency should provide two audit
samples to be analyzed along with the field samples from the
enforcement source test. The purpose of this audit is to assess
the data quality at the time of the analysis. The %A of the
audit samples is determined using Equation 8-1. The results of
the calculated %A should be included in the enforcement source
test report as an assessment of accuracy of the analytical phase
of Method 7 during the actual enforcement source test.
8.1.3 Audit of Data Processing - Calculation errors are preva-
345
lent in Method 7. ' ' Data processing errors can be determined
by auditing the recorded data on the field and laboratory forms.
The original and audit (check) calculations should agree within
round-off error; if not, all of the remaining data should be
checked. The data processing may also be audited by providing
the testing laboratory with specific data sets (exactly as would
occur in the field)and by requesting that the data calculation be
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 5 of 8
completed and the results returned to the agency/organization.
This audit is useful in checking both computer programs and
manual methods of data processing.
8.2 Systems Audit
A systems audit is an on-site qualitative inspection and
review of the total measurement system (sample collection, sample
analysis, data processing, etc.). Initially, a systems audit is
recommended for each enforcement source test, defined here as a
series of three runs at one source. After the test team gains
experience with the method, the frequency of audit may be re-
duced—for example, to once for every four tests.
The auditor should have extensive background experience in
source sampling, specifically with the measurement system being
audited.
The functions of the auditor are summarized in the follow-
ing:
1. Inform the testing team of the results of pretest
audits, specifying any area(s) that need special attention or
improvement.
2. Observe procedures and techniques of the field team
during sample collection.
3. Check/verify records of apparatus calibration checks
and quality control charts used in the laboratory analysis of
control samples from previous source tests where applicable.
4. Record the results of the audit and forward them with
comments to the team management so that appropriate corrective
action may be initiated.
While on site, the auditor observes the source test team's
overall performance including the following specific operations:
1. Setting up and leak testing the sampling train.
2. Preparing the absorbing solution and adding it to the
collection flasks.
3. Collecting the sample.
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 6 of 8
4. Sample absorption, recovery, and preparation for ship-
ment.
Figure 8.1 is a suggested checklist for the auditor.
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 7 of 8
Presampling Preparation
Yes No
_(/_ 1. Information concerning combustion effluents that may
act as interferents
v 2. Plant operation parameters variation
>X* 3. Calibration of the flask and valve volume
three determinations
\/ 4. Absorbing reagent preparation
On-site Measurements
yX 5. Leak testing of the sampling train
tX 6. Preparation and pipetting of absorbing solution
into sampling flask
Postsampling
(Analysis and Calculation)
7. Control sample analysis
>X 8. Sample aliquotting technique
* 9. Evaporation and chemical treatment of sample
S _ 10. Spectrophotometric technique
a. Preparation of standard nitrate samples
b. Measurement of absorbance, including blanks
c. Calibration factor
d. Wavelength and absorbance, including blanks
\s _ 11. Calculation procedure and checks
a. Use of computer program
b. Independent check of calculations
Comments
^
y
Figure 8.1. Method 7 checklist to be used by auditors
-------
Section No. 3.6.8
Revision No. 0
Date May 1, 1979
Page 8 of 8
Table 8.1. ACTIVITY MATRIX FOR AUDITING PROCEDURE
Audit
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Spectrophotom-
eter analysis
using reference
samples of
dilute KNO
solutions
V/M)
°-80< ^
-------
Section No. 3.6.9
Revision No. 0
Date May 1, 1979
Page 1 of 1
9.0 RECOMMENDED STANDARDS FOR ESTABLISHING TRACEABILITY
To achieve data of desired quality, two essential considera-
tions are necessary: (1) the measurement process must be in a
state of statistical control at the time of the measurement and
(2) the systematic errors, when combined with the random varia-
tion (errors or measurement), must result in an acceptable uncer-
tainty. As evidence in support of good quality data, it is
necessary to perform quality control checks and independent
audits of the measurement process; to document these data; and to
use materials, instruments, and measurement procedures that can
be traced to an appropriate standard of reference.
Data must be routinely obtained by repeat measurements of
standard reference samples (primary, secondary, and/or working
standards) and the establishment of a condition of process con-
trol. The working calibration standards should be traceable to
standards of higher accuracy, such as that below.
Class-S weights (made to NBS specifications) are recommended
for the analytical balance calibration. See Section 3.6.2 for
details on balance calibration checks.
-------
Section No. 3.6.10
Revision No. 0
Date May 1, 1979
Page 1 of 3
10.0 REFERENCE METHOD*
METHOD 7— DrrEiurNATToN or Nnioocif Om>*
EMISSIONS FROM STATIONABT Souwu
1. Prtndpli an4 Atfiltabiitt
1.1 Principle. A grab sample is collected in an evacu-
ated flask containing a dilute sulfuric acid-hydrogen
peroxide absorbing solution, and the nitrogen oxides,
except nitrous oxide, are measured colonmetericallr
osing the phenoldisulfonlc acid (PD8) procedure.
1.2 Applicability. This method Is applicable to the
measurement of nitrogen oxides emitted from stationary
sources. The range of the method has been determined
to be 2 to WO milligrams NO, (as NOi) per dry standard
cubic meter, without having to dilute toe sample.
3. Apftratut
2.1 Sampling (see Figure 7-1). Other grab earapUng
system* or equipment, capable ot measuring sample
volume to within ±2.0 percent and collecting a sufficient
sample volume to allow analytical reproduciblUty to
within ±3 percent, will be considered acceptable alter-
natives, subject to approval o( the Administrator, U.S.
Environmental Protection Agency. The following
equipment is used in sampling:
2.1.1 Probe. Boroallicate (last tubing, sufficiently
heated to prevent water condensation and equipped
with an in-stack or out-etack Biter to remove paniculate
matter (a plug of glast wool is satisfactory (or this
. ->• r«. » . _ . .... ' ^ ^
probe
purpose). Stainless steel or Teflon > tubing may also be
used for the probe. Heating Is not necessary I/ toe
remains dry during the purging period.
> Mention of trade name* or specific products does not
constitute endorsement by the Environmental Pro-
tection Agency,
2.1.2 Collection Flask Two-liter borosilicate, round
bottom flask, with short neck and 24/40 standard taper
opening, protected against implosion or breakage.
2.1.3 Flask Valve. T-bore stopcock connected to a
24/40 standard taper joint.
2.1.4 Temperature Gauge. Dial-type thermometer, or
other temperature gaupe, capable of measuring 1° C
(2' F) Intervals from -4 to 50f C (25 to 125° F).
2.1.5 Vacuum Line. Tubing capable of withstanding
a vacuum of 75 mm Hx (3 in. Hg) absolute pressure, with
"T" connection and T-bore stopcock.
2.1.6 Vacuum Gauge. U-tube manometer, 1 meter
!3C in.), with 1-mm (0.1-in.) divisions, or other gauge
capable of measuring pressure to within ±2.5 mm Kg
(0.10 in. Kg).
2.1.7 Pump. Capable of evacuating the collection
flask to a pressure equal to or less than 75 mm Hg (3 In.
Hi)-absolute.
2.US Squeeze Bulb. One-way.
2.1.9 Volumetric Pipette. 25 ml.
2.1.10 Stopcock ana Ground Joint Grease. A high-
vacuum, high-temperature chlorofluorocarbon grease la
required. Halccarbon 25-58 has been found to be effective.
2.1.11 Barometer. Mercury, aneroid, or other barom-
eter capable of measuring atmospheric pressure to within
2.S mm Hg (0.1 in. Hg). In many caws, the barometric
reading may be obtained from a nearby national weather
service station, in which case the station value (which IB
the absolute barometric pressure) shall be requested and
an adjustment for elevation differences between the
weather station and sampling point shall be applied at a
rate of minus 2.5 mm Hg iQ 1 in. Hg) per 30 m (100 ft)
elevation increase, or vice versa for elevation decrease.
2.2 Sample Recovery. Tbe following equipment Is
required lor sample recovery
2.2.1 Graduated Cylinder. 50 ml with 1-ml divisions.
2.2-2 Storage Containers. Leak-free polyethylene
bottles.
2.2.3 Wash Bottle. Polyethylene or glass.
2.2.4 Glass Stirring Rod.
2.2.5 Test Paper for Indicating pH. To cover the pH
range of 7 to 14.
2.3 Analvsk. For the analysis, the following equip-
ment Is needed:
2.3.1 Volumetric Pipettes. Two 1 ml. two 2 ml, one
3 ml, one 4 ml, two 10 ml, and one 29 ml for each sample
and standard.
2.3.2 Porcelain Evaporating Dishes. 174- to 250-ml
capacity with lip for pouring, one for each sample and
each standard. The Coors No. 45006 (shallow-form, 195
ml) has been found to be satisfactory. Alternatively,
Pplymethyl pentene beakers (Nalge No. 1203, ISO ml), or
glass beakers (ISO ml) may be used. When glass beakers
are used, etching of the beakers may cause solid matter
to be present In the analytical step, the solids should be
removed by filtration (set Section 4.3).
Z.JU Scram Bath, tow-temperature ovens or thermo-
statically controlled hot plates kept below 70° C (1«0* F)
«Tf acceptable alternatives. '
?•!'! S'PPP'J", P'P«"« <»• Dropper. Three required.
2.3.5 Polyethylene Policeman. One for each sample
and each standard.
?•?•? Graduated Cylinder. 100ml with 1-ml divisions.
2-3.7 Volumetric Flasks. SO ml (one for each sample),
100 ml (one for each sample and each standard, and one
for the working standard ZNOi solution), and 1000 ml
(one).
2.3.8 Spectrophotomeur. To measure absorbance at
410 run.
2-3.0 Graduated Pipette. 10 ml with 0.1-ml divisions.
2.3.10 T«t Paper for Indicating pH. To cover the
pH range of 'toll.
2.3.11 Analytical Balance. To measure to within 0.1
mg.
PROBE
FLASK VALVE'
r
FILTER
GROUND-GLASS SOCKET
§ NO. 12/6
110 run
3-WAY STOPCOCKr
T-BORE. i PYREfc
2-mm BORE. 8-mm 00
FLASK
FLASK SHIELD^. ,\
SQUEEZE BULB
MP VALVE
PUMP
THERMOMETER
GROUND-GL,
STANDARD TAPER.
SLEEVE NO. 24/40
210 mm
GROUND-GLASS
SOCKET. § NO. 12/5
PYREX
•FOAM ENCASEMENT
BOILING FLASK •
2-LiTER, ROUND-BOTTOM. SHORT NECK.
WITH I SLEEVE NO. 24/40
Figure 7-1. Sampling train, flask valve, and flask.
*40 CFR 60, July 1, 1978
-------
Section No. 3.6.10
Revision No. 0
Date May 1, 1979
Page 2 of 3
3.
Unless otherwise Indicated, It Is Intended thai all-
nwgetrts conform te \hi> specifications established by the
Comrnitiw on Analytical Rewenls of the American
Chemical Society, where snrri siHKificatioas are avail-
able; otherwise, use the best available grade.
3.1 Sampling. To prepare the absorbing solution,
cautiously add 2 & ml concentrated HjSOi to 1 liter of
4«Jonir.ed, distillnd witer. Mil well and add 6 ml of 3
percent hydrogen peroxide, (rashly prepared from 30
percent hydrogen peroxide solution. The absorbing
solution should be used within 1 week of Its preparation.
Do not expose ui raueme heat or direct sunlight.
1.2 Sample Recovery. Two reagents are required for
asa&ple recovery.
S.2.1 Sodium Hydroxide (IN). Dissolve 40 g NaOH
in drionlsed, distilled water and dilute to I liter.
1.2.2 Water. Dejonlted, distilled to conform to ASTM
•peciaoatioa XH193-74, Type 3. At the option of the
analyst, the KMNO< tot for oxlditable organic matter
may he omitted when hrjth concentrations of organic
muter are not expected to oe present.
3.3 Analysis, for the analysis, the following reagents
are required:
3.3.1 Fuming Bulfuric Acid. IS to 18 percent by weight
free sulfur trioiide. HANDLE WITH CAUTION.
3.3.2 Phenol. White solid.
3.3.3 Bulfuiic Acid. Concentrated, 85 percent mini-
mum aisay. HANDLE WITH CAUTION.
3.3.4 Potassium Nitrate. Dried at 104 to 110° C (220
to 230° F) for a minimum of 2 hours just prior to prepara-
tion of standard solution.
3.3.S Standard KNOi Solution. DUsolve exactly
2.1(18 ft of dried potassium nitrate (KNOi) In delonited,
distilled water and dilute to 1 liter with deloruted,
distilled water In a 1,000-rnl volumetric flask.
3.3.6 Working Standard KNOi Solution. Dilute 10
ml of (be standard solution to 100 ml with dtlontud
dlitllled water. One miUJllter of the working standard
solution li equivalent to lOOog nitrogen dloiTde (NOi).
8.3.7 Water. Deionited, distilled as In Section 3.2.2.
3.3.g Phtnoldisulfonlc Add Solution. Dissolve 25 g
of pur* whit* phtnol In 190 ml concentrated lulfuric
acid on a (team bath. Cool, add 7$ ml fuming tuUuric
acid, and heat at 100° C (212° F) for 2 hours. Store in
a dark, stoppered bottle.
4. Praafara
4.1 Sampling.
4.1.1 Pipette 23 ml of absorbing solution into a sample
flask, retaining a sufficient quantity for tise In preparing
the calibration standards. Insert the fistic valve stopper
Into the flask with the valve In the "purge" position.
Assemble the sampling train as shown In Figure 7-1
and place the probe at the sampling point Make sun
that all fittings are tight and leak-tree, and that all
(round glass Joints have been properly greased with a
nigh-vacuum, high-teinperature chiorofluorocaibon-
based stopcock grease. Turn the flask valve and the
pump val»e to their "evacuate" positrons. Evacuate
the flask to 75 mm Hg (3 in. Hg) absolute pressure, or
leas Evacuation to a pressure approaching the vapor
pressure of water at the existing temperature is desirable
Turn the pump valve to its "vent" position and t\im
off the pump. Check for leakage by observing the n;a-
uoraeUr tor any pcassun fluctuation. (Any variation
greater than 10 mm Hg (0.4 in. Hg) over a peri*i of
1 minute to not acceptable, and the Back Is not to be
• used until the leakage problem Is corrected. Pressure
in the flask Is not to exceed 75 mm Hg »in. Hg) absolute
at the time sampling is commenced.) Record the volume
of the flack and valve Wi), the flask temperature (T.),
and toe barometric pressure. Turn the flask valve
counterclockwise to its "purse" position and do the
aame with the pump valve. Purge the probe and the
vacuum tube using the tqueeu bulb. It condensation
occurs in the probe and the flask valve area, beat the
record 'he flask Unpnraturc (7"i), the barometric
pressure, and the difference between the mercury levels
n the manometer. The absolute internal pressure in
the flask (Pi) is the barometric pressure less the man-
ometer reading. Transfer the contents of the flask to a
leak-free polyethylene bottle Rinse the flask twice
with 5-m) portions of deioru'ted, distilled water and add
the rinse water to the bottle. Adjust the pH to between
8 and 12 by adding sodium hydroxide (1 N). dropwise
(about 25 to 35 drops). Check the pH by dipping a
stirring rod into the solution and then touching the rod
to the pH test paper Remove as little material as possible
during this'step. Mark the height c! the iiqu.o level so
that the container can be checked for le&kage after
transport. Label the container to clearly identify its
contents. Seal the container for shipping.
4.3 Analysis. Note the level of the liquid in container
said confirm whether or not any sample was lost during
shipment; note this on the analytical data sheet. If a
noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of
the Administrator, to correct the final results. Immedi-
ately prior to analysis, transfer the contests of the
•hipping container to a 50-znl volumetric flask, and
rinse the container twice with 5-ml portions of deionlted.
distilled water. Add the rinse water to the flask and ..
dilute to the mark with deionieed, distilled water; mix
thoroughly. Pipette a 2S-ml aliquot into the prooelaln
evaporating dish. Return any unused portion of the
•ample to the polyethylene storage bottle. Evaporate
the 26-ml aliquot to dryness on a steam bath and allow
to oool. Add 2 ml phenoldisulfonic acid solution to the
dried residue and triturate thoroughly with a poylethyl-
ane policeman. Make sure the solution contacts all the
residue. Add 1 ml deionited, distilled water and four
drops of concentrated sulfuric acid. Heat the solution
on a tteun hath lor 8 minutes with occasional stirring.
Allow the solution to oool, add 20 ml deionited, distilled
water, mix well by stirring, and add concentrated am-
monium hydroxide, dropwise, with constant stirring,
until the pH Is 10 (as determined by pB paper). 11 the
sample contains solids, these must be removed by
filtration (eentrlfugation is an acceptable alternative,
subject to the approval of the Administrator), as follows:
filler through Whatman No. 41 filter paper Into a 10!>ml
volumetric flask; rinse the evaporating dish with three
4-ml portions cf deioniied, distilled water; filter these
three rinses. Wash the filter with at least three 15-ml
portions of deionited, distilled water. Add the niter
washings to the contents of the volumetric flask and
dilute to the mark with deionited, distilled water 11
solids are absent, the solution can be transferred directly
to the 100-rol volumetric flask and diluted to the mark
with dcioniied. distilled water. Mix the contents of the
flask thoroughly, and measure the absorbance at the
optimum wavelength used for the standards (Section
5.2.1), using the blank Solution as a tero reference- Dilute
the sample and the blank with equal volumes of del on-
Ued, distilled water if the atisorbance exceeds A,, the
absorbance of the 400 MS NOi standard (we Section 5.2 2).
5 CaUbrtttm
8 1 Flask Volume. The volume of the collection fla^
flask valve combination must be known pnor to sam-
pling. Anseroble the fiask and flask valve and fill *it>
water, to the stopcock. Measure the volume of water to
±10 ml Record this volume on the flask.
8.2 Spectrophotometer Calibration.
B.Z.I Optimum Wavelength Determination. For bolt'
filed and variable wavelength spectrophotometers.
calibrate against standard certified wavelength of 410
run, every 6 months. Alternatively, for variable wave
length spectrophotometm. scan the spectrum betweei.
400 and 416 nm using a 500 /ig N Oj standard solution (see
6.5 Vacuum GauRt'. Cahbnjie mechanic*! Kaupes. If
used, against a mercury manometer such as that ei«i-
fiedin2.).». .
5.8 Analytical Balance. Calib-atc against (Kaixiwd
weights.
record the difference in the mercury levels in the manom-
eter. The absolute Internal pressure In the flask (P.)
is equal to the barometric pressure less the manometer
reading. Immediately turn the flask valve to the saw-
pie" posiliO'i and permit the gas to enter the flask until
pressures in the flafk and simple line (I e., duct, stack)
are equal. This -will usually require about 15 seconds;
Carry out the calculations, retaining M Icart one extr*
decimal figure beyond that of the acquirrd data. Round
off figures after final calculations.
6.1 Nomenclature.
X~ Absorbance of sample.
C—Concentration of NO. as NOi, c!-y basis, cor-
rected to standard condition*, ms/dtcm
Ob/dscD.
/•-Dilution factor (1 e , 25/5, 25/10, etc., required
only If sample dilution was nwied to rtiduw
the absorbance into the range of calibration).
KV-Spertrophotometer calibration tartar.
«i-HsssofNO.asNOiin|»ssaiBp;e. «r. .
f>/- Final absolute prwaure of flask, mm Hg tin . He) .
/"(-Initial absolute pressure of flask, mui Hj (In.
P.U, -Standard absolute pressure, 760 red Hg (29 92 in
Hj).
TV-Final absolute temperature of flask ,"K f°R)
T(-lnit!al absolute temperature of flask. °K C R).
Tat- Standard absolute temperature, 293° K (5?S° R)
V'., -Sample volume at standard conditions (dry
basis), ml.
V/— Volume of flask and valve, ml.
V.-Volume of absorbing solution, 25 ml.
2-80/2S, the aliquot toctor. (II other than a 24-m!
aliquot wait used for analyst, the correspond-
ing factor must be substituted/.
4.2 Sample volume, dry basis, eon-ncted to standard
renditions.
position and disconnect the flask from the sampling
train. Shake the flask for at least 5 minutes.
41.2 If the gas being sampled contains Insufficient
oxygen for the conversion of NO to NOi (e.g, an ap-
plicable subpart of the. standard ma; require taking a
sample of a calibration gas mixture of NO In Ni), then
oxygen shall be introduced into the flask to permit this
conve'sion. Oxygen may be Introduced Into the flask
by one of three methods; (1) Before evacuating th»
sampling flask, flush with pure cylinder oxygen, then
evacuate flask to 75 mm Hg (3 in. Hg) absolute pressure
or less; or (2) inject oxygen into the flask after samplinf.
or (3) terminate samphng with a minimum of 50 mm
HB (2 in. Hg) vacuum remaining In the flask, record
tins (Ins.! pressure, and then vent the flask to the ai-
mosnhere until the flask pressure is almost equal tc
atmospheric pressure
< 2 Sample Recovery. l>et the flask set for ajninimum
of 18 honre antl then shake the contents for 2 minutes
Gormen the flusk to B mercury filled U-tubemanometei
Or>.n tin valve fron Ihf nark to the manometc! anJ
J+Aj
Equation 7-1
where:
ATt« Calibration factor
A\~Absorbance of the lOO-vg NO: standard
>4:-Absorbance of the 20O«g NOj standard
y4j- Absorbance of the 3no-i* NO) standard
X4-Absorbance cf the 400i* v"rv. Fto—<»'H
5.3 Barometer. Calibrate apsinst a mercury bxin •
eter.
54 Temperature Oauc" Calmraw dmltlierni"r «
against mercury-m-filtts-s thermometers.
-K,(V,-
Equation Y-2
for metric units
where:
A',--0.3858
= 17.64 .- 7, for English units
in. ng
C.3 Total pg NOi per sample.
Equation 7-3
otE.— If other than a 25-ml aliquot is used for arc aly •
sis, the factor 2 must be replaced by a oorrespondli.g
factor.
6.4 Sample concentration, dry basis, corrected to
standard conditions.
C-K,
m
ff-
'««
Equation 7-4
where:
range, the wavelength at which this peak occurs shall be
the optimum wavelength for the measurement of ar>
sorbance for both the standards and samples.
822 Determination of Bpcctrophotometer Calibra-
tion Factor K,. Add 0.0. 1.0. 2.0, 3 0. and 4.0 ml of the
KNOi working standard solution (1 rol-100 *s NO;) to
a series of five porcelain evaporating; dishes. To each, add
25 ml of absorbing solution, 10 ml deionited, oistw»a
waier, and sodium hydroxide (IN), dropwise, until tne
pH Is between 9 and 12 (about 25 to 35 drops eac>-)
JBepinninR with the evaporation step, follow the anai>-
sls procedure of Section 4 3, until the solution has Iwn
transferred to the 100 ml volumetric flask and diluted to
the mark Measure the absorbance of each solution, at the
optimum wavelength, as determined in Section 62).
This calibration procedure must be repeated on each day
that samples are anatyifd. Calculate the spectrophotom-
eter calibration factor as follows
K. = 100
for metric units
B10»
-6.243X10-* - for English unit*
7. BMiofrtphy
1. Standard Methods of Chemical Analysis. Mh ed.
New York, D. Vna Nostrand Co., Inc. 1662. Vol. 1.
P2. Standard Method of Test for Oxides of Nitrpp.en in
Gaseous Combustion Products (Phenold'^jHoni'- Ar.4
Procedure). In: 1968 Book of ABTM Standi.-ds, Fort V'.
Philadelphia, Pa. 1968. ASTM Designation D-lCtvW.
P 1 Jacob M. B. The Chemical Analysis of Air IV.lut-
ants New York. Interscience Publishers, Inc. !900.
Vol. 10, p. S51-354. ,
4. Beatty, R. L., L. B. Berber, and H. H. Echrenk.
Determination of Oxides of Nitrogen by the Phe noldistu-
fonic Acid Method. Bureau of Mines, U S. Dcpt. of
Interior. R. 1. 3fiS7. February 1943.
5 Hamil, H. F. and D. E. Camann. CoilaVorat'vc
Study of Method tor the Determination o! Kit-opvn
Oxide. Emissions from Stationary Sources Oossil Fi:i'l-
Fired Steam Generators). Southwest Research liirtnn'.ft
report for Environmental Protection Agency. lUscarch
Tmnfle Park, N.C. October 5, 19Ti».
6 Hamil, H. F. and R. E. Thomas Colta^n,tiic
Study of Method for the Drtcraiijmtion of Nitwri
Oxide Emissions from Stationary Sources (Nitr)'' f.<^n
Plants). Southwest Research Institute report m r.'i-
vlronniental Protection Agency. Fey-arch Triani'lc
ParV, N C. Msy 8, JB74.
-------
Amendments to Reference Method 8; Correction*
In Method 7 of Appendix A, Section*
Section No. 3.6.10
Revision No. 0
Date May 1, 1979
Page 3 of 3
2.3.2, 2.3.7, 4.2, 4.3, 5.2.1. 6.2.2, 6 and 7
are amended as follows:
1. In Section 2.3.2, a semicolon re-
places the comma between the words
"step" and "the."
2. In Section 2.3.7, the phrase "(one
for each sample)" In the first line is
corrected to read "(one for each
sample and each standard)."
3. In Section 4.2. the letter "n" In
the seventh line Is corrected to read
"in."
4. In Section 4.3, the word "poyleth-
ylene" in the seventeenth line is cor-
rected to read "polyethylene."
5. In Section 5.2.1, delete the entire
section and insert the following:
Optimum Wavelength Determination.
Calibrate the wavelength scale o! the spec-
trophotometer every 6 months. The calibra-
tion may be accomplished by using an
energy source with an Intense line emission
such as a mercury lamp, or by using a series
of glass filters spanning the measuring
range of the spectrophotometer. Calibration
materials are available commercially' and
from the National Bureau of Standards.
Specific details on the use of such materials
should be supplied by the vendor; general
Information about calibration techniques
•can be obtained from general reference
books on analytical chemistry. The wave-
length scale of the spectrophotometer must
read correctly within ± 5 nm at all calibra-
tion points; otherwise, the spectrophoto-
meter shall be repaired and recalibrated.
Once the wavelength scale of the spectro-
photometer Is in proper calibration, use 410
nm as the optimum wavelength for the mea-
surement of the absorbance of the stan-
dards and samples.
Alternatively, a scanning procedure may
be employed to determine the proper mea-
suring wavelength. If the instrument Is a
double-beam spectrophotometer, scan the
spectrum between 400-and- 415 nm using a
200 ng NO, standard solution in the sample
'cell and a blank solution in the reference
cell. If a peak does not occur, the spectro-
photometer is probably malfunctioning and
should be repaired. When a peak is obtained
within the 400 to 415 nm range, the wave-
length at which this peak occurs shall be
the optimum wavelength for the measure-
ment of absorbance of both the standards
and the samples. For a single-beam spectro-
photometer, follow the scanning procedure
described above, except that the blank and
standard solutions shall be scanned sepa-
rately. The optimum wavelength shall be
the- wavelength at which the maximum dif-
ference in absorbance between the standard
and the blank occurs.
6. In Section 5.2.2, delete the first
seven lines and insert the following:
Determination of Spectrophotometer
Calibration Factor K_ Add 0.0 ml, 2 ml, 4
ml, 6 ml, and 8 ml of the KNO, working
standard solution (1 ml=100 us NO,) to a
series of five 50-ml volumetric flasks. To
each flask, add 25 ml of absorbing solution.
10 ml delonized, distilled water, and sodium
hydroxide (IN) dropwice until the pH is be-
tween 9 and 12 (about 25 to 35 drops each).
Dilute to the nark with deioniced, dlitllled
water. Mix thoroughly and 'pipette a 25-ml
aliquot of each solution Into a separate por-
celain evaporating dish.
7. In Section 6.1. the word "Haas" in
the tenth line is corrected to read
"Mass."
8. In Section 7. the word "Vna" in
(1) is corrected to read "Van." The
word "drtermination" in (6) is correct-
ed to read "Determination."
*Federal Register, Vol. 43, llo. 57-March 23, 1978
-------
Section No. 3.6.11
Revision No. 0
Date May 1, 1979
Page 1 of 2
11.0 REFERENCES
1. Quality Assurance Handbook for Air Pollution Measure-
ment Systems, Volume I - Principles. U.S. Environmen-
tal Protection Agency, Office of Research and Develop-
ment, Environmental Monitoring and Support Laboratory,
Research Triangle Park, N.C. EPA-600/9-76-005, March
1976.
2. Buchanan, J. W. and D. E. Wagoner. Guidelines for
Development of a Quality Assurance Program, Determina-
tion of Nitrogen Oxide Emissions from Stationary
Sources. EPA.
3. Hamil, Henry F. et. al. The Collaborative Study of EPA
Methods 5, 6, and 7 in Fossil Fuel Fired Steam Genera-
tors. Final Report, EPA-650/4-74-013, May 1974.
4. Hamil, H. F., and R. E. Thomas. Collaborative Study of
Method for the Determination of Nitrogen Oxide Emis-
sions from Stationary Sources (Nitric Acid Plants),
EPA-650/4074-028, May 1974.
5. Hamil, Henry F. Laboratory and Field Evaluations of
EPA Methods 2, 6, and 7. Final Report, EPA Contract
No. 68-02-0626. Southwest Research Institute, San
Antonio, Tex., October 1973.
6. Standard Methods of Chemical Analysis, 6th Edition. D.
Van Nostrand Co., Inc., N.Y., 1962. Vol. 1, pp.
329-330.
7. Standard Method of Test for Oxides of Nitrogen in
Gaseous Combustion Products (Phenoldisulfonic Acid
Procedure) In: 1968 Book of ASTM Standards, Part 26.
Philadelphia, Pa. 1968. ASTM Designation D-1608-60,
pp. 725-729.
8. Jacob, M. B. The Chemical Analysis of Air Pollutants.
Interscience Publishers, Inc., N.Y., 1960. Vol. 10,
pp. 351-356.
9. Beatty, R. L., L. B. Berger, and H. H. Schrenk. Deter-
mination of Oxides of Nitrogen by the Phenoldisulfonic
Acid Method. Bureau of Mines, U.S. Department of
Interior, R.I. 3687. February 1943.
-------
Section No. 3 .6.11
Revision No. 0
Date May 1, 1979
Page 2 of 2
10. Hamil, H. F. and D. E. Camann. Collaborative Study of
Methods for the Determination of Nitrogen Oxide Emis-
sions from Stationary Sources (Fossil Fuel Fired Steam
Generators). Southwest Research Institute report for
EPA, Research Triangle Park, N.C. October 5, 1973.
11. Hamil, H. F. and R. E. Thomas. Collaborative Study of
Methods for the Determination of Nitrogen Oxide Emis-
sions from Stationary Sources (Nitric Acid Plants).
Southwest Research Institute report for EPA, Research
Triangle Park, N.C. May 8, 1974.
12. Fuerst, R. G., R. L. Denny, and M. R. Midgett. A
Summary of Interlaboratory Source Performance Surveys
for EPA Reference Methods 6 and 7-1977. Available from
U.S. Environmental Protection Agency, Environmental
Monitoring and Support Laboratory (MD-77), Research
Triangle Park, N.C. 27711.
13. Fuerst, R. G. and M. R. Midgett. A Summary of Inter-
laboratory Source Performance Surveys for EPA Reference
Methods 6 and 7-1978. Report in preparation by U.S.
Environmental Protection Agency, Environmental
Monitoring and Support Laboratory (MD-77), Research
Triangle Park, North Carolina 27711.
-------
Section No. 3.6.12
Revision No. 0
Date May 1, 1979
Page 1 of 13
12.0 DATA FORMS
Blank data forms are provided on the following pages for the
convenience of the Handbook user. Each blank form has the cus-
tomary descriptive title centered at the top of the page. How-
ever, the section-page documentation in the top right-hand corner
of each page has been replaced with a number in the lower right-
hand corner that will enable the user to identify and refer to a
similar filled-in form in a text section. For example, Form
M7-1.2, indicates that the form is Figure 1.2 in Section 3.6.1 of
the Method 7 Handbook. Future revisions of these forms, if any,
can be documented by 1.2A, 1.2B, etc. Twelve of the blank
forms listed below are included in this section. Four are in the
Method Highlights subsection as shown by the MH following the
form number,
Form Title
1.2 Procurement log
2.1 Optimum Wavelength Determination Data Form
2.2 Analytical Balance Calibration Form
3.1 (MH) Pretest Checklist
3.2 (MH) Pretest Preparations
4.1A and 4.IB Nitrogen Oxide Field Data Form
(English and metric units)
4.2A and 4.2B NO Sample Recovery and Integrity Data Form
(English and metric units)
4.3 (MH) On-site Measurements
5.1 Standard Solution and Control Sample
Analytical Data Form
5.2 NO Laboratory Data Form
X
5.3 (MH) Posttest Operations
6.1A and 6.IB Nitrogen Oxide Calculation Form
(English and metric units)
8.1 Method 7 Checklist to be Used by Auditors
-------
PROCUREMENT LOG
Item description
Qty.
Purchase
order
number
Vendor
Date
Ord.
Rec.
Cost
Dispo-
sition
Comments
Quality Assurance Handbook M7-1.2
-------
OPTIMUM WAVELENGTH DETERMINATION DATA FORM
Spectrophotometer number
Calibrated by
Date
Reviewed by
Spectrophotometer
setting, nm
399
400
401
402
403
404
405
406
407
408
409
410
411
412
413
414
415
416
Absorbance
of standard
ODa
Absorbance
of blank
ODb
Actual
absorbance of
ODC
Absorbance of the 200 yg N02 standard in a single beam
spectrophotometer.
Absorbance of the blank in a single-beam spectrophoto-
meter .
c
For a single-beam spectrophotometer— absorbance of the
standard minus absorbance of the blank. For a double
beam spectrophotometer—absorbance of the 200 yg NO2
standard with the blank in the reference cell.
Spectrophotometer setting for maximum actual absorbance
of standard _ nm.
If the maximum actual absorbance occurs at a spectrophotometer
setting of £399 or M16 nm, the spectrophotometer must be
repaired or recalibrated.
Quality Assurance Handbook M7-2.1
-------
ANALYTICAL BALANCE CALIBRATION FORM
Balance name Number
Classification of standard weights
Date
0.5000 g
1.0000 g
10.000 g
50.0000 g
100.0000 g
Analyst
Quality Assurance Handbook M7-2.2
-------
NITROGEN OXIDE FIELD DATA FORM
(English units)
Plant
Sample location
Operator
City
Date
Barometric pressure (P, )
in. Hg
Sample
number
Sample
point
location
Sample
time
24-hr
Probe
temperature,
Flask
and valve
number
Volume
of flask
and valve (V^) ,
ml F
Initial pressure
in. Hg
Leg A±
Leg B.j^
V
Initial temperature
°F (t.)
°R (T.)b
Pi = Pbar - (Ai
b T± = t± + 460°F.
Quality Assurance Handbook M7-4.1A
-------
NITROGEN OXIDE FIELD DATA FORM
(metric units)
Plant
Sample location
Operator
City
Date
Barometric pressure (P, )
mm Hg
Sample
number
Sample
point
location
Sample
time
24-hr
Probe
temperature,
Flask
and valve
number
Volume
of flask
and valve (V ) ,
ml F
Initial pressure
mm Hg
Leg A±
Leg B±
>ia
Initial temperature
°C (t±)
°K (Tt)b
Pi - Pbar
V •
273°C .
Quality Assurance Handbook M7-4.1B
-------
Plant
NO SAMPLE RECOVERY AND INTEGRITY DATA FORM
x (English units)
Date
Sample recovery personnel
Barometric pressure, (P, )
in. Hg
Person with direct responsibility for recovered samples
Sample
number
Final pressure,
in. Hg
Leg Af
Leg Bf
V
Final temperature,
°F (tf)
°R (Tf)b
Sample
recovery
time,
24-h
PH
adjusted
9 to 12
Liquid
level
marked
Samples
stored
in locked
container
P.- = P, - (A,; + B.) .
f bar f f
Tf = t£
460°F
Lab person with direct responsibility for recovered samples
Date recovered samples received Analyst
All samples identifiable?
Remarks
Signature of lab sample trustee _
All liquids at marked level ?_
Quality Assurance Handbook M7-4.2A
-------
NO SAMPLE RECOVERY AND INTEGRITY DATA FORM
x (metric units)
Plant
Date
Sample recovery personnel
Barometric pressure, (P, )
mm Hg
Person with direct responsibility for recovered samples
Sample
number
Final pressure,
mm Hg
Leg Af
Leg Bf
Pf
Final temperature,
°C (tf)
K (Tf)
Sample
recovery
time,
24-hr
PH
adjusted
9 to 12
Liquid
level
marked
Samples
stored
in locked
container
Pf = Pbar - (Af
B
Tf = tf + 273 C.
Lab person with direct responsibility for recovered samples
Date recovered samples received Analyst
All samples identifiable?^
Remarks
Signature of lab sample trustee __
All liquids at marked level?_
Quality Assurance Handbook M7-4.2B
-------
STANDARD SOLUTION AND CONTROL SAMPLE
ANALYTICAL DATA FORM
Plant
Date
Analyst
Optimum wavelength
Blank used as reference?
nm
Sample
number
Al
A2
A3
A4
SI
S2
S3
Sample,
Pg
100
200
300
400
100
200
300
Working
solution
X
X
X
X
Control
sample
X
X
X
Measured,
absorbance,
OD
Calculated
a
absorbance,
OD
-
-
-
-
Absorbance
comparison
error, %
-.
-
-
—
Avg
K = 100
c
2 2 2
A2 + A3 + A4
Calculated absorbance: OD = ((Jg)/K i.e., SI calculated absorbance = 100/K
Absorbance comparison errors:
_
~
(measured absorbance, OD) - (calculated absorbance, OD).
calculated absorbance, OD
f*
Average of absolute values.
Quality Assurance Handbook M7-5.1
-------
NO LABORATORY DATA FORM
Plant
Date samples received
Aliquot factor
Run number(s)
Date analyzed
Blank absorbance
Calibration factor (K )
c
Samples analyzed by
Date reviewed by
Date of review
Sample
number
Sample
absorbance,
A
Dilution
factor,
F
Total mass of N0x
as N0» in sample,
z m
m = 2 K AF, Note: If other than a 25 ml aliquot is used for
analysis, the factor 2 must be replaced by a corresponding
factor.
Quality Assurance Handbook M7-5.2
-------
NITROGEN OXIDE CALCULATION FORM
(English units)
Sample Volume
Vf =
Pi "
ml,
. in. Eg, Tf = ___
„_ _ „_ ^
R
__. in. Hg, T. = . R
P.C P
V
sc
17.64 (Vf - 25)
Tf T±
= ml Equation 6.1
K
c —
Total yg N02 Per Sample
., A = _. OD, F = . Equation 6.2
m = 2K AF = . yg of N0
— — — —-
Sample Concentration
C = 6.243 x 10
-5 F m
V.
sc
x 10~5 Ib/dscf
Quality Assurance Handbook M7-6.1A
-------
NITROGEN OXIDE CALCULATION FORM
(metric units)
Sample Volume
. ml, Pf = mm Hg, T^ = K
I. —" "™" *"~ —~ 3- ~~ "~ *"" "~
P. =
mm Hg, T.
— _« M». — ^
= 0.3858 (Vf - 25)
K
. ml Equation 6-1
K — _ _
m = 2K AF =
c
Total yg N02 Per Sample
OD, F =
yg of N0~<
Equation 6-2
Sample Concentration
C = 1(T
[e-l
x 10 mg/dscf. Equation 6-3
Quality Assurance Handbook M7-6.1B
-------
METHOD 7 CHECKLIST TO BE USED BY AUDITORS
Presampling Preparation
Yes No
1. Information concerning combustion effluents that may
act as interferents
2. Plant operation parameters variation
3. Calibration of the flask and valve volume
three determinations
4. Absorbing reagent preparation
On-site Measurements
5. Leak testing of the sampling train
6. Preparation and pipetting of absorbing solution
into sampling flask
Postsampling
(Analysis and Calculation)
7. Control sample analysis
8. Sample aliquotting technique
9. Evaporation and chemical treatment of sample
10. Spectrophotometric technique
a. Preparation of standard nitrate samples
b. Measurement of absorbance, including blanks
c. Calibration factor
d. Wavelength and absorbance, including blanks
11. Calculation procedure and checks
a. Use of computer program
b. Independent check of calculations
Comments
Quality Assurance Handbook M7-8.1
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 1 of 13
Section 3.7
METHOD 8—DETERMINATION OF SULFURIC ACID MIST
AND SULFUR DIOXIDE EMISSIONS FROM STATIONARY SOURCES
OUTLINE
Number
Section Documentation of Pages
SUMMARY 3 ^ 7 2
METHOD HIGHLIGHTS 3.7 1Q
METHOD DESCRIPTION
1. PROCUREMENT OF APPARATUS 371 n
AND SUPPLIES
2. CALIBRATION OF APPARATUS 3.7.2 20
3. PRESAMPLING OPERATIONS 3.7.3 7
4. ON-SITE MEASUREMENTS 3.7.4 18
5. POSTSAMPLING OPERATIONS 3.7.5 17
6. CALCULATIONS 3.7.6 10
7. MAINTENANCE 3.7.7 3
8. AUDITING PROCEDURE 3.7.8 7
9. RECOMMENDED STANDARDS 379 i
FOR ESTABLISHING
TRACEABILITY
10. REFERENCE METHOD 3.7.10 4
11. REFERENCES 3.7.11 i
12. DATA FORMS 3.7.12 20
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 2 of 13
SUMMARY
A gas sample is extracted isokinetically from the stack.
The sulfuric acid mist (including sulfur trioxide, or SO,.) and
the SO~ are separated, and both fractions are measured separ-
ately by the barium-thorin titration method. The barium ions
react preferentially with sulfate ions in solution to form a
highly insoluble barium sulfate precipitate. When the barium
has reacted with all sulfate ions, the excess barium reacts
with the thorin indicator to form a metal salt of the
indicator and to give a color change.
This method is applicable for the determination of
sulfuric acid mist (including SO_) emissions from stationary
sources. Collaborative tests have shown that the minimum
detectable limits of the method are 0.05 mg SO^/m (0.03 x
10~7 lb/ft3) and 1.2 mg S02/m3 (0.74 x lo"7 lb/ft ). No upper
limits have been established. Based on theoretical calcula-
tions for 200 ml of 3% hydrogen peroxide solution, the upper
3 3
concentration limit in a 1.0 m (35.3 ft ) gas sample is about
12,500 mg SC>2/m3 (7.7 x lo"4 lb/ft3). The upper limit can be
extended by increasing the quantity of peroxide solution in
the impingers.
Possible interferences with this method are fluorides,
free ammonia, and dimethyl aniline. If any of these interfer-
ents are present (as determined by knowledge of the process),
alternative methods subject to the approval of the
administrator, U.S. Environmental Protection Agency, are
required. For example, if free ammonia is present, white
particulates can be seen in the probe and in the isopropanol
impinger.
Filterable particulate matter may be determined along
with SO and SO2 (subject to the approval of the administra-
tor); however, the procedure used for particulate matter must
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 3 of 13
be consistent with the specifications and procedures given in
Method 5.
The Method 8 description which follows is based on the
Reference Method that was promulgated on August 18, 1977. A
complete copy of the Reference Method is in Section 3.7.10.
Data forms are provided in Subsection 12 for the convenience
of the Handbook user.
Reference 1 was used extensively in preparing the method
description. References 2 and 3 are the collaborative test
studies of this method and other related methods; data from
these test studies were used in establishing quality control
limits. References 4 and 5 were used extensively in those
sections which include the description, calibration, and
maintenance of the sampling train. All references are listed
in Section 3.7.11.
A collaborative test program was conducted at a sulfuric
acid (H-S04) plant to determine the accuracy of Method 8. Six
laboratories simultaneously sampled the same stack, using two
Method 8 sampling trains per laboratory. The collaborative
test determined that the repeatability (within-laboratory
3
precision) of the method was 7.19 mg H9SO,/m and 22.30 mg
3 £ *
SO /m and that reproducibility (between-laboratory precision)
of the method was 8.03 mg H2SO4/m3 and 31.10 mg SO2/m3.6
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 4 of 13
METHOD HIGHLIGHTS
Specifications described in Section 3.7 are for
sampling and analysis of sulfuric acid mist (including
sulfur trioxide) and sulfur dioxide emissions from
stationary sources. The sampling system consists of the EPA
Method 5 sampling train modified by placing the filter
(unheated) between the first and second impingers.
Filterable particulate matter may be determined along with
S03 and S02 (subject to the approval of the administrator);
however, the procedure used for particulate matter must be
consistent with the specifications and procedures given in
Method 5.
The results of collaborative tests have shown that the
overall precision of the test method is good if sound
quality assurance procedures are applied. On the basis of
these results these procedures are recommended:
1. On-site checks of the orifice and dry gas meter
calibration coefficients of all control consoles with a dry
gas meter that has been calibrated with a spirometer.
2. Certification that all reagent isopropyl alcohol
is peroxide-free prior to the test.
3. Leak checks are performed at the beginning and at
the end of each sampling run before and after every port
change. Care should be taken to be sure that the sulfur
dioxide absorbing reagent, hydrogen peroxide, does not
contact the filter when the leak check is conducted; if
peroxide does contact the filter, the filter should be
replaced before sampling is continued.
The five blank data forms at the end of the highlights
may be removed from the Handbook and used in the pretest,
test, and posttest operations. Each form has a subtitle
(e.g., Method 8, Figure 3.1) for helping the user find a
similar filled-in form in the method description (e.g., in
Section 3.7.3). On the blank and filled-in forms, the
items/parameters that can cause the most significant errors
are starred.
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 5 of 13
I. Procurement of Equipment
Section 3.7.1 (Procurement of Apparatus and Supplies)
4
gives the specifications, criteria, and design features for
equipment and materials required for performing Method 8
tests. The sampling apparatus has the same design criteria as
Method 5, with the exception of the filter-impinger
arrangement. This section is designed as a guide in the
procurement and initial check of equipment and supplies. The
activity matrix (Table 1.1) at the end of Section 3.7.1 can be
used as a quick reference; it follows the same order as the
written descriptions in the main text.
2. Pretest Preparations
Section 3.7.2 (Calibration of Apparatus) provides a
step-by-step description of the required calibration
procedures. The calibration of the Method 8 equipment is
similar to that of Method 5, with the exception that the
Method 8 sampling rate is not to exceed 28.3 £/min (1 scfm),
and the stack thermometer need not be calibrated at the higher
temperatures if the equipment is used to measure acid plant
emissions only. The calibration section can be removed and
compiled, along with calibration sections from all other
methods, into a separate quality assurance reference manual
for use by calibration personnel. A pretest checklist
(Figure 2.5 of Section 3.7.2) or similar form should be used to
summarize the calibration data.
Section 3.7.3 (Presampling Operations) provides the
tester with a guide for supplies and equipment preparation for
field tests. Sample impingers may be charged in the base
laboratory if testing is to be performed within 24 h of
charging. The pretest preparation form (Figure 3.1 of Section
3.7.3) can be used as an equipment checkout and packing list.
The method for packing and the descriptions of the packing
containers should help protect the equipment, but are not
required.
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 6 of 13
3. On-Site Measurements
Section 3.7.4 (On-Site Measurements) contains a
step-by-step procedure for performing sampling and sample
recovery. Testing is performed isokinetically and similarly
to Method 5, with the exception that the sample rate is not to
3
exceed 1 ft /mm. The most common error results when hydrogen
peroxide solution is allowed to backup, wet the filter, and
enter the isopropanol impinger. Also precautions must be
taken to ensure that the isopropanol does not have hydrogen
peroxide impurities and that the same pipette or graduated
cylinder is not used to charge both isopropanol and hydrogen
peroxide. The on-site measurement checklist (Figure 4.4 of
Section 3.7.4) is provided to assist the tester with a quick
method of checking requirements.
4. Posttest Operations
Section 3.7.5 (Postsampling Operations) gives the post-
test equipment check procedures and a step-by-step analytical
procedure. Figure 5.1 (Section 3.7.5) or a similar form
should be used to summarize the posttest calibration checks
and should be included in the emission test report. The
posttest operation form (Figure 5.4 of Section 3.7.5) will
provide the tester and laboratory personnel with key parame-
ters to be checked. The step-by-step analytical procedure de-
scription can be removed and made into a separate quality as-
surance analytical reference manual for laboratory personnel.
Analysis of a control sample is required prior to the analysis
of the field samples. This analysis of an independently pre-
pared known standard will provide the laboratory with a qual-
ity control check on the accuracy and precision of the analyt-
ical techniques.
Section 3.7.6 (Calculations) provides the tester with the
required equations, the nomenclature, and the suggested number
of significant digits. It is suggested that a programmed
calculator be used if available to reduce the chance of
calculation error.
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 7 of 13
Section 3.7.7 (Maintenance) provides the tester with a
guide for a routine maintenance program. This program is not
required, but should reduce equipment malfunctions.
5. Auditing Procedure
Section 3.7.8 (Auditing Procedure) provides a
description of necessary activities for conducting performance
and system audits. The performance audit of the analytical
phase can be conducted using an aqueous ammonium sulfate
solution. Performance audits for the analytical phase and the
data processing are described in Section 3.7.8. A checklist
for a systems audit is also included in this section.
Section 3.7.9 (Recommended Standards for Establishing
Traceability) recommends the primary standards to which the
working standards should be traceable.
6. References
Sections 3.7.10 and 3.7.11 contain the Reference Method
and the suggested references.
-------
PRETEST SAMPLING CHECKS
(Method 8, Figure 2.5)
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 8 of 13
Date
Meter box number
Calibrated by
AH@
Dry Gas Meter*
Pretest calibration factor =
factor for each calibration run).
Impinger Thermometer
(within ±2% of the average
res
no.
Was a pretest temperature correction used?
If yes, temperature correction (within ±1°C (2°F) of re-
ference values for calibration and within ±2°C (4°F) of re-
ference values for calibration check).
Dry Gas Meter Thermometer
Was a pretest temperature correction made? yes no.
If yes, temperature correction (within ±3°C (5.4°F) of re-
ference values for calibration and 6°C (10.8°F) of reference
values for calibration check).
Barometer -
Was the pretest field barometer reading correct? yes no
(within ±2.5 mm (0.1 in) Hg of mercury-in-glass barometer).
Most significant items/parameters to be checked.
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 9 of 13
PRETEST PREPARATIONS
(Method 8, Figure 3.1)
Apparatus check
Probe
Type glass liner
Borosilicate
Quartz
Heated
Leak checked
Nozzle
Glass
Stainless steel
Other
Pitot Tube
Types
Other
Properly at-
tached
Modifications
c_
P
Differential
Pressure Gauge
Inclined manome-
ter
Other
Filter Holder
Borosilicate glass
Glass frit
Gasket
Silicone
Teflon
Viton
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Loaded
and packed
(continued)
-------
Section No. 3,7
Revision No. 0
Date May 1, 1979
Page 10 of 13
Apparatus check
Condenser
Impingers
Gr eenburg- Smi th
Modified Green-
burg-Smith
Impinger Temper-
ature Sensor
Thermometer
Other
Calibrated
Other
Barometer
Mercury
Aneroid
Other
Calibrated*
Stack Temperature
Sensor
Type
Calibrated*
Reagents
Distilled water
Hydrogen perox-
ide (30%)
Isopropanol (80%)
(checked for
peroxides)
Silica gel
Meter System
Pump leak free*
Orifice meter*
Dry gas meter*
Acceptable
Yes
No
Quantity
required
Ready
Yes
No
Loaded
and packed
Most significant items/parameters to be checked.
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 11 of 13
ON-SITE MEASUREMENTS
(Method 8, Figure 4.4)
Sampling
Impingers properly assembled?
Contents:* 1st
2nd
3rd
4th
Cooling system
Filter between 1st and 2nd impinger?
Proper connections?
Silicone grease added to all ground-glass joints?
Pretest leak check? (optional) Leakage?
Pitot tube lines checked for plugging or leaks?*
Meter box leveled? Periodically?
Manometers zeroed?*
Heat uniform along length of probe?*
AH@ from most recent calibration
Nomograph set up properly?
Care taken to avoid scraping sample port or stack wall?
Seal around in-stack probe effective?
Probe moved at proper time?
Nozzle and Pitot tube parallel to stack wall at all times?
Data forms complete and data properly recorded? ~
Nomograph setting changed when stack temperature changes
significantly?
Velocity pressures and orifice pressure readings recorded
accurately?
Posttest leak check performed?* (mandatory)
Leakage rate*
Sampling Recovery
System purged at least 15 min at test sampling rate?*
Filter placed in 1st impinger contents?
Ice removed before purging?
Contents of impingers placed in polyethylene bottles?
Glassware rinsed with distilled water?
Fluid level marked?*
Sample containers sealed and identified?*
Blanks obtained?*
* Most significant items/parameters to be checked.
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 12 of 13
POSTTEST SAMPLING CHECKS
(Method 8, Figure 5.1)
Meter Box Number
Dry Gas Meter
Pretest calibration factor Y =
Posttest check Y = Y = (+5% of pretest factor)*
Recalibration required? yes no
If yes, recalibration factor Y = (within +2% of average)
Lower calibration factor, Y = for pretest or posttest
calculations
Dry Gas Meter Thermometer
Was a pretest meter temperature correction used? yes no
If yes, temperature correction
Posttest comparison with mercury-in-glass thermometer
(within +6°C (10.8°F) of reference values)
Recalibration required? yes no
Recalibration temperature correction, if used (within +3°C
(5.4°F) of reference values)
If yes, no correction is needed whenever meter thermometer
temperature is higher
If recalibration temperature is higher, add correction to
average meter temperature for calculations
Barometer
Was pretest field barometer reading correct? yes no
Posttest comparison mm (in.) Hg (within ±5.0 mm (0.2 in.)
Hg of mercury-in-glass barometer)
Was recalibration required? yes no
If yes, no correction is needed whenever the field barometer
has the lower reading
If the mercury-in-glass reading is lower, subtract the dif-
ference from the field data readings for the calculations
*Most significant items/parameters to be checked.
-------
Section No. 3.7
Revision No. 0
Date May 1, 1979
Page 13 of 13
POSTTEST OPERATIONS
(Method 8, Figure 5.4)
Reagents
Normality of sulfuric acid standard*
Date of purchase Date standardized
Normality of barium perchlorate titrant*
Date standardized
Normality of control sample*
Date prepared
Volume of burette* Graduations
Sample Preparation
Has liquid level noticeably changed?
Original volume Corrected volume
Sulfuric acid samples diluted to 250 ml?*
Sulfur dioxide samples diluted to 1000 ml?*
Analysis
Aliquot analyzed*
Do replicate titrant volumes agree within 1% or 0.2 ml?
Number of control samples analyzed
Are replicate control samples within 0.2 ml?
Is accuracy of control sample analysis +10%?*
All data recorded? Reviewed
*
Most significant items/parameters to be checked.
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 1 of 13
1.0 PROCUREMENT OF APPARATUS AND SUPPLIES
A schematic of the sampling train used in Method 8 is
shown in Figure 1.1. It is similar to the Method 5 train, but
the filter position is different and the filter holder does
not have to be heated. Commercial models of this train are
available. For those who desire to build their own, complete
construction details are described in APTD-0581. Changes
from the APTD-0581 document and allowable modifications to
Figure 1.1 are discussed in the following subsections.
The operating and maintenance procedures for the sampling
train are described in APTD-0576. Since correct usage is
important in obtaining valid results, all users should read
the APTD-0576 document and adopt the operating and maintenance
procedures therein, unless otherwise specified. Further
details and guidelines on operation and maintenance in Method
5 should be read and followed whenever they are applicable.
Maintenance of equipment is also covered in Section 3.7.7.
Specifications, criteria, and/or design features as
applicable, are given in this section to aid in the selection
of equipment to ensure the collection of data of good quality.
Procedures and, where applicable, limits for acceptance checks
are given. During the procurement of equipment and supplies,
it is suggested that a procurement log (Figure 1.2) be used to
record the descriptive title of the equipment; the
identification number, if applicable; and the results of
acceptance checks. Also, if calibration is required as part
of the acceptance check, the data are to be recorded in the
calibration log book. Table 1.1 at the end of this section
contains a summary of the quality assurance activities for
procurement and acceptance of apparatus and supplies.
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 2 of 13
X
TEMPERATURE SENSOR
PROBE
PROBE
V- PITOTTUBE
TEMPERATURE SENSOR
THERMOMETER
FILTER HOLDER
CHECK
VALVE
7
REVERSE TYPE
PITOT TUBE
VACUUM
LINE
VACUUM
GAUGE
ORIFICE-INCLINED
MANOMETER
MAIN VALVE
DRY TEST METER
Figure 1.1. Schematic of Method 8 sampling train.
-------
Item description
to/ Rber- Vft»e-
Qty.
Purchase
order
number
77A2S
Vendor
AftC
Date
Ord. Rec
Cost
»5,ooo
Dispo-
sition
Comments
*n o» en
P> 0) CD (0
iQ ft < O
0> (D H-ft
TO K-
W S H-O
(D O 3
o *: 3
U)
Figure 1.2. Example of a procurement log.
> O
vo o
-J -
vo .
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 4 of 13
Determination of filterable particulate matter
simultaneously with sulfuric acid mist (and with S03 and S02)
will not be discussed in this subsection.
1.1 Sampling
1.1.1 Probe Liner - Borosilicate or quartz glass tubing
equipped with a heating system capable of preventing visible
condensation during sampling should be protected with an outer
sheath of stainless steel. Borosilicate or quartz probe
liners can be used for stack temperatures up to about 480 C
(900°F). Quartz liners should be used for high-temperature
probes for stacks with temperatures between 480° and 900°C
(900° and 1650°F). Both types of liners may be used at
temperatures higher than specified for short periods of time,
subject to the approval of the administrator. Metal probe
liners may not be used because of the requirement that the
liner material must not react with the gas constituents.
Upon receiving a new probe, it should be visually checked
for the length and composition ordered and for breaks or
cracks and then leak checked on a sampling train as shown in
Figure 1.1. Also the probe heating system should be checked
as follows:
1. Connect the probe with a nozzle attached to the
inlet of the pump.
2. Electrically connect and turn on the probe heater
for 2 or 3 min. It should become warm to the touch.
3. Start the pump and adjust the needle valve until a
3 3
flow rate of about 0.02 m /min (0.75 ft /min) is achieved.
4. Check the probe. It should remain warm to the touch.
The heater should be capable of maintaining the exit air at a
minimum of 100°C (212°F) under these conditions. If it cannot,
the probe should be repaired, returned to the supplier, or
rejected.
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 5 of 13
1.1.2 Probe Nozzle - Same as Method 5, Section 3.4.2.
1.1.3 Pitot Tube - Same as Method 5, Section 3.4.2.
1.1.4 Differential Pressure Gauge - Same as Method 5,
Section 3.4.2.
1.1.5 Filter Holder - A borosilicate glass filter holder with
a glass frit filter support and a silicone rubber gasket is
required by the Reference Method. Other gasket materials
(e.g., Teflon or Viton) may be used, subject to the approval
of the administrator. The holder design must provide a
positive seal against leakage from the outside or around the
filter. A filter holder should be durable, easy to load, and
leak free in normal applications. The filter holder is placed
between the first and second impingers, and the filter is
located toward the direction of flow. Do not heat the filter
holder.
1.1.6 Impingers - Four impingers are required, as shown in
Figure 1.1. The first and third impinger must be of the
Greenburg-Smith design with standard tips. The second and
fourth should be of the Greenburg-Smith design, but modified
by replacing the insert with an approximately 13-mm (0.5-in.)
inside diameter (ID) glass tube having an unconstricted tip
located 13 mm (0.5 in.) from the bottom of the flask.
Connections between impingers should be of glass. (Plastic or
rubber tubing is not permitted because of absorption and
desorption of gaseous species.) Silicone grease may be used,
if necessary, to prevent leakage.
Upon receipt of a new Greenburg-Smith impinger, fill the
inner impinger tube with water. If the water does not drain
through orifice within 6 to 8 s, the impinger tip should be
replaced or enlarged to prevent an excessive pressure drop in
the sampling system. Each impinger is checked visually for
damages such as breaks or cracks and for manufacturing flaws
such as poorly shaped connections.
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 6 of 13
Collection absorbers and flow rates other than the
specif ed ones may be used subject to the approval of the
administrator. The collection efficiency must, however, be
shown to be at least 99% for each test run to obtain approval
and must be documented in the emission test report. If the
efficiency is found to be acceptable after a series of three
tests, further documentation is not required. To conduct the
efficiency test, extra absorbers must be added for the
sulfuric acid mist and the SO2, and then each must be analyzed
separately. These extra absorbers must not contain more than
1% of the total H2SO4 or S02.
1.1.7 Metering System - Same as Method 5, Section 3.4.1.
1.1.8 Barometer - Same as Method 5, Section 3.4.1.
1.1.9 Gas Density Determination Equipment - Same as Method 5,
Section 3.4.1.
1.1.10 Temperature Gauge - Same as Method 5, Section 3.4.1.
1.2 Sample Recovery Apparatus
1.2.1 Wash Bottles - Two 500-ml polyethylene or glass wash
bottles are needed for quantitative recovery of collected
samples.
1.2.2 Storage Bottles - Two 1000-ml polyethylene bottles are
required for each sample run, plus one 100-ml polyethylene
bottle to retain a blank for each absorbing solution used in
testing. Visually check wash bottles and/or storage bottles
for damage. Also check each storage bottle seal to prevent
sample leakage during transport.
1.2.3 Graduated Cylinders - One 250-ml and one 1000-ml glass
graduated cylinder (Class A) or volumetric flasks are needed
to measure the impinger contents.
1.2.4 Trip Balance - A trip balance with a 500-g capacity and
an accuracy of +0.5 g is needed to weigh the silica gel, only
if a moisture content analysis is to be done. A moisture
determination has to be performed unless the gas stream can be
considered dry. Check the trip balance by using a range of
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 7 of 13
standard weights, and adjust or return to supplier if neces-
sary.
1.3 Analysis Glassware
1.3.1 Pipettes - Several volumetric pipettes (Class A),
including 5-, 10-, 20-, 25-, and 100-ml sizes, should be
available for the analysis.
1.3.2 Volumetric Flasks - Volumetric flasks (Class A) are
required, and should include 50-, 100-, and 1000-ml sizes.
1.3.3 Burette - A 50-ml burette (Class A) is required for all
titrations.
1.3.4 Erlenmeyer Flasks - One 250-ml Erlenmeyer flask is
required for each sample, blank, standard, and control sample.
1.3.5 Dropping Bottle - One 125-ml glass dropping bottle is
needed to prepare the thorin indicator.
1.3.6 Graduated Cylinder - A 100-ml glass graduated cylinder
(Class A) is needed in the preparation of the thorin indicator
and the sample. Check all glassware for cracks, breaks, and
discernible manufacturing flaws.
1.3.7 Trip Balance - Same as Subsection 1.2.4.
1.4 Reagents
Unless otherwise indicated, all reagents should conform
to the specifications established by the Committee on
Analytical Reagents of the American Chemical Society (ACS),
when such specifications are available; otherwise use best
available grade.
1.4.1 Sampling - The following are required for sampling:
Filters - Same as Method 5, Section 3.4.1.
Silica Gel - Same as Method 5, Section 3.4.1.
Water - Deionized distilled water to conform to ASTM
specification D1193-74, Type 3. At the option of the analyst,
the potassium permanganate (KMn04) test for oxidizable organic
matter may be omitted when high concentrations of organic
matter are not expected to be present.
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 8 of 13
Isopropanol, 80% - Mix 800 ml of reagent grade or
certified ACS isopropanol with 200 ml of deionized distilled
water. Check each lot of isopropanol for peroxide (H?O?)
impurities as follows:
1. Shake 10 ml of isopropanol with 10 ml of freshly
prepared 10% potassium iodide (KI) solution.
2. Prepare a blank by similarly treating 10 ml of
deionized distilled water.
3. After 1 min, read the absorbance of the alcohol
sample at 352 nm on a spectrophotometer; if the absorbance
exceeds 0.1, reject the isopropanol.
Peroxides may be removed from isopropanol by redistilling
or by passing the mixture through a column of activated
alumina; after peroxides are removed, check for peroxide
impurities using the same method as above. However, reagent
grade isopropanol with suitably low peroxide levels may be
obtained from commercial sources. Therefore, rejection of
contaminated lots may be a more efficient procedure.
Potassium iodide solution, 10% - Dissolve 10.0 g of
reagent grade or certified ACS KI in deionized distilled
water, and dilute to 100 ml. Prepare when needed. This
solution is used to check for peroxide impurities in the
isopropanol only.
Hydrogen peroxide, 3% - Dilute 30% reagent grade or
certified ACS ^2°2 1:9 (v/v) witn deionized distilled water.
Prepare fresh daily.
1.4.2 Sample Recovery - The following are required for sample
recovery:
Water - Deionized distilled water, as in Subsection 1.4.1
above.
Isopropanol 100% - See Subsection 1.4.1.
1.4.3 Analysis - The following are required for sample
analysis.
Water - Use deionized distilled water as described in
Subsection 1.4.1.
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 9 of 13
Isopropanol 100% - Use reagent grade or certified ACS iso-
propanol, and check for peroxide impurities, as in Subsection
1.4.1 above.
Thorin indicator - Reagent grade or certified ACS
l-(o-arsonophenylazo)-2-naphthol-3,6-disulfonic acid disodium
salt. Dissolve 0.20 g in 100 ml of deionized distilled water.
Barium perchlorate solution, 0.0100N - Dissolve 1.95 g of
reagent grade or certified ACS barium perchlorate trihydrate
(Ba(C104)2 • SH-O) in 200 ml deionized distilled water, and
dilute to 1 £ with isopropanol. Alternatively, 1.22 g of
(BaCl2 • 2H20) may be used. Standardize as in Section 3.7.5.
Sulfuric acid standard, 0.0100N - Either purchase the
manufacturer's certified 0.0100N H2S04, or standardize the
H2S04 to 0.0100N +0.0002N against 0.0100N reagent grade or
certified ACS sodium hydroxide (NaOH) that has previously been
standardized against primary standard grade potassium acid
phthalate.
1.5 Analytical Equipment
A spectrophotometer is needed to check the isopropanol
for peroxide impurities. The absorbance is read at 352 nm on
the spectrophotometer.
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 10 of 13
Table 1.1. ACTIVITY MATRIX FOR PROCUREMENT OF APPARATUS & SUPPLIES
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sampling
Sampling probe
with heating
system
Capable of 100°C
(212°F) exit air at
flow rate of 20 A/min
Visually check; run
heating system check-
out
Repair, re-
turn to sup-
plier, or re-
ject
Probe nozzle
Stainless steel (316);
sharp, tapered leading
edge (angle <30°);
difference between
measured ID's
-------
Section No, 3.7.1
Revision No. 0
Date May 1, 1979
Page 11 of 13
Table 1.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Orifice meter
AH@ of 46.74 +6.35 mm
(1.84 +0.25 in.)
(recommended)
Visually check upon
receipt for damage;
calibrate against
wet test meter
Repair, if
possible;
otherwise,
return to
supplier
Irapingers
Standard stock glass;
pressure drop across
impingers not excessive
(Sec. 3.7.1)
Visually check upon
receipt; check pres-
sure drop (Sec.3.7.1)
Return to
supplier
Filter holder
Leak free
Visually check before
use
As above
Filters
Glass fiber without or-
ganic binder designed
to remove 99.95% (<0.05%
penetration) of 0.3-|J
dioctyl phthalate smoke
particles
Manufacturer's guar-
antee that filters
meet ASTM standard
method D2986-71; ob-
serve under light
for defects
Return to
supplier and
replace
Dry gas meter
Capable of measuring
total volume with
accuracy of +2% at
flow rate of
0.02 m3/min
(0.75 ft3/min)
Check for damage upon
receipt; calibrate
against wet test
meter (Sec. 3.7.2)
Reject if
damaged, be-
haves errati-
cally, or can-
not be pro-
perly adjusted
Wet test meter
Capable of measuring
total volume with
accuracy of +1%
Upon assembly, leak
check all connections
and check calibration
by a liquid displace-
ment method
As above
Thermometers
Within +1°C (2°F) of
value in range of 0°C
to 25°C (32°F to 67°F)
for impinger thermome-
ter; +3°C (6°F) of true
value in range of 0°C
to 90°C (32°F to 194°F)
for dry gas meter
thermometers
Check each thermome-
ter upon receipt for
damage--i.e., dents
or bent stem; cal-
ibrate (Sec. 3.7.2)
Reject if
unable to
calibrate
(continued)
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 12 of 13
Table 1.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Barometer
Capable of measuring
atmospheric pressure
to within 2.5 mm
(0.1 in.) Hg
Check against a mer-
cury-in-glass barome-
ter or equivalent;
calibrate (Sec.
3.7.2)
Determine cor-
rection factor,
or reject if
difference in
the readings
exceeds +2.5
mm (0.1 in.)
Hg
Sample Recovery
Wash bottles
Polyethylene or glass,
500 ml
Visually check for
damage upon receipt
Replace or
return to
supplier
Storage bottles
Polyethylene, 1000 ml
and 100 ml
Visually check for
damage upon receipt;
be sure caps make
proper seals
As above
Graduated cyl-
inders
Glass (Class A), 250
ml and 1000 ml
Visually check upon
receipt
As above
Trip balance
500-g capacity, +0.5 g;
needed to weigh silica
gel only if moisture
measurement desired
Check with standard
weights up to 500 g
Adjust or
return to
supplier
Analysis Glass-
ware
Pipettes, volu-
metric flasks,
burette, and
graduated
cylinder
Glass (Class A)
Upon receipt, check
for stock number,
cracks, breaks, and
manufacturer's flaws
As above
Reagents
Distilled water
ASTM-D1193-74, Type 3
Check each lot or
specify type when
ordering
As above
(continued)
-------
Section No. 3.7.1
Revision No. 0
Date May 1, 1979
Page 13 of 13
Table 1.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Isopropanol
100% isopropanol, re-
agent grade or certified
ACS with no peroxide
impurities; absorbance
£0.1 at 352 nm on spec-
trophotometer
Upon receipt, check
each lot for peroxide
impurities with a
spectrophotometer
Redistill,
pass through
alumina column,
or replace
Hydrogen perox-
ide
30% H202, reagent grade
or certified ACS
Upon receipt, check
label for grade or
certification
Replace or
return to
Potassium
iodide
KI reagent grade or
certified ACS
As above
As above
Thorin indica-
tor
1-(o-arsonophenylazo)-
2-naphthol-3,6 disul-
fonic acid disodium
salt, reagent grade or
certified ACS
Upon receipt, check
label for grade or
certification
As above
Barium perchlor-
ate trihydrate
solution
Ba(C104)2.3H20, re-
agent grade or
certified ACS
As above
As above
Sulfuric acid
solution
H2S04, 0.0100N +0.0002N
Certified by manufac-
turer, or standardize
against 0.0100N NaOH
previously standard-
ized against potassium
acid phthalate (pri-
mary standard grade)
As above
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 1 of 20
2.0 CALIBRATION OF APPARATUS
Calibration of the apparatus is one of the most important
functions in maintaining data quality. The detailed calibra-
tion procedures included in this section are designed for the
equipment specified by Method 8 and described in the previous
section. A laboratory log book of all calibrations must be
maintained. Table 2.1 at the end of this section summarizes
the quality assurance functions for calibration.
2.1 Metering System
2.1.1 Wet Test Meter - Wet test meters are calibrated by the
manufacturer to an accuracy of +0.5%. The calibration of the
wet test meter must be checked initially upon receipt and
yearly thereafter. A wet test meter with a capacity of 3.4
3 3
m /h (120 ft /h) will be necessary to calibrate the dry gas
meter. For large wet test meters (>3£/rev), there is no
convenient method to check the calibration. For this reason,
several methods are suggested, and other methods may be
approved by the administrator. The initial calibration may be
checked by any of the following methods:
1. Certification from the manufacturer that the wet
test meter is within +1% of true value at the wet test meter
discharge, so that only a leak check of the system is then
required. Determine from manufacturer if the air entering the
wet test meter should be saturated.
2. Calibration by any primary air or liquid
displacement method that displaces at least one complete
revolution of the wet test meter.
3. Comparison against a smaller wet test meter that has
previously been calibrated against a primary air or liquid
displacement method, as described in Section 3.5.2.
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 2 of 20
4. Comparison against a dry gas meter that has pre-
viously been calibrated against a primary air or liquid
displacement method.
The calibration of the test meter should be checked
annually. The calibration check can be made by the same
method as that of the original calibration, with the exception
that the comparison method need not be recalibrated if the
calibration check is within +1% of the true value. When this
agreement is not obtained, then the comparison method or wet
test meter must be recalibrated against a primary air or
liquid displacement method.
2.1.2 Sample Meter System - The sample meter system—consist-
ing of the pump, vacuum gauge, valves, orifice meter, and dry
gas meter—is initially calibrated by stringent laboratory
methods before it is used in the field. After the initial
acceptance, the calibration is rechecked after each field test
series. This recheck is designed to provide the tester with a
method that can be used more often and with less effort to
ensure that the calibration has not changed. When the quick
check indicates that the calibration factor has changed, the
tester must again use the complete laboratory procedure to
obtain the new calibration factor. After recalibration, the
metered sample volume must be multiplied by either the initial
or the recalibrated calibration factor—that is, the one that
yields the lower gas volume for each test run.
Before initial calibration of the metering system, a leak
check should be conducted. The meter system should be leak
free. Both positive (pressure) and negative (vacuum) leak
checks should be performed. Following is a pressure
leak-check procedure that will check the metering system from
the quick disconnect inlet to the orifice outlet and will
check the orifice-inclined manometer:
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 3 of 20
1. Disconnect the orifice meter line from the
downstream orifice pressure tap (the one closest to the
exhaust of the orifice), and plug this tap.
2. Vent the negative side of the inclined manometer to
the atmosphere. If the inclined manometer is equipped with a
three-way valve, this step can be performed by merely turning
the three-way valve that is on the negative side of the
orifice-inclined manometer to the vent position.
3. Place a one-hole rubber stopper with a tube through
its one hole in the exit of the orifice, and connect a piece
of rubber or plastic tubing to the tube, as shown in
Figure 2.1.
4. Open the positive side of the orifice-inclined
manometer to the "reading" position. If the inclined
manometer is equipped with a three-way valve, this will be the
line position.
5. Plug the inlet to the vacuum pump. If a quick
disconnect with a leak-free check valve is used on the control
module, the inlet will not have to be plugged.
6. Open the main valve and the bypass valve.
7. Blow into the tubing connected to the end of the
orifice until a pressure of 127 to 178 mm (5 to 7 in.) H2O has
built up in the system.
8. Plug or crimp the tubing to maintain this pressure.
9. Observe the pressure reading for a 1-min period. No
noticeable movement in the manometer fluid level should occur.
If the meter box has a leak, a bubbling-type leak-check
solution may aid in locating the leak(s).
•
After the metering system is determined to be leak free by
the positive leak-check procedure, the vacuum system to and in-
cluding the pump should be checked by plugging the air inlet to
the meter box. If a quick disconnect with a leak-free stopper
system is presently on the meter box, then the inlet will not
have to be plugged. Turn the pump on, pull a vacuum within
-------
AIR
INLET
RUBBER
TUBING
RUBBER
STOPPER
ORIFICE
VACUUM
GAUGE~
BLOW INTO TUBING
UNTIL MANOMETER
READS 5 TO 7 IN. HO
WATER COLUMN 2
MAIN VALVE
CLOSED
ORIFICE
MANOMETER
AIRTIGHT
PUMP
CU JD fl> CD
iQ rt < O
(D (D I-1- rt
tn H-
.U g H- O
PJ O O
O "< 3
Hi, 2
H a o
to- O •
o
M U)
Figure 2.1. Positive leak check of metering system.
VO
to
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 5 of 20
7.5 cm (3 in.) Hg of absolute zero, and observe the dry gas
-4 3
meter. If the leakage exceeds 1.5 x 10 m /min (0.005
o
ft /min), the leak(s) must be found and minimized until the
above specifications are satisfied.
Leak checking the meter system before initial calibration
is not mandatory, but is recommended.
Note; For metering systems having diaphragm pumps, the
normal leak-check procedure described above will not detect
leakages within the pump. For these cases, the following
leak-check procedure is suggested: make a 10-min calibration
run at 0.00057 m /min (0.02 ft /min); at the end of the run,
take the difference of the measured wet test meter and dry gas
meter volumes; divide the difference by 10, to get the leak
3
rate. The leak rate should not exceed 0.00057 m /min (0.02
ft3/min).
Initial calibration - The dry gas meter and orifice meter
can be calibrated simultaneously and should be calibrated when
first purchased and any time the posttest check yields a Y
outside the range of the calibration factor Y +0.05Y. A
calibrated wet test meter (properly sized, with +1% accuracy)
should be used to calibrate the dry gas meter and the orifice
meter.
The dry gas meter and the orifice meter should be
calibrated in the following manner:
1. Before its initial use in the field, leak check the
metering system, as described in Subsection 2.1.2. Leaks, if
present, must be eliminated before proceeding.
2. Assemble the apparatus, as shown in Figure 2.2, with
the wet test meter replacing the probe and impingers—that is,
with the outlet of the wet test meter connected to a needle
valve that is connected to the inlet side of the meter box and
with the inlet side of the wet test meter connected to an
impinger with water or to a saturator.
-------
MANOMETER
WATER OUT
LEVEL ADJUST
AIR
INLET
IMPINGER
OR
SATURATOR
*T3 D V Cfl
DJ JD (T) 0)
in rt < O
CO (D H- rt
_ CO H-
ov.^p. o
o ^§3
Hi ^
.. M2 O
o* ? •
Figure 2.2. Sample meter system calibration setup.
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 7 of 20
3. Run the pump for 15 min with the orifice meter
differential (AH) set at 12.7 mm (0.5 in.) H2O to allow the
pump to warm up and to permit the interior surface of the wet
test meter to be wetted.
4. Adjust the needle valve so that the vacuum gauge on
the meter box will read between 50 and 100 mm (2 to 4 in. ) Hg
during calibration.
5. Collect the information required in the forms
provided (Figure 2.3A or 2.3B). Sample volumes, as shown,
should be used.
6. Calculate Y. for each of the six runs, using the
equation in Figure 2.3A or B under the Y. column, and record
the results on the form in the space provided.
7. Calculate the average Y for the six runs using the
following equation:
Y + Y +Y +Y +Y +Y
Y = 1 2 *3 X4 *5 *6 .
Record the average on Figure 2.3A or B in the space provided.
8. The dry gas meter should be cleaned, adjusted, and
recalibrated, or rejected if one or more values of Y fall
outside the interval Y +0.02Y. Otherwise, the average Y
(calibration factor) is acceptable and will be used for future
checks and subsequent test runs.
9. Calculate AH@. for each of the six runs using the
equation in Figure 2.3A or B under the AH@. column, and record
on the form in the space provided.
10. Calculate the average AH@ for the six runs using the
following equation:
AH<§L + AH@0 + AH@_ + AH®. + AH@C + AH@C
AH@ = i 2 3 4 5 6 .
b
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 8 of 20
Date 8//0/7g
Barometric pressure, P, = 3,1-
in. Hg.
Meter box number
Calibrated by
Orifice
manometer
setting
(AH),
in. H20
0.5
1.0
1.5
2.0
3.0
4.0
Gas Volume
Wet test
meter
ft3
5
5
10
10
10
10
Dry gas
meter
.
ft3
/3o. aao
, 35.1+0
Temperature8
Wet test
meter
.
°F
91
98
Outlet
(td),
0
°F
82.
&5
Average
(td)f
°F
09
Time
min
*%
Average
Yi
/
AH@i
1-79
AH
o s
1.0
1.5
2.0
3.0
4.0
AH
Utl
13.6
0 0368
0.0737
0.110
0.147
0.221
0.294
V P (t . + 460)
w b d
"i
vd(pb + Bil> «v + 460)
5 rz9. 6+)(*&J
X./4- (?<).tf}(53(.5}
(t + 460) Q
.„. 0.0317 AH w
iHyi P. (t. + 460) V
DO w
(0. 03/ 7)tO.S) 1 & &• ^ ('*• 76) 1*
SX> 6+ ) (S4<) ) L f J
If there is only one thermometer on the dry gas meter, record the temperature
under t,.
d
Figure 2.3A. Dry gas meter calibration data (English units)
(front side)
-------
Nomenclature:
3
V = Gas volume passing through the wet test meter, ft .
3
V, = Gas volume passing through the dry test meter, ft .
t = Temperature of the gas in the wet test meter, F.
w
d. = Temperature of the inlet gas of the dry test meter, F.
d = Temperature of the outlet gas of the dry test meter, F.
t, = Average temperature of the gas in the dry test meter, obtained by the average t, and
t- T? i
t , F. i
o
AH = Pressure differential across orifice, in. H~0.
Y. = Ratio of accuracy of wet test meter to dry test meter for each run. Tolerance Y. =
1 Y +0.02 Y.
Y = Average ratio of accuracy of wet test meter to dry test meter for all six runs.
Tolerance Y = Y +0.01 Y.
3
AH@. = Orifice pressure differential at each flow rate that gives 0.75 ft /min of air at
standard conditions for each calibration run, in. H»0. Tolerance = AH@ +0.15 (recommended).
3
AH@ = Average orifice pressure differential that gives 0.75 ft /min of air at standard
conditions for all six runs, in. H00. Tolerance = 1.84 +0.25 (recommended). o> cu CD (D
* ~ IQ rt < O
fl> CD H- ft
0 = Time for each calibration run, min. ^ S H- o
0> O 3
O f^* ""^
P, = Barometric pressure, in. Hg. HI z
° M 3 o
to - 0 •
o
M oo
u> o •
Figure 2.3A. Dry gas meter calibration data (English units). ^ ;->
(back side) NJ
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 10 of 20
Date Si//o/7S
Barometric pressure, P, =
mm Hg.
Meter box number
Calibrated by
Orifice
manometer
setting
(AH),
mm H20
10
25
40
50
75
100
Wet test
meter
•
°C
18
/6
Drj
Inlet
v
°C
ga
>9
f gas meter
Outlet
(td>.
o
°C
16
n
Average
,
°C
/e
Time
min
/o%
Average
Yi
W
AHf^
23
AH
i n
25
40
50
75
100
AH
TO £
13 »o
n ?
1.8
2.94
3.68
5.51
7.35
T Vw Pb(td + 273)
TT /T) 1 ^" \ /.- .1. _ _ _ \
Vd(rb ' 13. 6} (tw I273)
(o. /s) fat) ( 23 n
(0./S2-)(737)C2.9/)
(t + 273) G
0.00117 AH w
^ti@. - "V> " /4- _i_ O7T\ V
i P. (t, + LIZ) vw
(o. oo// 7~)f/o1 [ (zQ/ ) (ta. 02) 1 2
'f-rxifirt /. o'.is2. 'J
If there is only one thermometer on the dry gas meter, record it under
Figure 2.3B. Dry gas meter calibration data (metric units).
(front side)
-------
Nomenclature:
3
V = Gas volume passing through the wet test meter, m .
3
V, = Gas volume passing through the dry test meter, m .
t = Temperature of the gas in the wet test meter, °C.
d. = Temperature of the inlet gas of the dry test meter, °C.
d = Temperature of the outlet gas of the dry test meter, °C.
t, = Average temperature of the gas in the dry test meter, obtained by the average of t, and
td , C. i
o
AH = Pressure differential across orifice, mm H~0.
Y. = Ratio of accuracy of wet test meter to dry test meter for each run. Tolerance Y. =
Y +0.02 Y. 1
Y = Average ratio of accuracy of wet test meter to dry test meter for all six runs.
Tolerance Y = Y +0.01 Y.
3
AH@. = Orifice pressure differential at each flow rate that gives 0.021 m of air at standard
conditions for each calibration run, mm H20. Tolerance AH@. = AH@ +3.8 mm H?0 (recommended).
Aa@ = Average orifice pressure differential that gives 0.021 m of air at standard $ ^ $ %
conditions for all six runs, mm H00. Tolerance AH@ = 46.74 +6.3 mm H00 (recommended). *Q rj" < o
L — / CD (D H* (T
CO H-
0 = Time of each calibration run, min . M pf o" 3
*< 3
O 25
P, = Barometric pressure, mm Hg. HI H 55 o
t> •» O •
tO •
O I-1 U>
VO O •
-J ^J
Figure 2.3B. Dry gas meter calibration data (metric units). ^° 'M
(back side)
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 12 of 20
Record the average on Figure 2.3A or B in the space provided.
11. Adjust the orifice meter or reject it if AH§. varies
by more than +3.9 mm (0.15 in.) H25%, recalibrate the meter-
ing system (as in Subsection 2.1.2), and use whichever meter
coefficient (initial or recalibrated) yields the lower gas
volume for each test run.
Alternate procedures—for example, using the orifice
meter coefficients—may be used, subject to the approval of
the administrator.
2.2 Thermometers
The thermometers used to measure the temperature of gas
leaving the impinger train should be initially compared with a
-------
^
1
^
M
^
^^
^
^
^
^
co
rl
cu
§
G
4J
CO
CU
H
^i
V
c*
^
si
^»
<$
>H
4-1
rn
WJ
4J CU
3 S
rH rl
PM PM
1
J
N
t
v^
M
CU
l~t
1
rl 3
CU (3
a 4J
g §
ft CO
cd
rl 60
CU
w h
4) H
s (-5
00
.
pj
^
S
fc
1!
J3
4V"\
V^j
\
^
ff^
§J,
^*
PM
CU
rl
3
CO
CO
cu
^1
p.
u
•H
rl
4-1
cu
CU 0
4-1 rJ
cd cd
a M
0*
vO
II i°
•H
>< 43
PM
£r
o
•o-
^.
>J
vO
i-H
PM
13
>
•H
»t
3 a oo
3 -H 133
CJ 4-
1
Cd 4J
> cu a
CO -H
«v
CU s-^
H ^*e
cued
60
« /-
rl
rl CU 4-
^
4J
CO CU «~
arH
4J
CU 34-
rl >-, C5 >-
4-1 Q
Cd 4J /-
rl CU
K
\
o
^
n
\
O fTi
T3 0
/
rt
s
•H PM
CU rH -O O
B* c iJ,
H 4J
CO <
^
4-1
>• cu >
co t-> g >—
o
cu
S 4J
3 CO ,.
rH CU ft •
0 4J ^ s*
>4J | >
co cu B v-'
cd 3
ca
rl
OJ «
0) 4-1 60
u cu a '
•H B *H /->
MH o 4-1 CE
•H (3 4J <
M Cd CU v^
O S w
t
> CO
TJ 4J
MH
t
\
CO
3 4->
MH
0
33
•S
£
'5
^ «0
5 T
*i
^J tf
s^
OB'*
«*3
v- H
x§
^
«•»
'^^
^i
^^
9ft
(^
55
^
\f\
•L
(y^
QO
jg
fs
*-
i III
_ 25
•*) l>\
*
^
CD oO
o
rH
*J»
.
<<>
o
rH
o
rH
II
Section Nq. ,3.7,2
Revision No. 0
Date May 1, 1979
Page 13 of 20
gas meter, record the temperature under t,.
a
1
CU
rfi
4J
§
Vi
cu
4-1
cu
o
rl
CU
43
4J
CU
g
^
rH
rj
O
ca
•H
CU
rl
CU
43
1 J
CU
MH rl
H *
cd U
co co
4-1 4J
MH MH
•V A
cu cu
4-J IT
cu c)
4-1 4-1
CO CO
CU CU
4J
4-1
CU
43
•a
3
o
^4
43
4-1
60
rJ
•H
CO
CO
cd
p.
OJ
Q
3
rH
0
>
ca
cd
O
II
£
^
4J
r?
•o
cu
43
4-1
43
60
3
o
rl
43
4-1
t)0
rj
•H
CO
CO
cd
o.
0)
H
3
i-H
o
>
CO
cd
0
II
rg
^
•
o
rT
CU
4-1
ca
cu
4-1
4J
cu
[5
cu
43
4-1
£3
•H
CO
cd
60
cu
^r{
4-1
MH
O
CU
rl
3
4J
cd
rl
2.
s
E-l
II
tj
4J
f
£
a
4J
4-1
to
CU
4-1
1
cu
43
4-1
MH
0
ca
cd
60
4J
CU
rH
a
•H
CU
43
4-1
MH
O
cu
3
4-1
cd
cu
P4
e
cu
H
II
•H
T3
4-1
O
A
i-i
cu
4-1
4-1
CO
0)
4J
•o
J
4-1
MH
O
CO
cd
M
4-1
!--]
4-1
3
O
cu
43
4J
MH
0
cu
rj
4-1
cd
rl
CU
Pj
cu
H
II
O
4->
1
^
T3
4-1
MH
O
cu
60
2
cu
0)
4J
(U
3
cd
4-1
•g
0)
1
CO
cu
4J
rl
0)
45
CO
cd
00
J
4J
MH
0
cu
3
4-1
cd
rl
CU
4J
CU
00
rl
CU
^
II
T3
4J
H
M
•S
cd
cu
o
MH
rl
cu
1
4J
ca
. (U
0 4J
CN
pel >>
M
£3 T3
O
« 4-1
CD
CJ
•H
MH
•H
^i
O
co
CO
o
CJ
i_i
cd
•H
4J
a
cu
cu
•H
cu
3
ca
ca
cu
PM
II
P3
Q
cd
in
O
O
cd
MH
O
o
•H
4-1
fV]
II
•rl
^1
CO
CU
0)
43
4J
rH
H
cd
o
cu
4J
CO
H
o in
o
cJ C5
cd 7p 1
^i
3 ^i
y
CJ 4-1
cd co
cu
MH 4-1
O CU
t-t
o PM
4-> II
cd
rl CU
u
bO cd
Cd rl
M CU
CU rH
<3 E~*
II
^,
60
w
.
G
•H
n
cu
rj
CO
ca
cu
M
a.
u
•H
rl
4-1
CU
1
rl
cd
u
^
CM
.
45
8
A
£j
£j
^1
(3
5
•H
4-1
cd
•rl
rH
cd
O
MH
O
H
II
O
-------
1
X
^6
r^
^
CO
Vl
CU
43
g
£3
CS
4-1
CO
0)
H
10
£
^
.
5
1
^
F^s
^t
^
*
Q>
>>
4-1
^ CO
4-1 CU
C 4J
« 01
rH Vl
P-t PM
N.
i^
.'v
^
^
i
5
T
Vl
cu
43
a
n ^
CU (3
43
S H
3 CU
fi 4->
M S
?s 3
O
^O 0)
CO
J-l 60
0)
*J >>
QJ J-i
*>* Q
bO
ttj
»»M
§
§
3
N
H
43
4?
x^
Vr^
P-i
•v
0)
Vl
3
CO
CO
cu
VI
Cu
O
•rl
Vl
4J
CU
CU O
4-1 Vl
cd cd
O M
(
II
"•H
CO
CN
+
13
4-1
**
'~v — . «v
« ^ f*
r-
+
r>
4-1
VD
1-°
T3
>
•H
£ (
3 f
«
O
3 W
3 -H SB
0 4-1
cd 4-1 6
> CD B
CO
g x-C
Vl
CO
4-1
2
a
CO
cd
bO
CU
4-1 n
cd
Vl
CO Vl
cd ^3
C5
cu
§4J
CO
rH Q)
g «
cued
60
cd /-
Vl
CU 4.
> s-
4-1
cu i-
4J
Si
4J f-
CO
H
(3 4-
Vi f-
"
R ^^
2 -
*v
v CO
4J *J t>3 B
CO 0)
cd >
o
Vi
cu
CO 4-1
u cu
•rl g
MH O
•H C
vi cd
o a
i ^~
3
•«
60
(3
H x-
S
" O
•- CM
4J BB 33
4-1 <
Q) •—
Cfl
' €
a
N* H-
" «?
^^
^ \tJf*.
«[ ^IliJ
vl *
II
v^ *V
(^S ^J
VA yip
^
^\ Ci
Xrf VJ
^^
(^
^^
^C ^W
A fv%
*v t^
^ IW
• .
^^y 1^^
•^ X^
t \
^^
o
*^
-•
^
—
^3
•i
*
•
13
4-1
Vl
cu
II 13
cu
Vi
4-1
cd
cu
i-
cu
4-1
cu
43
*rl
\J
o
o
cu
^
Vl
cu
4J
CD
g
M
cd
60
w
J_J
T3
>,
«l
o
CO
•H
cu
Vl
CU
43
M-l Vl
M CU
ct) 5
Section No. 3.7.2
Revision No, 0
Date May 1, 1979
Page 14 of 20
*
") 1
CU
4J
4-1
CO
cu
4-1
4-1
CU
CU
4-1
O
Vi
4-1
60
CO
CO
Cfl
&*
cu
S
3
rH
0
^
CO
cd
0
II
£
^
.
"!°J
vT
(U M
4-> CU
CO 4-1
4-1
CO 4-1
CU CO
4-1 CU
4-1
Vl 4-1
13 0)
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 15 of 20
mercury-in-glass thermometer that meets ASTM E-l No. 63C or
63F specifications as follows:
1. Place both the mercury-in-glass and the dial type or
equivalent thermometer in an ice bath. Compare readings after
the bath stabilizes.
2. Allow both thermometers to come to room temperature.
Compare readings after both stabilize.
3. Accept the dial type or equivalent thermometer if
values agree within ±1°C (2°F) at both points. If the
difference is greater than +1°C (2°F), the thermometer should
be either adjusted and recalibrated until the above criteria
are met, or rejected.
4. Prior to each field trip, compare the temperature
reading of the mercury-in-glass thermometer at room temperature
with that of the meter thermometer in the equipment. If the
readings are not within +2°C (4°F) the meter thermometer should
be replaced or recalibrated.
The thermometers used to measure the metered sample gas
temperature should also be initially compared with a
mercury-in-glass thermometer that meets ASTM E-l No. 63C or
63F specifications:
1. Place the dial type or equivalent thermometer and
the mercury-in-glass thermometer in a hot water bath, 40° to
50°C (105° to 122°F). Compare readings after the bath
stabilizes.
2. Allow both thermometers to come to room temperature.
Compare readings after thermometers stabilize.
3. Accept the dial type or equivalent thermometer if:
(1) values agree within ±3°C (5.4°F) at both points or (2) the
temperature differentials at both points are within ±3°C
(5.4°F) and the temperature differential is taped to the
thermometer and recorded on the pretest sampling checks form
(Figure 2.5).
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 16 of 20
Date
Calibrated by U> &D
Meter box number £*/*)- / AH@
I.
Dry Gas Meter*
Pretest calibration factor = Q.
factor for each calibration run).
Impinger Thermometer
(within +2% of the average
Was a pretest temperature correction used? _ yes \S no.
If yes, temperature correction _ (within +1°C (2°F) of re-
ference values for calibration and within ±2°C (4°F) of re-
ference values for calibration check).
Dry Gas Meter Thermometer
Was a pretest temperature correction made? _ yes _
If yes, temperature correction _ (within +3°C (3.4°F) of
reference values for calibration and within ±6°C (10.8°F) of
reference values for calibration check).
Barometer
Was the pretest field barometer reading correct? _k_yes
(within ±2.5 mm (0.1 in) Hg of the mercury-in-glass barometer)
no
Most significant items/parameters to be checked.
Figure 2.5. Pretest sampling checks.
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 17 of 20
4. Prior to each field trip, compare the temperature
reading of the mercury-in-glass thermometer at room temperature
with that of the meter system thermometer. The values or
corrected values should be within ±6°C (10.8°F) of one another,
or the meter thermometer should be replaced or recalibrated.
Record any temperature correction factors on Figure 2.5 or on a
similar form.
2.3 Barometer
The field barometer should be adjusted initially and
before each test series to agree within ±2.5 mm (0.1 in.) Hg of
the mercury-in-glass barometer or the station pressure value
reported from a nearby National Weather Service station,
corrected for elevation. The tester should be aware that the
reported pressure is normally corrected to sea level; the
tester should request the uncorrected reading. The correction
for elevation difference between the weather station and the
sampling point should be applied at a rate of -2.5 mm Hg/30 m
(-0.1 in./lOO ft). Record results on Figure 2.5 or on a
similar form.
2.4 Probe Nozzle
The nozzle should be stainless steel (316) or glass with
sharp, tapered leading edges. The angle of taper should be
£30°, and the taper should be on the outside to preserve a
constant ID. Also the probe nozzles should be calibrated
before their initial use in the field. Using a micrometer,
measure the ID of the nozzle to the nearest 0.025 mm
(0.001 in.). Make three separate measurements using different
diameters each time, and then average the measurements. The
difference between the high and low numbers should not exceed
0.1 mm (0.004 in.).
When nozzles become nicked, dented, or corroded, they
should be reshaped, sharpened, and recalibrated before use.
Each nozzle should be permanently and uniquely identified.
Figure 2.6 is an example sample nozzle calibration data form.
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 18 of 20
Date
Calibrated by
, r,
Nozzle
identificaton
number
3*7
D ,
mm, (in. )
0.257
D2'
mm, (in.)
D3'
mm, (in. )
0.2SZ
AD,
mm, (in. )
aooz
avg
a i*
where :
D1I2'3':= Nozzle diameter measured on a different diameter, mm (in.)
Tolerance = measure within 0.025 mm (0.001 in.).
AD = maximum difference in any two measurements, mm (in.).
Tolerance = 0.1 mm (0.004 in.).
Davg = avera
-------
Section No. 3.7.:
Revision No. 0
Date May 1, 1979
Page 19 of 20
2.5 Pitot Tube
The type-S Pitot tube assembly should be calibrate!
according to the procedure outlined in Method 2
Section 3.1.2.
2.6 Trip Balance
The trip balance should be calibrated initially by usin<
Class-S standard weights and should be within +0.5 g of th<
standard weight. Adjust or return the balance to the manu-
facturer if limits are not met.
-------
Section No. 3.7.2
Revision No. 0
Date May 1, 1979
Page 20 of 20
Table 2.1. ACTIVITY MATRIX FOR CALIBRATION OF EQUIPMENT
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Wet test meter
Capacity of at least
3.4 in /h (120 ftJ/h)
and an accuracy within
+1-0%
Calibrate initially
and then yearly
by the liquid dis-
placement technique
Adjust until
specifications
are met, or
return to manu-
facturer
Dry gas meter
Y. = Y +0.02 Y at a
flow rate of 0.02-0.03
m /min (0.66-1)
Calibrate vs. wet
test meter initially,
and when the posttest
check is not within
Y +0.05 Y
Repair or re-
place and then
recalibrate
Thermometers
Impinger thermometer
+1°C (2°F) ; dry gas
meter thermometer with-
in +3°C (5.4°F) over
range
Calibrate each ini-
tially as a separate
component against a
mercury-in-glass
thermometer and then
before each field
trip compare each as
part of the train
with the mercury-in-
glass thermometer
Adjust; de-
termine a con-
stant correc-
tion factor;
or reject
Barometer
+2.5 mm (0.1 in.) Hg of
mercury-in-glass barom-
eter
Calibrate initially
using mercury-in-
glass barometer, and
check before and
after each field test
Adjust to
agree with
certified
barometer
Probe nozzle
Average of three ID
measurements of nozzle;
difference between high
and low not to exceed
0.1 mm (0.004 in.).
ap r <30°
Use a micrometer to
measure to the near-
est 0.025 mm (0.001
in.)
Recalibrate,
reshape, and
sharpen when
nozzles are
nicked, dented,
or corroded
Trip balance
Standard weights mea-
sured within +0.5 g of
stated value
Balance calibration
verified when first
purchased, any time
moved or subjected to
rough handling, and
during routine oper-
ations when cannot
weigh within +0.5 g
Manufacturer
should recali-
brate or ad-
just
Type-S Pitot
tube
Initially calibrated
according to Sec. 2 of
Method 2, and tube tips
undamaged
Visually check before
each field test
Repair or
replace
-------
Section No. 3.7.3
Revision No. 0
Date May 1, 1979
Page 1 of 7
3.0 PRESAMPLING OPERATIONS
The quality assurance functions for presampling prepar-
ations are summarized in Table 3.1 at the end of this section.
See Section 3.0 of this Handbook for details on preliminary
site visits.
3.1 Apparatus Check and Calibration
Figure 3.1 or a similar form is recommended to aid the
tester in preparing an equipment checklist, status form, and
packing list.
3.1.1 Sampling Train - The schematic of the Method 8 sampling
train is given in Figure 1.1. Commercial models of this
system are available. Each individual or fabricated train
must be in compliance with the specifications in the reference
method, Section 3.7.10.
3.1.2 Probe and Nozzle - The probe and nozzle should be
cleaned internally by brushing first with tap water, then with
deionized distilled water followed by acetone, and finally
allowed to dry in the air. In extreme cases, the glass probe
liner can be cleaned with stronger reagents. The objective is
to leave the glass liner free from contaminants. The probe
heating system should be checked to see that it is operating
properly. The probe must be leak free at a vacuum of 380 mm
(15 in.) Hg when sealed at the inlet or tip.
3.1.3 Impingers, Filter Holder, and Glass Connections - All
glassware should be cleaned first with detergent and tap water
and then with deionized distilled water. Any items that do
not pass a visual inspection for cracks or breakage must be
repaired or discarded.
3.1.4 Pump - The vacuum pump and oiler should be serviced as
recommended by the manufacturer, every 3 mo, or after the 10th
test (whichever comes first), or upon erratic behavior (nonuni-
form or insufficient pumping action).
-------
Section No. 3.7.3
Revision No. 0
Date May 1, 1979
Page 2 of 7
Apparatus check
Probe
Type glass liner
Borosilicate
Quartz
Heated
Leak checked
Nozzle
Glass
Stainless steel
Other
Pitot Tube
Type
Other
Properly attached
Modifications
P
Differential
Pressure Gauge
Inclined manometer
Other
Filter Holder
Borosilicate glass
Glass frit
Gasket
Silicone
Teflon
Viton
Acceptable
Yes
•X
iX
•X
iX
v/
V
iX
No
Quantity
required
3 X2C&
*7"^ ^56*
"5"
/
Ready
Yes
^f
^^^
V
No
Loaded
and packed
•X
^
(continued)
Figure 3.1. Example of a pretest preparation checklist.
-------
Section No. 3.7.3
Revision No. 0
Date May 1, 1979
Page 3 of 7
Apparatus check
Condenser
Impingers
Greenbur g- Smi th
Modified Green-
burg- Smith
Impinger Temper-
ature Sensor
Thermometer
Other
Calibrated
Other
Barometer
Mercury
Aneroid
Other
Calibrated*
Stack Temperature
Sensor
Type
Calibrated*
Reagents
Distilled water
Hydrogen perox-
ide (30%)
Isopropanol (80%)
( checked for
peroxides )
Silica gel
Meter System
Pump leak free*
Orifice meter*
Dry gas meter*
Acceptable
Yes
I/
*/
I/
\s
I/
^
\s
I/
I/
I/
1^
I/
K'
^
No
Quantity
required
6>
/V
V
/
2
3%JL
*ft
Hjf*,
?-*
I
Ready
Yes
\S
\S
IS
\s
IS
*/
IS
\s
IS
\S
IS
IS
\s
No
Loaded
and packed
\S
^
\s
i/
^
S
i/
s
•^
i/
I/
I/
IS
Most significant items/parameters to be checked.
Figure 3.1 (continued)
-------
Section No. 3.7.3
Revision No. 0
Date May 1, 1979
Page 4 of 7
3.1.5 Dry Gas Meter - A dry gas meter calibration check
should be made in accordance with the procedure in
Section 3.7.2.
3.1.6 Silica Gel - Either dry the used silica gel at 120° -
150°C (248° - 302°F) or weigh out fresh silica gel in several
200- to 300-g portions in airtight containers to the nearest
0.5 g. Record the total weight (silica gel plus container) on
each container. The silica gel does not have to be weighed if
the moisture content is not to be determined.
3.1.7 Filters - Check filters visually against light for ir-
regularities, flaws, or pinhole leaks. The filters do not
have to be weighed, labeled, or numbered.
3.1.8 Thermometers - The thermometers should be compared with
the mercury-in-glass thermometer at room temperature prior to
each field trip.
3.1.9 Barometer - The field barometer should be compared with
the mercury-in-glass barometer or the weather station reading
after making an elevation correction, prior to each field
trip.
3.2 Reagents and Equipment
3.2.1 Sampling - The first impinger solution (80% isopropa-
nol) is prepared by mixing 800 ml of reagent grade or certi-
fied ACS isopropanol (100%) with 200 ml of deionized distilled
water. The second and third impinger absorbing reagent (H2C>2,
3%) is prepared by diluting 100 ml of 30% H2O2 to 1 Z (1000
ml) with deionized distilled water. The 3% HLO2 should be
prepared fresh daily, using certified ACS reagent grade compo-
nents. Solutions containing isopropanol must be kept in
sealed containers to prevent evaporation and must be prepared
fresh for each test series.
3.2.2 Sample Recovery - Deionized distilled water and 80%
isopropanol are required on site for quantitative transfer of
impinger solutions to storage containers. The water and iso-
propanol are used to clean the sampling train in the process
of sample recovery.
-------
Section No. 3.7.3
Revision No. 0
Date May 1, 1979
Page 5 of 7
3.3 Packing Equipment for Shipment
The condition of equipment may depend upon the careful
packing of equipment with regard to (1) accessibility in the
field, (2) care of movement on site, and (3) optimum func-
tioning of measurement devices in the field. Equipment should
be packed under the assumption that it will receive severe
treatment during shipping and field operations. One major
consideration in shipping cases is the construction materials.
3.3.1 Probe - Pack the probe in a case protected by poly-
ethylene foam or other suitable packing material. The inlet
and outlet should be sealed and protected from breakage. An
ideal container is a wooden case, or equivalent, lined with
foam material in which separate compartments are cut to hold
individual devices. The case, equipped with handles or
eye-hooks that can withstand hoisting, should be rigid enough
to prevent bending or twisting of the devices during shipping
and handling.
3.3.2 Impingers, Connectors, and Assorted Glassware - All
impingers and glassware should be packed in rigid containers
and protected by polyethylene foam or other suitable packing
material. Individual compartments for glassware help to
organize and protect each individual item.
3.3.3 Volumetric Glassware - A sturdy case lined with poly-
ethylene foam material protects drying tubes and assorted vol-
umetric glassware.
3.3.4 Meter Box - The meter box—which contains the manome-
ters, orifice meter, vacuum gauge, pump, dry gas meter, and
thermometers—should be packed in a rigid shipping container
unless its housing is sufficient to protect components during
travel. Additional pump oil should be packed if oil is
required for its operation. It is advisable to always ship a
spare meter box in case of equipment failure.
3.3.5 Wash Bottles and Storage Containers - Storage contain-
ers and miscellaneous glassware should be packed in rigid
foam-lined containers.
-------
Section No. 3.7.3
Revision No. 0
Date May 1, 1979
Page 6 of 7
Table 3.1. ACTIVITY MATRIX FOR PRESAMPLING OPERATIONS
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Probe
1. Probe liner should
be free of contaminants
and constructed of boro-
silicate glass, or
quartz, or the equiva-
lent (no metal liners)
2. Probe must be leak
free at 380 mm (15 in.)
Hg
3. Probe must prevent
condensation of mois-
ture
1. Clean probe in-
ternally by brushing
with tap deionized
distilled water, then
acetone; allow to dry
in air before test
2. Visually check be-
fore test
3. Check out heating
system initially and
when moisture cannot
be prevented during
testing (Sec. 3.7.1)
1. Retrace
cleaning pro-
cedure and
assembly
2. Replace
3. Repair or
replace
Impingers, fil-
ter holders,
and glass con-
nectors
Clean, free of breaks,
cracks, leaks, etc.
Clean with detergent
and tap water, then
deionized distilled
water
Repair or
discard
Pump
Maintain a smooth sam-
pling rate of about
0.3-0.5 m /min (1-1.7
ft /min) at up to 380
mm (15 in.) Hg vacuum
at pump inlet
Service every 3 mo or
upon erratic behavior;
check oiler jars every
10 tests
Repair or
return to
manufacturer
Dry gas meter
+2% of calibration
factor and clean
Calibrate according
to Sec. 3.7.2, and
check for excess oil
As above
Reagents and
Equipment
Sampling
All reagents must be
certified ACS or rea-
gent grade
Prepare fresh daily
and store in sealed
containers
Prepare new
reagent
(continued)
-------
Section No. 3.7.3
Revision No. 0
Date May 1, 1979
Page 7 of 7
Table 3.1 (continued)
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sample
recovery
Deionized distilled wa-
ter on-site and leak-
free sample storage
bottles as specified in
Sec. 3.7.1
Water and reagent
grade isopropanol are
used to clean imping-
er after testing and
prior to taking sam-
ple.
Prepare new
reagent
Package Equip-
ment for Ship-
ment
Probe
Pack in rigid contain-
er and protect with
polyethylene foam
Pack prior to each
shipment
Repack
Impingers, con-
nectors, and
assorted
glassware
Pack in rigid contain-
ers and protect with
polyethylene foam
Pack prior to each
shipment
Repack
Pump
Sturdy case lined with
polyethylene foam ma-
terial or as part of
meter box
As above
As above
Meter box
Meter box case and/or
additional material to
protect train compon-
ents; pack spare meter
box
As above
As above
Wash bottles
and storage
containers
Pack in rigid foam-
lined containers
As above
As above
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 1 of 18
4.0 ON-SITE MEASUREMENTS
The on-site measurement activities include transporting
the equipment to the test site, unpacking and assembling the
equipment, making duct measurements, velocity traverse,
determination of molecular weight and stack gas moisture
content (in certain cases the moisture content can be assumed
to be zero), sampling for sulfuric acid mist and sulfur
dioxide, and recording data. Table 4.1 at the end of this
section summarizes the quality assurance activities for
on-site measurements. A copy of all field data forms
mentioned are contained in Section 3.7.12.
4.1 Transport of Equipment to the Sampling Site
The most efficient means of transporting the equipment
from ground level to the sampling site should be decided
during the preliminary site visit (or prior correspondence).
Care should be exercised to prevent damage to the test
equipment or injury to test personnel during the moving phase.
A laboratory type area should be designated for preparation of
absorbing reagents, placing the filter in the filter holder,
charging of the impingers, sample recovery, and documentation.
This area should be fairly clean and should not have excessive
drafts.
4.2 Sampling
The on-site sampling includes the following steps:
1. Preliminary measurements and setup,
2. Preparation and/or addition of the absorbing
reagents to the impingers,
3. Placement of the filter in the filter holder,
4. Setup of the sampling train,
5. Preparation of the probe,
6. Leak check of entire train,
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 2 of 18
7. Insertion of the probe into the stack,
8. Sealing the port,
9. Checking the temperature of the probe,
10. Sampling at designated points, and
11. Recording of the data.
A final leak check of the train must always be performed upon
completion of sampling.
4.2.1 Preliminary Measurements and Setup - The sampling site
location should be selected in accordance with Method 2. If
this is not possible due to duct configuration or other
reasons, the sampling site location should be approved by the
administrator. A 115-V, 30-amp electrical supply is necessary
to operate the standard sampling train. Measure the stack and
either determine the minimum number of traverse points by
Method 1 or check the traverse points determined from the
preliminary site visit, Section 3.0 of this Handbook. Record
all data on the traverse point location form, as shown in
Section 3.0. These measurements will be used to locate the
Pitot tube and the sampling probe during preliminary measure-
ments and actual sampling.
4.2.2 Stack Parameters - Check the sampling site for cyclonic
or nonparallel flow as described in Method 1 (Section 3.0).
The sampling site must be acceptable before a valid sample can
be made. Determine the stack pressure, temperature, and the
range of velocity heads using Method 2; it is recommended that
a leak check of the velocity pressure system (Method 2) be
performed. Be sure that the proper differential pressure
gauge is chosen for the range of velocity heads encountered
(see Method 2). Determine the moisture content using the
approximation Method 4 or its alternatives for the purpose of
setting the isokinetic sampling rate. If the particular
source has been tested before or a good estimate of the
moisture is available, this should be sufficient. The
Reference Method uses the condensate collected during sampling
to determine the moisture content used in final calculations.
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 3 of 18
Note; For contact-process sulfuric acid plants, the
moisture can be assumed to be zero if a scrubber is not in
use.
Determine the dry molecular weight of the stack gas, as
required in Method 2. If an integrated gas sample is
required, follow Method 3 procedures and take the sample
simultaneously with, and for the same total length of time as,
the sulfuric acid mist and SCX sample run. Sampling and
analytical data forms for molecular weight determinations are
presented in Method 3 .
Using the stack parameters obtained by these preliminary
measurements, the nomograph can be set up as outlined in
APTD-0576. An example of a nomograph data form is presented
in Method 5 .
Method 8 sampling is performed isokinetically like
3
Method 5, but the sampling rate is not to exceed 0.03 m /mm
3
(1.0 ft /min) during the test. To accomplish this, select a
nozzle size based on the range of velocity heads, so that it
is not necessary to change the nozzle size in order to
maintain isokinetic sampling rates. Select also a nozzle that
3
will not allow the maximum sampling rate to exceed 0.03 m /mm
3
(1.0 ft /min) during the run. Check the maximum AH, using the
following equation:
Elation 4-!
Maximum AH <
m
where
Maximum AH = pressure differential across the orifice, in.
H2O, that will produce a flow of 1.0 ft /min;
P = pressure of the dry gas meter, in. Hg;
M = molecular weight of stack gas;
AH@ = pressure differential across the orifice that will
produce a flow of 0.75 scfm, in. H2O; and
T = temperature of the meter, °R.
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 4 of 18
This maximum AH will limit the sampling flow rate to <0.03
m3/min (1.0 ft3/min).
During the run, do not change the nozzle size. Install
the selected nozzle using a Viton-A O-ring when stack temp-
eratures are <260°C (500°F) and using an asbestos string
gasket when temperatures are higher (see APTD-0576 for
details). Other connecting systems such as Teflon ferrules
may be used. Mark the probe with heat resistant tape or by
some other technique to denote the proper distance into the
stack or duct for each sampling point.
Select a suitable probe liner and probe length so that
all traverse points can be sampled. For large stacks,
consider sampling from opposite sides of the stack to reduce
the length of the probe.
Select a total sampling time greater than or equal to the
minimum total sampling time specified in the test procedures
for the specific industry so that (1) the sampling time per
point is >_2 min (or some greater time interval specified by
the administrator) and (2) the sample volume taken (corrected
to standard conditions) will exceed the required minimum total
gas sample volume (normally 1.15 dscm (40.6 dscf)). The
latter can be based on an approximate average sampling rate.
It is recommended that the number of minutes sampled at
each point be an integer or an integer plus one-half min, in
order to avoid timekeeping errors.
In some circumstances (e.g., batch cycles), it may be
necessary to sample for shorter times at the traverse points
and to obtain smaller gas sample volumes. In these cases, the
administrator's approval must first be obtained.
4.2.3 Preparation and/or Addition of Absorbing Reagents
and Filter to Collection System - Absorbing reagents
can be prepared on site if necessary, according to the
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 5 of 18
directions given in Section 3.7.3. A pipette or graduated
cylinder should be used to place 100 ml of 80% isopropanol
into the first impinger. Be sure that the pipette or
graduated cylinder was not used previously to add the H202
solution. It is suggested that the graduated cylinders or
pipettes be marked to reduce the chance of interchanging.
Place 100 ml of 3% H202 into the second impinger and 100 ml of
3% H202 into the third impinger. Also, place approximately
200 g of silica gel into the fourth impinger.
Note: If moisture content is to be determined by
impinger analysis, either weigh each of the first three
impingers (plus absorbing solution) to the nearest 0.5 g and
record these weights, or determine to the nearest 1 ml
volumetrically. The weight of the silica gel (or silica gel
plus container) must also be determined to the nearest 0.5 g,
and recorded.
Using tweezers or clean disposable surgical gloves, place
a filter in the filter holder. Be sure that the filter is
properly centered and that the gasket is properly placed in
order to prevent the sample gas stream from circumventing the
filter. Check the filter for tears after assembly is
completed.
4.2.4 Assembling Sampling Train - During preparation and
assembly of the sampling train, keep all sample train surfaces
that are to be exposed to the sample covered until just prior
to assembly or until sampling is about to begin.
Assemble the sampling train as shown in Figure 1.1, using
(if necessary) a very light coat of silicone grease on all
ground-glass joints. Apply grease only to the outer portion
of the glass joint to avoid the possibility of contaminating
the sample. Place crushed ice and water around the impingers.
4.2.5 Leak Checks - Leak checks are necessary to assure that
the sample has not been biased low by dilution air. The
Reference Method specifies that leak checks be performed at
certain times. These are discussed below in this subsection.
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 6 of 18
Pretest leak check - A pretest leak check is recommended,
but not required. If the tester opts to conduct the pretest
leak check, the following procedure should be used:
1. After the sampling train has been assembled, turn on
the probe heating system, set it at the desired operating
temperature, and allow time for the temperature to stabilize.
2. If a Viton A O-ring or other leak-free connection is
used in assembling the probe nozzle to the probe liner, leak
check the train at the sampling site by plugging the nozzle
and pulling a 380 mm (15 in.) Hg vacuum. Note; A lower
vacuum may be used, if it is not exceeded during the test.
If an asbestos string is used for the probe gasket, do
not connect the probe to the train during the leak check.
Instead, leak check the train by first plugging the inlet to
the first impinger and pulling a 380 mm (15 in.) Hg vacuum
(see note immediately above). Then connect the probe to the
train and leak check at about 25 mm (1 in. ) Hg vacuum;
alternatively, the probe may be leak checked with the rest of
the sampling train in one step at a vacuum of 380 mm (15 in.)
Hg. Leakage rates in excess of 4% of the average sampling
rate or at 0.00057 m3/min (0.02 ft3/min), whichever is less,
are not acceptable.
The following leak-check instructions for the sampling
train described in APTD-0576 and APTD-0581 may be helpful:
1. Start the pump with the bypass valve fully open and
the coarse adjust valve completely closed.
2. Partially open the coarse adjust valve and slowly
close the bypass valve until the desired vacuum is reached.
Do not reverse the direction of the bypass valve; this will
cause hydrogen peroxide to back up into the filter holder. If
the desired vacuum is exceeded, either leak check at this
higher vacuum or end the leak check as shown below and start
over.
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 7 of 18
When the leak check is completed, first slowly remove the
plug from the inlet to the probe or the first impinger and
then immediately turn off the vacuum pump. This prevents the
absorbing solution in the impingers from being forced backward
into the filter holder and prevents the silica gel from being
entrained backward into the third impinger. Visually check to
be sure that H20? did not contact the filter and that the
filter has no breaks, and so forth.
Leak checks during the sample run - If during the
sampling run a component (e.g., a filter assembly) change
becomes necessary, a leak check should be conducted
immediately before the change is made. The leak check should
be done according to the procedure outlined above, except that
it should be done at a vacuum equal to or greater than the
maximum value recorded up to that point in the test. If the
3
leakage rate is found to be no greater than 0.00057 m /mm
3
(0.02 ft /min) or 4% of the average sampling rate (whichever
is less), the results are acceptable, and no correction will
need to be applied to the total volume of dry gas metered; if,
however, a higher leakage rate is obtained, the tester either
should record the leakage rate and plan to correct the sample
volume (as shown in Section 3.7.6 of this method) or should
void the sampling run.
Note; Be sure to record the dry gas meter reading before
and after each leak check performed during and after each test
run so that the sample volume can be corrected.
Immediately after component changes, leak checks are
again optional; if such leak checks are done, the procedure
outlined above should be used.
Posttest leak check - A leak check is mandatory at the
conclusion of each sampling run. The leak check should be
done in accordance with the procedures previously outlined,
except that it should be conducted at a vacuum equal to or
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 8 of 18
greater than the maximum value reached during the sampling
run. If the leakage rate is found to be no greater than
0.00057 m3/min (0.02 ft3/min) or 4% of the average sampling
rate (whichever is less), the results are acceptable, and no
correction will need to be applied to the total volume of dry
gas metered. If, however, a higher leakage rate is obtained,
the tester should record the leakage rate and should correct
the sample volume as shown in Section 3.7.6 of this method.
Note: Be sure to record the dry gas meter reading before
performing the leak check in order to determine the sample
volume.
4.2.6 Sampling Train Operation - Just prior to sampling,
clean the portholes to minimize the chance of sampling any
deposited material. Particulate matter can interfere with the
wet chemical analysis for sulfuric acid mist. Verify that the
probe heating system is at the desired temperature and that
both the Pi tot tube and the nozzle are located properly.
Follow the procedure outlined below for sampling:
1. Record the initial dry gas meter readings, barometer
readings, and other data as indicated in Figure 4.1.
2. Position the tip of the probe at the first sampling
point so that the nozzle tip is pointing directly into the gas
stream; then turn on the pump.
3. Immediately adjust the sample flow to isokinetic
conditions.
4. Take other readings required by Figure 4.1 at least
once at each sampling point during each time increment.
5. Record the dry gas meter readings at the end of each
sampling time increment.
6. Repeat steps 3 through 5 for each sampling point.
7. At the conclusion of each traverse, turn off the
pump, remove the probe from the stack, and record the final
readings.
-------
Location Un',4-
Operator
Date
p,
hg |1 ft
Run number S ft T^- I
Sample box number R. C, - ) ,3.
Meter box number F /Vl - I fa
Meter AH? 1. M )
Meter calibration Y j .
Pi tot tube CP CVSH
Probe length £.
Probe liner material
Probe heater setting
Ambient temperature
Barometric pressure
Assumed moisture
Static pressure
C factor
Reference AP
Maximum AH
Sheet
of
o. \
O
O
Nozzle identification number
Nozzle diameter O. a. .5" ,5.
Final leak rate
O. O I 3,
5> ^ , °) fe
Q
Vacuum during -leak check
Remarks :
', ^ , -V4
Traverse point
number
-S-to_r -V
I
J^
a
*^
^5-
c
T
?
q
lo
I \
\^
Total or
Avg
Sampling
time
(0),
min
O
,y
1 O
I ^~
^1O
SL^
"*rO
•% i^~
HO
H>
?o
5^
fcO
to
Clock
time
24 h
usa.
I.3A2L
Ig3 3
/AS" 3
Vacuum,
mm Hg
(in. Hg)
—
.r>
a ..!>"
S.<
^.5"
?>.O
^•S'
^ . ?£_
a.S
-s .0
3>. 0
A-d
r»>o
1.-0
Stack
temperature
•*&!•
—
»ao
\a \
\ a "J.
) io
\ aa.
i asi.
i i °i
I ^.3
\^a
iai
la*
last
\Et v-~i
Velocity
head
(AP ),
mm H,0
(in. H20)
o.q.^
1 •OS' __
i .05"
).0<
.1^"
.93
-
Pressure
differential
across
orifice
meter ,
mm H,0
(in. H20)
•
\.<1
D.O
p .0
a .0
i .3
I.-2
\-T
l.T.r
l.°l
5.0
1 .1^
\ .q
l.-S^
Gas sample
volume,
mj (ft3)
Ml. MM
i i £ i *
ntf.iq
las.T^
lSfc.tr.0
1 7,0 . ,-iC
1 .1, S . 1 1
1-^T --*fc
141 -C.I
I.Mfc..%l
IS^.O!
l.'TSt-nC,
1 ^fe^t I
IH5.0*0
Gas sample temperature
at dry gas meter
J^p,
—
-10
13
1C,
-)<*
?>
61
*4
SI
q^
<^T
^q
t oo
Wi
—
TO
1 1
"19-
1M
1C,
I*
•R5L
&3.
«.r
%T
?«
•5!^
?3.fc>
Temperature
of gas
leaving
condenser or
last impinger,
°C (°F)
—
f,6
£,4
f, ?
C. 3.
fco
hi
fr, 1
Q,i
f,M
foM
ftl
a
rt
H-
O
25
O
rt
O
H)
Figure 4.1. Method 8 field test data form.
P-
O
2,
O
10
*J
10
o •
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 10 of 18
8. Conduct a leak check, as described in Subsec-
tion 4.2.4, at the conclusion of the last traverse. This
leak check is mandatory. Record all leakage rates. Note:
If the velocity determination is required for the emissions
calculation, a leak check of the Pitot-tube-manometer system
is mandatory. The procedures are detailed in Section 4 of
Method 2.
9. Disconnect the probe and then cap the nozzle and the
end of the probe with polyethylene caps or the equivalent.
See Subsection 4.3 on how to recover the probe contents.
10. Drain the ice bath, and purge the remaining part of
the train by drawing clean ambient air through the system for
15 min at the average sampling rate. Provide clean ambient
air by passing the air through a charcoal filter, or use
ambient air without purification. See Subsection 4.3 for
details on how to protect the probe from contamination during
purging, and so forth. Note; Ambient air that is in
compliance with normal state or Federal ambient air standards
for S02 will have less than a 0.5% effect on the final results
when not cleaned by passing it through a charcoal filter.
During the sampling run, maintain an isokinetic sampling
rate within ^10% unless otherwise specified by the
administrator. Adjust the sampling flow rates when a 20%
variation in the velocity head reading occurs. Make periodic
checks of the manometer level and zero during each traverse.
Vibrations and temperature fluctuations can cause the
manometer zero to drift.
Periodically during the test, observe the connecting line
between the probe and the first impinger for signs of
condensation. If signs do occur, adjust the probe heater
setting upward to the minimum temperature required to prevent
condensation.
4.3 Sample Recovery
The Reference Method requires the sample to be recovered
from the probe, the impingers, all connecting glassware, and
the filter. Sample recovery should be performed in a labora-
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 11 of 18
tory type area to prevent contamination of the test sample.
Upon completion of sampling, the probe should have been
disconnected and capped off with polyethylene caps or the
equivalent. Also, the impinger section should be capped off
with polyethylene caps or the equivalent upon completion of
purging with clean ambient air. Then the impinger box and the
sampling probe can be transported safely to the clean-up area
without contaminating or losing the sample.
4.3.1 Sulfuric Acid Mist Sample Recovery - The sulfuric acid
mist (including S03) sample is collected in the probe, the
first impinger, all connecting glassware before the filter,
the front half of the filter holder, and the filter. To
recover the sample:
1. Transfer the contents of the first impinger into a
250-ml graduated cylinder. (If a moisture content analysis is
to be done, each impinger and its contents should be weighed
to the nearest 0.5 g and recorded before transferring its
contents.)
2. Rinse the probe, the first impinger, all connecting
glassware before the filter, and the front half of the filter
holder with 80% reagent grade or certified ACS isopropanol.
3. Add the rinse solution to the graduated cylinder and
dilute to 250 ml with 80% reagent grade or certified ACS
isopropanol.
4. Remove the filter with a pair of tweezers, and add
to the solution; mix; and transfer to the 1000-ml storage
containers. Protect the solution from evaporation.
5. Mark the level of liquid on the container, and
identify the sample container. An example of a sample label
is shown in Figure 4.2.
6. Place about 100 ml of the 80% isopropanol in a
polyethylene bottle, and label the bottle for use as a blank
during sample analysis.
4.3.2 Sulfur Dioxide Sample Recovery - The S02 is captured in
the second and third impingers and in all connecting
glassware. To recover the S02 sample:
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 12 of 18
'c Acid P/QKJ city ficiA\f\\lt f 05A
Site Drtil .1 CXt-H€t Sample type H
Date ^/mlff Run number SAP "\ A
Front rinseQ^Front filterQ Front solutionQ
Back rinseD Back filterD Back solutionD
Solution ^)*?» IPA Level marked [*T m
AJ
Volume: Initial |Q6fV>L Final
Cleanup by
Figure 4.2. Example of a sample label.
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 13 of 18
1. Transfer the solutions from the second and third
impingers to a 1000-ml graduated cylinder. (If a moisture
content analysis is to be done, each impinger and its contents
should be weighed to the nearest 0.5 g and recorded before
transferring its contents.)
2. Rinse all connecting glassware (including back half
of the filter holder) between the filter and the silica gel
impinger with deionized distilled water; add this rinse water
to the graduated cylinder; and dilute to a volume of 1000 ml
with deionized distilled water.
3. Transfer the solution to a storage container; mark
the level of liquid on the container; and seal and identify
the sample container.
4. Place 100 ml of the absorbing reagent (3% H2O2) in a
polyethylene bottle, and label the bottle for use as a blank
during sample analysis.
4.4 Sample Logistics (Data) and Packing of Equipment
The above procedures are followed until the required number
of runs are completed. Log all data on the form shown in
Figure 4.3. If the probe and the glassware (impingers, filter
holder, and connectors) are to be used in the next test, rinse
all of the glassware and the probe with deionized distilled
water. Rinse the probe, the first impinger, all connecting
glassware before the filter, and the front half of the filter
holder with 80% isopropanol.
The following are recommended at the completion of the test
series:
1. Check all sample containers for proper labeling
(time and date of test, location of test, number of test, and
any pertinent documentation). Be sure that a blank has been
taken.
2. All data recorded during the field test should be
recorded and duplicated by the best means available. One set
of data can then be either mailed to the base laboratory or
given to another team member or to the Agency; the original
data should be hand-carried.
-------
Plant
t\CJlA
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 14 of 18
Sample location UNFiT JJ
Field Data Checks
Sample recovery personnel U?. MflSe /N)
Person with direct responsibility for recovered samples fi.
Sample
number
1
2
3
Blanks
Sample
identification
number
H2S04
54P- I A
KL*
so2
SAP- |5
SAP-*
ftlQht
Date
of
recovery
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 15 of 18
3. All sample containers and sampling equipment should
be examined for damage, and then properly packed for shipment
to the base laboratory. All shipping containers should be
properly labeled to prevent loss of samples or equipment.
4. A quick check of the sampling and sample recovery
procedures can be made using the data form, Figure 4.4.
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 16 of 18
Sampling
Impingers properly assembled?
Contents:* 1st
2nd .? *7. #-, O. - joo /n!L
3rd J % //, o, - /oo
of
Cooling system
Filter between 1st and 2nd impinger?
Proper connections?
Silicone grease added to all ground-glass joints?
Pretest leak check? CJjt*> _ (optional) Leakage^?
Pitot tube lines checked for plugging and leaks?
Meter box leveled? ^^ _ Periodically?
Manometers zeroed?*
Heat uniform along length of'probe?* ~
AH@ from most recent calibration / gj
Nomograph set up properly?
_
Care taken to avoid scraping sampleport or stack wall?
_ _ ,
Seal around^in-stack probe effective?
Probe moved at proper time?
Nozzle and Pitot tube parallel to'stack wall at all times?
Data forms complete and data properly recorded?
Nomograph setting changed when stack temperature hanges
significantly?
_ _
Velocity pressures and orificepressure readings recorded
accurately?
_
Posttest leak check performed?* t/juj (mandatory)
Leakage rate* £>. 0j ^5J/n>'/^ y ~ _
Sampling Recovery
System purged at least 15 min at test sampling rate?*
Filter placed in 1st impinger contents?
Ice removed before purging?
Contents of impingers placed in/polyethylene bottles?
Glassware rinsed with distilled water?
Fluid level marked?*
_
Sample containers sealed and identified?*7
Blanks obtained?*
* Most significant items/parameters to be checked.
Figure 4.4. On-site measurements checklist.
-------
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 17 of 18
Table 4.1
ACTIVITY MATRIX FOR ON-SITE MEASUREMENT CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sampling
Preparation
and/or addi-
tion of ab-
sorbing rea-
gents to col-
lection sys-
tem
100 ml of 80% isopro-
panol to first impinger
and 100 ml of 3% H20
to each of the second
and third impingers
Prepare H-0 and 80%
isopropanol fresh
daily; use pipette or
graduated cylinder to
add solutions
Reassemble col-
lection system
Filter
Properly centered; no
breaks, damage, or con-
tamination during load-
ing
Use tweezers or surg-
ical gloves to load
Discard fil-
ter and
reload
Assembling sam-
pling train
1. Assemble to speci-
fications in Fig. 1.1
2. Leakage rate <4% or
0.00057 m /min (0.02
ft /min)
1. Before each sam-
pling
2. A leak check be-
fore sampling is re-
commended; plug the
nozzle or inlet to
the first impinger
and pull a vacuum of
380 mm (15 in.) Hg
1. Reassemble
2. Correct leak
Sampling (iso-
kinetically)
1. Sampling must be
performed within +10%
of isokinetic
1. Calculate for each
sample run
2. Check applicable
standard for minimum
sampling time and vol-
ume; minimum sampling
time/point should be
2 min
3. Sampling rate~shoul
not exceed 0.03 m /min
(1.0 ft /min)
2. Make a quick cal-
culation before and
an exact calculation
after testing
3. Select proper noz-
zle size. Sec. 3.7.4,
Eq. 4-1
1. Repeat
sample or
obtain accept-
ance from a
representative
of the
Administrator
2. As above
3. As above
(continued)
-------
Table 4.1 (continued)
Section No. 3.7.4
Revision No. 0
Date May 1, 1979
Page 18 of 18
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
4. Minimum number of
points sampled, as spe-
cified by Meth. 1
5. Leakage rate^not to
exceed 0x00057 m /min
(0.02 ft /min) or 4% of
average sampling rate;
apply correction to
sample volume if rate
is exceeded
6. Purge remaining SO
from isopropanol
4. Check before the
first test run by mea-
suring duct and sam-
pling site location
5. Leak check after
each test run or be-
fore equipment re-
placement during a
run at maximum vacuum
occurring during the
run (mandatory)
6. Drain ice, and
purge with clean air
for 15 min
4. As above
5. Correct
sample volume
or repeat
sample
6. Repeat
sample
Sample recovery
Noncontaminated sample
Transfer sample to
labeled polyethylene
container after each
test run. Mark level
of solution in the
container
Repeat
sample
Sample logistics
(data) and
packing of
equipment
1. All data recorded
correctly
2. All equipment exam-
ined for damage and la-
beled for shipment
3. All sample contain-
ers properly labeled
and packaged
1. Upon the comple-
tion of each sample
and before packing
for shipment
2. As above
3. Visually check up
on completion of each
sample
1. Complete
data
2. Repeat
sampling if
damage occur-
red during
testing
3. Correct
when possible
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 1 of 17
5.0 POSTSAMPLING OPERATIONS
Table 5.1 at the end of this section summarizes quality
assurance activities for postsampling operations.
5.1 Apparatus Checks
Posttest checks have to be conducted on most of the
sampling apparatus. These checks include three calibration
runs at a single orifice meter setting; cleaning; and/or
routine maintenance. The cleaning and maintenance will be
discussed in Section 3.7.7, and is discussed in APTD-0576.
Figure 5.1 should be used to record data from the posttest
checks.
5.1.1 Metering System - The metering system has two
components that must be checked—the dry gas meter and the dry
gas meter thermometer(s).
The dry gas meter thermometer(s) should be checked by
comparison with the ASTM mercury-in-glass thermometer at room
temperature. If the readings agree within 6°C (10.8°F), they
are acceptable; if not, the thermometer must be recalibrated
according to Section 3.7.2 after the posttest check of the dry
gas meter. For calculations, the dry gas meter thermometer
readings (field or recalibration) that would give the higher
temperature is used; that is, if the field reading is higher,
no correction of the data is necessary; if the recalibration
value is higher, the difference in the two readings should be
added to the average dry gas meter temperature reading.
The posttest check of the dry gas meter is described in
Section 3.7.2. If the posttest dry gas meter calibration factor
(Y) is within 5% of the initial calibration factor, the initial
calibration is used for calculations; if it deviates by >5%, re-
calibrate the metering system (as shown in Section 3.7.2) and use
for the calculations the calibration factor (initial or recali-
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 2 of 17
Meter box number f
Dry Gas Meter
Pretest calibration factor Y = Q.
Posttest check Y- = p. QfrT Y7 = _ (+5% of pretest calibra-
tion factor)*
Recalibration required? _ yes ,/ no
If yes, recalibration factor Y = _ (within +2% of the average
factor for each calibration run)
Lower calibration factor, Y = fy <\ •£ fe for pretest or posttest
calculations
Dry Gas Meter Thermometer
Was a pretest meter temperature correction used? _ yes t>/ no
If yes, temperature correction •—
Posttest comparison with mercury-in-glass thermometer
_ (within +6°C (10.8°F)of the reverence values)
Recalibration required? _ yes _ no
Recalibration temperature correction, if used _ (within +3°C
(5.4°F) of the reference values)
If yes, no correction is needed whenever meter thermometer
temperature is higher
If recalibration temperature is higher, add correction to
average meter temperature for calculations
Barometer
Was pretest field barometer reading correct? _ yes _ no
Posttest comparison _ mm (in.) Hg within (+5.0 mm (0.2 in.)
Hg of mercury-in-glass barometer)
Was recalibration required? _ yes ^ no
If yes, no correction is needed whenever the field barometer
has the lower reading
If the mercury-in-glass reading is lower, subtract the dif-
ference from the field data readings for the calculations
*Most significant items/parameters to be checked.
Figure 5.1. Posttest sampling checks.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 3 of 17
brated) that yields the lesser gas volume. For each test run,
the lesser calibration factor will give the lower gas volume.
5.1.2 Barometer - The field barometers are acceptable if they
agree within +5 mm (0.2 in.) Hg when compared with the
mercury-in-glass barometer. When they do not agree, the
lesser calibration value should be used for the calculations.
If the field barometer reads lower, no correction is
necessary. If the mercury-in-glass barometer reads lower,
subtract the difference from the field data readings for the
calculations.
5.2 Analysis (Base Laboratory)
Calibrations and standardizations are of primary impor-
tance to a precise and accurate analysis. The analytical
method is based on the insolubility of barium sulfate (BaSC»4)
and the formation of a colored complex between barium ions and
the thorin indicator (l-(o-arsonophenylazo)-2-naphthol-3,
6-disulfonic acid disodium salt). Aliguots from the impinger
solutions are analyzed by titration with barium perchlorate to
the pink endpoint. The chemical reaction for this standardiza-
tion is shown in Equation 5-1. The barium ions (Ba ) react
preferentially with sulfate ions (SO ~) in solution to form a
highly insoluble barium sulfate (BaS04) precipitate. After the
++ = ++
Ba has reacted with all SO. , excess Ba reacts with the
thorin indicator (x ) to form a metal salt of the indicator
and to give a color change:
Ba + SO4~ + thorin(x ) -» BaS04 + thorin(Ba ) Equation 5-1
(yellow) (pink)
Upon completion of each step of the standardization or of
each sample analysis, the data should be entered on the proper
data form. At the conclusion of the sample analysis, the data
form should be reviewed and signed by the laboratory person
with direct responsibility for the sample.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 4 of 17
5.2.1 Reagents (Standardization and Analysis) - The following
reagents are required for the analysis of the sulfuric acid
mist (including S03) and the S0_ samples.
Water - Deionized distilled water to conform to ASTM
specification D1193-74, Type 3. At the option of the analyst,
the KMnO4 test for oxidizable organic matter may be omitted
when high concentrations of organic matter are not expected to
be present. Note: It is imperative that the distilled water
meet the ASTM specifications since SO ~ and other polyvalent
ions present in distilled water are not determined in the
normal standardization of the acid by NaOH titration (which
measures the hydrogen ion (H ) concentration rather than the
SO ~ concentration). This added SO ~ concentration would
result in an erroneous standardization of the Ba(Cl04)2
titration, which directly measures SO ~ concentration and not
+
H concentration. A check on the acceptability of the
distilled water is detailed in Section 3.7.1.
Isopropanol, 100% - Certified ACS reagent grade isopro-
panol. Check for peroxide impurities as described in Section
3.7.1.
Thorin indicator - l-o-arsonophenylazo-2-naphthol-3,
6-disulfonic acid disodium salt, or equivalent. Dissolve 0.20
g +0.002 g in 100 ml of deionized distilled water. Measure
the distilled water in a 100-ml Class-A graduated cylinder.
Barium perchlorate solution O.OIOON - Dissolve 1.95 g of
barium perchlorate trihydrate (Ba(ClO4)2 . 3H2O) in 200 ml of
deionized distilled water and dilute to 1 & with isopropanol.
Alternatively, 1.22 g of barium chloride dihydrate (BaCl2 .
2H,0) may be used instead of the trihydrate. Standardize as in
£*
the subsection below with H2S04- Note: Protect the O.OIOON
barium perchlorate solution from evaporation at all times by
keeping the bottle capped between uses.
Sulfuric acid standard, O.OIOON - Either purchase a
standard guaranteed by the manufacturer or standardize to
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 5 of 17
+0.0002N H2SO4 against 0.0100N NaOH that has been standardized
against potassium acid phthalate (primary standard grade), as
described in the subsection below.
The 0.01N H?SO4 may be prepared in the following manner:
a. Prepare 0.5N H2S04 by adding approximately 1500 ml
of deionized distilled water into a 2 SL volumetric flask.
b. Cautiously add 28 ml of concentrated H2SO4 and mix.
Cool, if necessary.
c. Dilute to 2 £ with deionized distilled water.
d. Prepare 0.01N H2SO4 by adding approximately 800 ml
of deionized distilled water to a I SL volumetric flask.
e. Add 20.0 ml of the 0.5N H2S04.
f. Dilute to 1 SL with distilled water and mix
thoroughly. Note: It is recommended that 0.1N sulfuric acid
be purchased. Pipette 10.0 ml of H2S04(0.1N) into a 100-ml
volumetric flask, and dilute to volume with deionized
distilled water that has been determined to be acceptable as
detailed in Subsection 5.2.4. When the 0.01N sulfuric acid is
prepared in this manner, procedures in Subsections 5.2.2. and
5.2.3. may be omitted since the standardization of the barium
perchlorate will be validated with the control sample.
5.2.2 Standardization of Sodium Hydroxide - To standardize
NaOH, proceed as follows:
1. Purchase a 50% w/w NaOH solution. Dilute 10 ml to 1
a with deionized distilled water. Dilute 52.4 ml of the
diluted solution to 1 i with deionized distilled water.
2. Dry the primary standard grade potassium acid phtha-
late (KHP) for 1 to 2 h at 110°C (230°F), and cool in desiccator,
3. Weigh, to the nearest 0.1 mg, three 40-mg portions
of the phthalate. Dissolve each portion in 100 ml of freshly
boiled deionized distilled water in a 250-ml Erlenmeyer flask.
4. Add two drops of phenolphthalein indicator, and
titrate the phthalate solutions with the NaOH solution. All
titrations should be done against a white background to
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 6 of 17
facilitate the detection of the endpoint—the first faint pink
color that persists for at least 30 s.
5. Compare the endpoint colors of the other two
titrations against the first one. The normality is the
average of the three individual values calculated using
Equation 5-1.
XT _ ma KHP „ . . .. -
NNaOH - ml titrant * 204.23 Equation 5-1
where
NNaOH = calcula'ted normality of NaOH, N,
mg KHP = the weight of KHP, mg, and
ml titrant = the volume of NaOH titrant, ml.
The chemical reaction for this standardization is shown in
Equation 5-2. The NaOH is added to the KHP and the colorless
phenolpthalein solution until an excess of sodium ions (Na+)
causes the phenolphthalein to change to a pink color.
NaOH + KHP + phenolphthalein(H+) Equation 5-2
(colorless)
•* KNaP + HOH + phenolphthalein
(pink)
5.2.3 Standardization of Sulfuric Acid - To standardize
H2S04, proceed as follows:
1. Pipette 25 ml of H2S04 into three 250-ml Erlenmeyer
flasks.
2. Add 25 ml of deionized distilled water.
3. Add two drops of phenolpthalein indicator, and
titrate with the standardized NaOH solution to a persistent
pink endpoint, using a white background.
4. Titrate a blank of 25 ml of deionized distilled
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 7 of 17
water, using the same technique as step 3 above. The normal-
ity will be the average of the three independent values calcu-
lated using Equation 5-3.
where
(ml NaO^ - ml NaOHblank) x
_ 2 4 _ Equation 5-3
25
Nti en = calculated normality of H0SOA, N,
H2so4 t 4
ml NaOILj SQ = volume of NaOH titrant used for H2S04/ ml,
ml NaOHKiani, = volume of NaOH titrant used for blank, ml, and
NXT rxt = normality of NaOH, N.
JNaurl
5.2.4 Standardization of Barium Perchlorate (0.0100N) - To
standardize Ba(Cl04)_, proceed as follows:
1. Pipette 25 ml of standard 0.0100N H2S04 into each of
three 250-ml Erlenmeyer flasks.
2. Add 100 ml of reagent grade isopropanol and two to
four drops of thorin indicator, and titrate to a pink endpoint
using 0.0100N Ba(C104)2. All thorin titrations should be done
against a white background to facilitate the detection of the
pink endpoint.
3. Run a blank that contains 25 ml of deionized
distilled water and 100 ml of isopropanol. The blank must not
exceed 0.5 ml of titrant to obtain the endpoint; otherwise the
distilled water has excess SOA~. If this 0.5-ml volume is
exceeded, all reagents made with the distilled water will have
to be remade using acceptable distilled water.
4. Use the endpoint of the first titration as a visual
comparator for the succeeding titrations.
5. Record data on the form in Figure 5.2. The
normality of the Ba(ClO4)2 will be the average of the three
independent values calculated using Equation 5-4.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 8 of 17
Plant Sui-fcirIC Acid ?fa»\t
Sample location Utiij" I
Date
Analyst
Volume and normality of
barium perchlorate
1.
2.
2&Q ml Ba(Cl0)
ml Ba(C104)2
N = A O/O
Blank 25. 0 ml Ba(C10.)0
- 4 2
soln
Sulfur Trioxide Analysis
- Total volume of solution in which the
sulfuric acid sample is contained, ml
V - Volume of sample aliquot, ml
3.
V - Volume of barium perchlorate
titrant used for sample, ml
1st titration
2nd titration
Average
V * - Volume of barium perchlorate 1st titration
titrant used for blank, ml 2nd titration
Average
Run 1
2fo
/oo
W-0
/?. 1
/9.DS
0*0
0.0
o.o
Run 2
Run 3
1st titration
2nd titration
0.99 to 1.01 or (1st titration - 2nd titration | £0.2 ml
Sulfur Dioxide Analysis
V - - Total volume of solution in which the
sulfur dioxide sample is contained, ml
V - Volume of sample aliquot, ml
EL
V - Volume of barium perchlorate 1st titration
titrant used for sample, ml 2nd titration
Average
v , * - Volume of barium perchlorate 1st titration
titrant used for blank, ml 2nd titration
Average
1st titration = Q^g fc
Znd titration
Signature of analyst
Run 1
/O66
10
H>*
IL*
n.3
O.Q
Q.O
0*0
Run 2
Run 3
tltratlon _ 2nd titrationf <0.2 ml
—
Signature of reviewer or supervisor
A4
Volume of blank and sample titrated should be the same; otherwise a
volume correction must be made.
Figure 5.2. Method 8 analytical data form.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 9 of 17
NH2S04 *
£• *±
,
Ba(ClO4)2 ml Ba(C104)2 Equation 5-4
where
= calculated normality of Ba(ClO..)0, N,
Q £•
NH so = normality of standard H2S04, N, and
ml Ba(ClO.)9 = volume of Ba(ClOA)9 required to titrate
H2S04, ml.
The chemical reaction for this standardization is shown in
Equation 5-5. The Ba reacts preferentially with S04~ in
solution to form a highly insoluble BaS04 precipitate. When
++ = ++
the Ba has reacted with all of the SO, , the excess Ba
++
reacts with the thorin indicator (x ) to form a metal salt of
the indicator and to give a color change.
Ba + + SO ~ + thorin (x++) -* BaS04 + thorin (Ba++) Equation 5-5
(yellow) (pink)
The standardized Ba(ClO4)2 should be protected from
evaporation of the isopropanol at all times. Note: It is
suggested that the analyst unfamiliar with this titration
carry out titrations on aliquots of low, medium, and high
concentrations in the following manner:
1. Pipette 3.0-, 10. 0-, and 20 -ml aliquots of 0.01N
H2SO4 into three 250-ml Erlenmeyer flasks.
2. Dilute each to 25 ml with distilled water.
3. Add a 100-ml volume of 100% isopropanol and two to
four drops of thorin indicator to each flask.
4. Titrate with Ba(ClO4)2 to become familiar with the
endpoint.
5.2.5 Control Samples - The accuracy and precision of the
sample analysis should be checked. The accuracy of the
analysis technique is determined by control samples; the
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 10 of 17
precision, by duplicate analyses of both the control and the
field samples. Acceptable accuracy and precision should be
demonstrated on the analysis of the control samples prior to
the analysis for the field samples.
Each control sample should be prepared and analyzed in
the following manner:
1. Dry the primary standard grade ammonium sulfate
((NH4)2S04) for 1 to 2 h at 110°C (230°F), and cool in a desic-
cator.
2. Weigh, to the nearest 0.5 mg, 1.3214 g of primary
standard grade (NH4)2S04.
3. Dissolve the reagent in about 1800 ml of distilled
water in a 2-& volumetric flask.
4. Dilute to the 2-£ mark with distilled water. The
resulting solution is 0.01N (NH4)2S04.
5. Enter all data on the form shown in Figure 5.3.
6. Pipette 25 ml of the control sample into each of
four 250-ml Erlenmeyer flasks, and prepare a 25-ml blank of
distilled water in a fourth 250-ml Erlenmeyer flask. Note;
Each control sample will contain 16.5 mg of ammonium sulfate.
7. Add 100 ml of reagent grade isopropanol and two to
four drops of thorin indicator to each flask.
8. Initially titrate the blank to a faint pink endpoint
using the standardized Ba(Cl04)2. The blank must contain
<0.5 ml of titrant; otherwise, the distilled water is
unacceptable for use in this method.
9. Titrate two of the control samples with the stand-
ardized Ba(ClO4)2 to a faint pink endpoint, using the blank
endpoint that persists for at least 30 s. All titrations
should be done using a white background.
10. If the titrant volumes from the first two control
samples agree within 0.2 ml, the average of the two values can
be used to complete the calculations shown in Figure 5.3. If
the agreement is not within 0.2 ml, titrate the third control
sample. If the third titrant volume agrees within 0.2 ml of
either of the first two samples, use the two titrant volumes
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 11 of 17
Plant
$ciJ
Analyst
/?.
Date analyzed
NBa(Cl04)2
Weight of ammonium sulfate is 1.3214 gram?
Dissolved in 2 Si of distilled water?
6/£ S
~ '
Titration of blank Q.O ml Ba(ClO4)2
(must be less than the 0.5 ml titrant)
Control
Sample
Number
/
Time of
Analysis
24 h
0930
Titrant volume, ml
1st
ir-o
2nd
AS--O
3rd
Ave.
zr-o
(Two consecutive volumes must agree within 0.2 ml)
ml Ba(C10 ) x N
z
25 ml x 0.01N
(control sample) (control sample)
- O
N =
(must agree within +5%, i.e., 0.233 to 0.268)
Does value agree? yes no
Signature of analyst
Signature of reviewer
Figure 5.3. Control sample analytical data form.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 12 of 17
that are consistent for the remaining calculations. When this
criterion cannot be met with the first set of two control
samples, the analyst should follow the same procedure on a
second set of two control samples.
11. If the criterion cannot be met for the second set of
control samples, the analyst should have the analytical
techniques observed by a person knowledgeable in chemical
analysis.
12. After consistent titrant volumes are obtained, the
calculation of the analytical accuracy should be completed, as
shown in Figure 5.3. If the measured value is within +5% of
the stated value, the technique is considered acceptable, and
the field samples may be analyzed. When the +5% accuracy
cannot be met, the barium perchlorate must be restandardized,
or the control sample must be checked until the accuracy
criterion of the control sample analysis can be obtained.
The 5% accuracy limit is based on the control limit from EPA
audits discussed in Section 3.5.8.
13. The recommended frequency for analysis of control
samples is the following:
a. Analyze two control samples each analysis day
immediately prior to analysis of the actual collected source
samples.
b. Analyze two control samples after the last col-
lected source sample is analyzed each analysis day.
14. Enter results from the control sample analyses on
Figure 5.3 and submit Figure 5.3 with the source test report
as documentation of the quality of the source test analysis.
5.2.6 Sample Analysis - Check the level of liquid in the
container, determine whether any sample was lost during
shipment, and note this on Figure 4.3. Figure 5.4 can be used
to check analytical procedures. If a noticeable amount of
leakage has occurred, follow the alternative method prescribed
below. Approval should have been requested prior to testing
in case of subsequent leakage. The alternative method is as
follows:
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 13 of 17
Reagents
Normality of sulfuric acid standard* Q. Q too
Date of purchase £ /7 jy-g Date standardized
Normality of barium perchlorate titrant* fi. p >
Date standardized 9
Normality of control sample* (
Date prepared
Volume of burette* ppr> Graduations 0. I
Sample Preparation
Has liquid level noticeably changed? JQ^
Original volume U/fl Corrected volume AJ
Sulfuric acid samples diluted to 250 ml?* ^
Sulfur dioxide samples diluted to 1000 ml?*
Analysis
Volume of aliquots analyzed* /Q m/ S>Q^ ion »%*-/
Do replicate titrant volumes agree within 1% or 0.2 ml?
Number of control samples analyzed j
Are replicate control samples within 0.2 ml?
Is accuracy of control sample analysis +4%?
All data recorded? ^,?z Reviewed by
Most significant items/parameters to be checked.
Figure 5.4. Posttest operations.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 14 of 17
1. Mark the new volume level of the sample.
2. Transfer the sample to a 100-ml volumetric flask.
3. Put water in the sample storage container to the
initial sample mark, and measure the initial sample volume
4. Put water in the sample storage container to the
mark of the transferred sample, and measure the final volume
(V
soln
i
5. Use Equation 5-6 to correct the sample volume
(VSQln) if the final volume (Vgoln ) is >50% of the initial
volume.
V
soln1 soln
where
soln.
solnf
Equation 5-6
Vsoln' = samPle volume that will be used for the sample
calculations, ml,
Vsoln = total v°lume of solution in which the sample
is contained, ml,
Vsoln = init;i-al sample volume placed in sample storage
i container, ml, and
V , = final sample volume removed from sample storage
f container, ml.
6. Report both the corrected and the uncorrected values
to the Agency, and proceed with the applicable analysis listed
below.
Sulfuric acid mist (including SO3) analysis - Proceed
with the analysis as follows:
1. Shake the container holding the isopropanol solution
and the filter. If the filter breaks up, allow the fragments
to settle for a few minutes before removing a sample.
2. Pipette a 100-ml aliquot of this solution into a
250-ml Erlenmeyer flask.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 15 of 17
3. Add two to four drops of thorin indicator, and
titrate to a pink endpoint using 0.0100N Ba(ClO4)2.
4. Repeat the titration with a second aliquot from the
same sample. Replicate titrant volumes should be within 1% or
0.2 ml, whichever is greater. If the titrant volumes do not
meet this criterion, repeat analyses on new aliquots until two
consecutive titrations agree within 1% or 0.2 ml, whichever is
greater.
5. Record all data on Figure 5.2. The consistent
titrant volumes should be averaged and used as V. in subse-
quent calculations. All analytical data must then be reviewed
by an individual familiar with procedures. The review of the
data will also be noted on Figure 5.2. Note; Protect the
0.0100N Ba(C104)2 solution from evaporation at all times.
Sulfur dioxide analysis - Proceed with the S02 analysis
as follows:
1. Thoroughly mix the solution in the container holding
the contents of the second and third impingers.
2. Pipette a 10-ml aliquot of the sample into a 250-ml
Erlenmeyer flask.
3. Add 40 ml of isopropanol and two to four drops of
thorin indicator.
4. Titrate to a pink endpoint using 0.0100N Ba(ClO4)2.
Note; Protect the 0.0100N Ba(ClO4)2 solution from evaporation
at all times. Repeat titration with a second aliquot from the
same sample. Replicate titrant volumes should be within 1% or
0.2 ml, whichever is greater. If the titrant volumes do not
meet this criterion, repeat analyses on new aliquots until two
consecutive titrations are within 1% or 0.2 ml, whichever is
greater.
5. Record all data on the Method 8, Figure 5.2. The
consistent titrant volumes should be averaged and used as Vt
in subsequent calculations. All analytical data must then be
reviewed by an individual familiar with procedures. The
review of the data should also be noted on Figure 5.2.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 16 of 17
Blanks - Prepare blanks by adding two to four drops of
thorin indicator to 100 ml of 80% isopropanol. Titrate the
blanks in the same manner as the samples. Record on
Figure 5.2 in the space provided.
To aid the analyst or reviewer in a method of checking
the analytical steps or procedures, the posttest operations form
Figure 5.4 is given.
-------
Section No. 3.7.5
Revision No. 0
Date May 1, 1979
Page 17 of 17
Table 5.1. ACTIVITY MATRIX FOR POSTSAMPLING OPERATIONS
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Sampling
Apparatus
Dry gas meter
Within +5% of pretest
calibration factor
Make three runs at
one intermediate ori-
fice setting and at
highest vacuum of
test (Sec. 3.7.2)
Recalibrate
and use cali-
bration factor
that gives
lower sample
volume
Meter thermome-
ter
Within +6°C (10.8°F) at
ambient temperature
Compare with mercury-
in-glass thermometer
after each test
Recalibrate
and use higher
temperature
for calcula-
tions
Barometer
Within +5.0 mm (0.2 in.)
Hg at ambient pressure
Compare with mercury-
in-glass barometer
after each test
Recalibrate
and use lower
barometric
values for
calculations
Analysis
Reagents
Prepare according to
Sec. 3.7.5
Prepare and/or stand-
ardize within 24 h of
analysis
Prepare new
solutions and/
or restan-
dardize
Control sample
Titrants differ by £0.2
ml; analytical results
within +5% of stated
value
Before and after
analysis of field
samples
Prepare new
solutions and/
or restan-
dardize
Sample analysis
Titrants differ by <1%
or 0.2 ml, whichever is
greater
Titrate until two or
more aliquots agree
within 1% or 0.2 ml,
whichever is greater;
review all analytical
data
Void sample
if any two
consecutive
titrations
do not meet
criterion
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 1 of 10
6.0 CALCULATIONS
Calculation errors due to procedural or mathematical
mistakes can be a large component of total system error.
Therefore, it is recommended that each set of calculations be
repeated or spot-checked, preferably by a team member other
than the one who performed the original calculations. If a
difference greater than typical round-off error is detected,
the calculations should be checked step by step until the
source of error is found and corrected. A computer program is
advantageous in reducing calculation errors. Use a computer
program that prints the input data back out so that it can be
checked. If a standardized computer program is used, the
original data entry should be checked; if differences are
observed, a new computer run should be made. Table 6.1 at the
end of this section summarizes the quality assurance
activities for calculations.
Calculations should be carried out retaining at least one
decimal figure beyond that of the acquired data and should be
rounded after final calculation to two significant digits for
each run or sample. All rounding of numbers should be in
accordance with the ASTM 380-76 procedures. Record all
calculations on Figures 6.1A or B and on Figures 6.2A or B, or
on similar forms, following the nomenclature list.
6.1 Nomenclature
The nomenclature is used in the calculations that follow
this alphabetical list,
2 2
An = Cross-sectional area of nozzle, m (ft ).
B = Water vapor in the gas stream, proportion by
volume.
CH qo = Sulfuric acid (including SCO concentration,
W2 U4 g/dscm (Ib/dscf). J
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 2 of 10
, = Sulfur dioxide concentration, g/dscm (Ib/dscf).
2
I = Percent of isokinetic sampling, %.
N = Normality of Ba(ClO4)2 titrant, g-eq/£.
= Barometric pressure at the sampling site, mm
(in.) Hg.
P = Absolute stack gas pressure, mm (in.) Hg.
s
= Standard absolute pressure, 760 mm (29.92 in.)
Hg.
T = Average absolute dry gas meter temperature,
m K (°R).
T = Average absolute stack gas temperature,
S
Tstd = standard absolute temperature, 293K (528°R).
V = Volume of sample aliquot titrated, 100 ml for
H2S04 and 10 ml for S02 .
V, = Total volume of liquid collected in impingers
and silica gel, ml.
V = Volume of gas sample measured by dry gas meter,
m dcm (dcf).
V /o^-a-i - Volume of gas sample measured by the dry gas
* ' meter and corrected to standard conditions, dscm
(dscf).
V = Average stack gas velocity calculated by Method
2, using data from Method 8, m/s (ft/s).
V , = Total volume of solution in which the H^SO. or
S02 sample is contained, 250 ml or 1000 ml?
respectively .
V. = Volume of Ba(ClO.,)0 titrant used for the sample,
L. -i ft /.
ml .
V. , = Volume of barium perchlorate titrant used for
the blank, ml.
Y = Dry gas meter calibration factor.
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 3 of 10
6.2
AH = Average pressure drop across orifice meter, mm
(in.) H20.
0 = Total sampling time, min.
13.6 = Specific gravity of mercury.
60 = s/min.
100 = Conversion to percent.
Calculations
The following are the formulas used to calculate the
concentrations of sulfuric acid mist (including S03 and S02)
along with the calculation forms (Figures 6.1A, 6.IB, 6.2A,
and 6.2B) used to record the data.
6.2.1 Dry Sample Gas Volume, Corrected to Standard Conditions •
Correct the sample volume measured by the dry gas meter to
standard conditions 20°C and 760 mm (68°F and 29.92 in. Hg) by
using Equation 6-1. The average dry gas meter temperature and
average orifice pressure drop are obtained by averaging the
field data (see Figure 4.1).
V
m(std)
/T \
,r / std\
» I TmJ
AH
Pbar + 1376
Pstd
Equation 6-1
= K
AH
1376
-1 v~
1 m
where
K-, = 0.3858 K/mm Hg for metric units, or
= 17.64°R/in. Hg for English units.
Note: If the leakage rate observed during any mandatory leak
check exceeds the specified acceptable rate, the tester should
either correct the value of V in Equation 6-1 (as described
m
in Reference Method 5) or invalidate the test run.
-------
Sample Volume
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 4 of 10
Y =/.£/£, AH= /.0ef in. H00
— — ^* __ _« __ ^/
in. Hg
v,sta • ».«« vm vl
P + (AH/13. 6)
Equation 6-1
Sulfuric Acid Mist (Including S03) Concentrations
N = -.0^00 g-eg/fc, Vt =
=. ml
V
soln
' Va = ^ ^^-^ m1' Vm
std
Equation 6-2
N(Vt -
= 1.081 x 10
~4
~^
2 4
V
= .0/15* 10"4 Ib/dscf
— —
m
std
Figure 6.1A. Sulfuric acid mist (including S03) calculation
form (English units).
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 5 of 10
vm =
Sample Volume
&1. 4 m' T = 3 QLl K' p = ./_/ *, AH = ^ £. 0 mm.
Equation 6-1
V = 0.3858 V Y
mstd m
bar
m
- L-JLIO nr
Sulfuric Acid Mist (Including SO-) Concentrations
N * .0/00 g-eg/£, v
— . ... _. . -
, V., = Q>Q_& ml
~~ •• *—
v
soln
. ml, Va =
, V
m
std
Equation 6-2
= 0.04904
2 4
N(Vt -
V
m
std
= -QJYS 1 g/dscm
Figure 6.IB. Sulfuric acid mist (including SO.,)
calculation form (metric units).
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 6 of 10
Sample Volume
y =
ft3,
= /_./? in. H20
= _. in. Hg
V = 17.64 Vm Y
mstd m
bar
m
Equation 6-1
Sulfuric Acid Mist (Including SO.,). Concentrations
N = .j
V
soln
ml
v - _/£..£ ml,
Equation 6-2
= 7.061 x 10
-5
V_
=^-_/77 x 10"4 Ib/dscf
m
std
Figure 6.2A. Sulfur dioxide calculation form (English units).
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 7 of 10
Sample Volume
vm = £-
Y = J_.Q 24.' AH =
Hg
H2°
Equation 6-1
P. + (AH/13. 6)
V = 0.3858 V, Y
mstd m
m
-]-*«
SO- Concentration
N = .O I OO g-eg/H, V. = / 1 . £4 ml, V,, = 0. OZm.1
_ — — _ -^ -^ — — — tD — — —
V
soln
' m1' va = /^--
Equation 6-2
Cor. = 3.203 X 10
oL/«
-2
N(vt - vtb)
V.
m
std
g/dscm
Figure 6.2B. Sulfur dioxide calculation form (metric units)
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 8 of 10
6.2.2 Volume of Water Vapor and Moisture Content - Calculate
the volume of water vapor and moisture content of the stack
gas as described in Sections 6.4 and 6.5 of Method 5,
respectively.
6.2.3 Sulfuric Acid Mist (Including SCs) Concentration
CH2S04 K2!
N (V - V )
Vsoln "
L I J
Vm(std)
Equation 6-2
where
K2 = 0.04904 g/meg for metric units, or
= 1.081 x 10 Ib/meq for English units.
6.2.4 Sulfur Dioxide Concentration -
'SO,
= K,
V
N Vt - Vtb
soln
V
a J
m(std)
Equation 6-3
where
K3 = 0.03203 g/meq for metric units, or
= 7.061 x 10 Ib/meq for English units.
6.2.5 Isokinetic Variation (I) in Raw Data -
I =
r
Ts|K4Vlc +
^m
LTm
r i AH
ibar 13.6
jx 100
Equation 6-4
60 e vsPsAn
where
K. = 0.003464 mm Hg-m /ml-K for metric units, or
= 0.002676 in. Hg-ft3/ml-°R for English units.
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 9 of 10
6.2.6 Isokinetic Variation (I) in Intermediate Values -
Cation 6-5
"
TStd 60 e VsPsAn
T \7
s m(std)
= KB 0 VsPsAn
where
K5 = 4.320 for metric units, or
= 0.09450 for English units.
6.3 Acceptable Results
If 90% <_ I £ 110%, the results are acceptable. If the
results are low in comparison with the standards and if the I
is beyond the acceptable range, the administrator may opt to
accept the results. Otherwise, the results may be rejected
and the test repeated. It is suggested that, for Method 8
tests, the data not be rejected only because of noncompliance
with isokinetic requirements.
-------
Section No. 3.7.6
Revision No. 0
Date May 1, 1979
Page 10 of 10
Table 6.1. ACTIVITY MATRIX FOR CALCULATION CHECKS
Characteristics
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Analysis data
form
All data and calcula-
tions given
Visually check
Complete
missing
data values
Calculations
Difference between
check and original cal-
culations not to exceed
round-off error; retain
at least one decimal
figure beyond that of
acquired data
Repeat all calcula-
tions, starting with
raw data for hand cal-
culations; check all
raw data input to com-
puter calculations;
hand calculate one
sample/test
Indicate
errors on
analysis data
form, Fig.
6.3
Isokinetic
variations
90% < I < 110%
For each traverse
point, calculate I
Repeat test
and adjust
flow rates
to maintain
I within 10%
variation
-------
Section No. 3.7.7
Revision No. 0
Date May 1, 1979
Page 1 of 3
7.0 MAINTENANCE
The normal use of emission testing equipment subjects it
to corrosive gases, extremes in temperature, vibrations, and
shocks. Keeping the equipment in good operating order over an
extended period of time requires a knowledge of the equipment
and a program of routine maintenance which is performed
3 3
quarterly or after 28.4 m (1000 ft ) of operation, whichever
is greater. In addition to the quarterly maintenance, a
yearly cleaning of the entire meter box is recommended.
Maintenance procedures for the various components are
summarized in Table 7.1 at the end of this subsection.
The following procedures are not required, but are
recommended to increase the reliability of the equipment.
7.1 Pumps
In the present commercial sample train, several types of
pumps are used. The two most common are the fiber vane pump
with in-line oiler and the diaphragm pump. The fiber vane
pump requires a periodic check of the oiler jar; its contents
should be translucent at the time of filling and at each
periodic check, and it is recommended that the oil be changed
if it is not translucent. Use the oil specified by the
manufacturer; if none is specified, use SAE 10, nondetergent
oil. Whenever the fiber vane pump starts to run erratically
or during the yearly disassembly, the head should be removed,
and the fiber vanes should be changed. Erratic operation of
the diaphragm pump is normally due either to a bad diaphragm,
which will cause leakage, or to malfunction of the valves,
which should be cleaned annually by complete disassembly of
the train.
7.2 Dry Gas Meters
The dry gas meter should be checked for excess oil or
corrosion of the components by removing the top plate every
-------
Section No. 3.7.7
Revision No. 0
Date May 1, 1979
Page 2 of 3
3 mo. The meter should be disassembled, and all components
should be cleaned and checked when the rotation of the dials
is erratic, when the meter will not calibrate properly over
the required flow rate range, and during yearly maintenance.
7.3 Sample Train
All remaining sample train components should be checked
visually every 3 mo and disassembled completely and cleaned or
replaced yearly. Many of the items such as quick disconnects
should be replaced when damaged rather than checked periodi-
cally. Normally, the best procedure for maintenance in the
field is to use another entire unit such as a meter box,
sample box, or umbilical cord (the hose that connects the
sample box and the meter box) rather than to replace
individual components.
7.4 Inclined Manometer
The fluid in the inclined thermometer should be changed
whenever there is discoloration or visible matter in the fluid
and during the yearly disassembly. No other routine main-
tenance is required since the inclined manometers will be leak
checked during both the leak check of the Pitot tube and the
leak check of the entire control console.
-------
Section No. 3.7.7
Revision No. 0
Date May 1, 1979
Page 3 of 3
Table 7.1. ACTIVITY MATRIX FOR EQUIPMENT MAINTENANCE CHECKS
Apparatus
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Routine main-
tenance
No erratic behavior
Routine maintenance
quarterly. Disas-
semble and clean
yearly
Replace parts
as needed
Fiber vane pump
In-line oiler free of
leaks
Periodic check of
oiler jar; remove
head and change fiber
vanes
Replace as
needed
Diaphragm pump
Leak-free valves func-
tioning properly
Clean valves during
yearly disassembly
Replace when
leaking or
malfunctioning
Dry gas meter
No excess oil, corro-
sion, or erratic rota-
tion of the dial
Check every 3 mo for
excess oil or corro-
sion by removing top
plate. Check valves
and diaphragm when
meter dial runs er-
ratically or when me-
ter will not cali-
brate
Replace parts
as needed, or
replace meter
Inclined mano-
meter
No discoloration or
visible matter in the
fluid
Check periodically
during yearly disas-
sembly
Replace parts
as needed
Sample train
No damage
Visually check every
3 mo and completely
disassemble and clean
or replace yearly
If failure
noted, use
another entire
control con-
sole, sample
box, or
umbilical cord
Nozzle
No dents, corrosion, or
other damage
Visually check before
and after each test
run
Use another
nozzle or
clean out,
sharpen, and
recalibrate
-------
Section No. 3.7.8
Revision No. 0
Date May 1, 1979
Page 1 of 7
8.0 AUDITING PROCEDURE
An audit is an independent assessment of data quality.
Independence is achieved if the individual(s) performing the
audit and their standards and equipment are different from the
regular field crew and their standards and equipment. Routine
quality assurance checks by a field team are necessary in
generation of good quality data, but they are not part of the
auditing procedure. Table 8.1 at the end of this, section
summarizes the quality assurance functions for auditing.
Based on the results of a collaborative test2 of Method
8, two specific performance audits are recommended:
1. Audit of the analytical phase of Method 8, and
2. Audit of data processing.
It is suggested that a systems audit be conducted as specified
by the quality assurance coordinator, in addition to these
performance audits. The two performance audits and the
systems audit are described in detail in Subsections 8.1 and
8.2, respectively.
8.1 Performance Audits
Performance audits are made to quantitatively evaluate
the quality of data produced by the total measurement system
(sample collection, sample analysis, and data processing). It
is recommended that these audits be performed by the respon-
sible control agency once during every enforcement source
test. A source test for enforcement comprises a series of
runs at one source. The performance audit of the analytical
phase is subdivided into two steps: (1) a pretest audit which
is optional and (2) an audit during the actual analysis of the
field samples which is required.
8.1.1 Pretest Audit of Analytical Phase Using Aqueous
Ammonium Sulfate (Optional) - The pretest audit
described in this subsection can be used to determine the
-------
Section No. 3.7.8
Revision No. 0
Date May 1, 1979
Page 2 of 7
proficiency of the analyst and the standardization of
solutions in the Method 8 analysis and should be performed at
the discretion of the agency auditor. The analytical phase of
Method 8 can be audited with the use of aqueous ammonium
sulfate samples provided to the testing laboratory before the
enforcement source test. Aqueous ammonium sulfate samples may
be prepared by the procedure described in Section 3.7.5 on
control sample preparation.
The pretest audit provides the opportunity for the
testing laboratory to check the accuracy of its analytical
procedure. This audit is especially recommended for a
laboratory with little or no experience with the Method 8
analysis procedure described in this Handbook.
The testing laboratory should provide the agency/organi-
zation requesting the performance test with a notification of
the intent to test 30 days prior to the enforcement source
test. The testing laboratory should request that the
agency/organization provide the following performance pretest
audit samples: two samples at a low concentration (500 to
1000 mg SO2/dscm of gas sampled or approximately 10 to 20 mg of
ammonium sulfate/sample) and two samples at a high
concentration (1500 to 2500 mg S02/dscm of gas sampled or
about 30 to 50 mg of ammonium sulf ate/sample). At least 10
days prior to the time of the enforcement source test, the
agency/organization should provide the four audit samples.
The concentration of the two low and the two high audit samples
should not be identical.
The testing laboratory will analyze one sample at the low
concentration and one at the high concentration, and submit
their results to the agency/organization prior to the
enforcement source test. (Note; The analyst performing this
optional audit must be the same analyst audited during the
field sample analysis described in Subsection 8.1.2 below).
The agency/organization determines the percent accuracy,
%A, between the measured SO2 concentration and the audit or
known values of concentration. The %A is a measure of the
-------
Section No. 3.7.8
Revision No. 0
Date May 1, 1979
Page 3 of 7
bias of the analytical phase of Method 8. Calculate %A using
Equation 8-1.
C (M) - C (A)
- ?_ - 2 - Equation 8-1
so2
x
where
C_o (M) = concentration measured by the lab analyst
2 mg/ml , and
CSQ (A) = audit or known concentration of the audit
2 sample, mg/ml.
The recommended control limit for the pretest audit is the
90th percentile value for %A based on the results of three
audits (11/77, 5/78, and 10/78) performed by the Environmental
Monitoring and Support Laboratory, USEPA, Research Triangle Park,
6 7
North Carolina. ' By definition, 90% of the laboratory partici-
pants in the audit obtained values of %A less than the values
tabulated below. The control limit is expected to be exceeded by
10% of the laboratories to be audited, based on these three
audits. The 90th percentile values and the known audit concen-
trations are given below for each concentration range, 500 to
1000 mg SO2/dscm and 1500 to 2500 mg SOVdscm.
500 to 1000 mg SCU/dscm
Known audit
concentration, 90th percentile for %A,
Audit date mg SO?/dscm _ % _
5/78 686 4.1
10/78 572 6.4
1500 to 2500 mg SO2/dscm
Known audit
concentration, 90th percentile for %A ,
Audit date mg SCU/dscm _ ^ _
11/77 1411 6.6
11/77 2593 4.0
5/78 2479 4.5
5/78 1907 4.5
10/78 2555 4.9
10/78 1754 5.2
-------
Section No. 3.7.8
Revision No. 0
Date May 1, 1979
Page 4 of 7
Based on the results of these audits, the recommended 90th per-
centile control limit for pretest audits is 7% for both con-
centration ranges.
If the results of the pretest audit exceed 7% the agency/
organization should provide the correct results to the testing
laboratory. After taking any necessary corrective action, the
testing laboratory should then analyze the two remaining samples
and report the results immediately to the agency/organization
before the enforcement source test analysis.
8.1.2 Audit of Analytical Phase Using Aqueous Ammonium
Sulfate (Required) - The agency should provide two
audit samples to be analyzed along with the field samples from
the enforcement source test. The purpose of this audit is to
assess the data quality at the time of the analysis. The
percent accuracy of the audit samples is determined using
Equation 8-1. The results of the calculated %A should be
included in the enforcement source test report as an
assessment of accuracy of the analytical phase of Method 8
during the actual enforcement source test.
8.1.3 Audit of Data Processing - Calculation errors are
prevalent in Method 8. Data-processing errors can be deter-
mined by auditing the data recorded on the field and
laboratory forms. The original and audit (check) calculation
should agree within roundoff; if not, all of the remaining
data should be checked. The data processing may also be
audited by providing the testing laboratory with specific data
sets (exactly as would occur in the field) and by requesting
that the data calculation be completed and that the results be
returned to the agency/organization. This audit is useful in
checking both computer programs and manual methods of data
processing.
8.2 Systems Audit
A systems audit is an on-site qualitative inspection and
review of the total measurement system (sample collection,
-------
Section No. 3.7.8
Revision No. 0
Date May 1, 1979
Page 5 of 7
sample analysis, data processing, etc.). Initially, a systems
audit is recommended for each enforcement source test, defined
here as a series of three runs at one source. After the test
team gains experience with the method, the frequency of audit
may be reduced—once for every four tests.
The auditor should have extensive background experience
in source sampling, specifically with the measurement system
being audited. The functions of the auditor are summarized in
the following:
1. Inform the testing team of the results of pretest
audits, specifying any area(s) that need special attention or
improvement.
2. Observe procedures and techniques of the field team
during sample collection.
3. Check/verify records of apparatus calibration checks
and quality control used in the laboratory analysis of control
samples from previous source tests, where applicable.
4. Record the results of the audit and forward them
with comments to the team management so that appropriate
corrective action may be initiated.
While on site, the auditor observes the source test team's
overall performance including the following specific
operations:
1. Setting up and leak testing the sampling train.
2. Preparing and adding the absorbing solution to the
impingers.
3. Checking for isokinetic sampling.
4. Purging the sampling train.
Figure 8.1 is a suggested checklist for the auditor.
-------
Section No. 3.7.8
Revision No. 0
Date May 1, 1979
Page 6 of 7
Presampling Preparation
Yes No Comment
I. Knowledge of process conditions
r 2. Calibration of pertinent equipment, in particular,
the dry gas meter, prior to each
field test
On-site Measurements
^ 3. Leak-testing of sampling train after sample run
4. Preparation and addition of absorbing solutions
to impingers
5. Isokinetic sampling
6. Purging of the sampling train and rinsing of the
impingers and connecting tubes to recover the
sample
7. Recording of pertinent process condition during
sample collection
8. Maintaining the probe at a given temperature
Postsampling
9. Control sample analysis - accuracy and precision
OK. 10. Sample aliquotting techniques
OK 11. Titration technique, particularly endpoint
precision
12. Use of detection blanks in correcting field
sample results
13. Calculation procedure/check
14. Calibration checks
15. Standard barium perchlorate solution
General Comments
3
Xcdt J*t
Figure 8.1 Method 8 checklist to be used by auditors.
-------
Section No. 3.7.8
Revision No. 0
Date May 1, 1979
Page 7 of 7
Table 8.1. ACTIVITY MATRIX FOR AUDITING PROCEDURE
Audit
Acceptance limits
Frequency and method
of measurement
Action if
requirements
are not met
Analytical phase
of Method 8
using aqueous
ammonium sul-
fate
The measured value of
the pretest audit sam-
ple should be less than
the 90th percentile
value, 7%
Once during every en-
forcement source test,
measure reference sam-
ples and compare with
their true values
Review oper-
ating techni-
que
Data-processing
errors
The original and check
calculations should
agree within round-off
error
Once during every en-
forcement source test,
perform independent
calculations, start-
ing with recorded
data
Check and
correct all
data for the
source test
Systems audit--
observance of
technique
Operation technique de-
scribed in this section
of the Handbook
Once during every en-
forcement test until
experience gained;
then every fourth
test. Observation of
technique, assisted
by audit checklist,
Fig. 8.1
Explain to
team its
deviations
from recom-
mended tech-
niques , and
note on
Fig. 8.1
-------
Section No. 3.7.9
Revision No. 0
Date May 1, 1979
Page 1 of 1
9.0 RECOMMENDED STANDARDS FOR ESTABLISHING TRACEABILITY
To achieve data of desired quality, two considerations
are necessary: (1) the measurement process must be in a state
of statistical control at the time of the measurement, and (2)
the systematic errors, when combined with the random variation
(errors of measurment), must result in a small uncertainty.
To ensure good quality data, it is necessary to perform
quality control checks and independent audits of the measure-
ment process; to document these checks and audits by recording
the results on quality control charts, as appropriate; and to
use materials, instruments, and measurement procedures that
can be traced to an appropriate standard of reference.
Data must be routinely obtained by repeat measurements of
control standard samples and working standards. The working
calibration standards should be traceable to standards that
are considered to be primary. Two primary standards
recommended for establishing traceability are:
1. Dry gas meter should be calibrated against a wet
test meter that has been verified by an independent liquid
displacement meter, as described in Section 2.1.1.
2. Barium perchlorate should be standardized against
sulfuric acid that has already been standardized with primary
grade potassium acid phthalate. Then standardized barium
perchlorate should be validated with an aqueous ammonium
sulfate to make the titrant solution traceable to two primary
standard grade reagents.
-------
Section No. 3.7.10
Revision No. 0
Date May 1, 1979
Page 1 of 4
10.0 REFERENCE METHOD*
METHOD 8—DETERMINATION or Sauuftic ACID Moi
ASI> SuLrua DIOXIDE EMiisiONs FROM Sr_noNKRY
Sou lie £i
1, l^ineipie and Applicability
1 l 1'nnciplp A gas sample ii eitractad Isold net Ically
from the stack. The sul.'unc acid mist {Including sulfur
tnoxidi) end the sulfur dioxide are separated, and both
fractious are measured separately by the banuni-thonn
Utrat ion method.
1.2 Applicability. This method is applicable for the
determination of sulfuric acid mist (including sulfur
trioiide, and in the absence of other paniculate matter)
and suHur dioxide omissions Irom stationary sources.
Collaborative tests have shown that the minimum
detectable limits of the method are 0 OS milligrams/cubic
meter (003> I0~r pounds/cubic foot) tor sulfur trioiid*
and 1 2 n.g/m> (0 74 10-' Ih/ftn for sulfur dioiide. No
upper Imuu have been established. Uased on theoretical
calculations tar 2UO niilhUters of 3 percent hydrogen
peroitde sol at ion, the upper concentration limit for
sulfur dioxide HI a 1 U m> (35.3 ft1) gas sample is about
12.500 rnK/ru> (77xi0~* Ib.'fl*). The upper limit can be
extended by increasing the quantity of peroxide solution
in '.he un pi tigers.
Possible interfering agents of this method are fluorides,
free ammonia, and dimethyl aniline. If any of these
interfering agents are present (this can be determined by
knowledge of the process), alternative methods, subject
to the approval of the Administrator, are required.
Filterable paniculate matter may IHJ determined along
with SOi and SOj (subject to the appruval of the Ad-
rrJniatrAtor), however, ih* proci-dure us*rd for paniculate
matter must b« consistent with the spexlficailons and
procedures given In Mithod 5
2 Apparatus
'.* 1 Sampling A schematic of the sampling train
used IQ this method ts shown In Figure *-!; It Is similar
to the .Method 5 train vsccpi that the filler position is
different and the Otter holdiT dot's not have to w heated.
Commercial models of this tram are available. For thow
who desire to build their own. however, complete con-
st run ton details are discritx-U lit APTDAVH Changes
from the Al'TD-U'41 document and allowable modi-
ncallons to Figure 8-1 are dbcusMrd In the following
subsections.
The operating and maintenance procedures for the
sampling tnUnurudrsulUMi In Al'TD-0576. Since correct
it&uge la Important In obtaining valid results, all users
should nud thu Al'TI>-057fl dwtirr.fiit and adopt the
opi'ratlng and maintenance pr>M.iiiurvs outlined In ft,
unless otherwlM! sp*Tific
-------
Section No. 3.7.10
Revision No. 0
Date May 1, 1979
Page 2 of 4
U.I Wash Bottle*. Polyethylene or flax, MO ml.
(two).
1.1.1 Graduated Cylinder*. 1M ml, 1 UVer. (Vohr
metric flasks may also be used.)
JJ.I Storage Bottles. Leak-free polyethylene bottles,
lOOn ml lite (two lor etch sampUni run).
2.2 4 Trip Balance SOfHrram capacity, to measure to
±0.5 ( (neCMsary only U a moisture content analyst! la
to be done).
2.3 Analysis
2.3.1 Pipettes. Volumetric 2S ml, 100ml.
2.3.2 Burretle.tOml.
2.3.3 Erie nmeyer Flask. 250 ml. (one for each sample
blank and standard).
2.3.4 Graduated Cylinder. 100 ml.
2 3.5 Trip Balance. HO I capacity, to measure to
.
2.3.6 Dropping Bottle. To add Indicator solution,
124-ml site.
\ Unless otherwise indleelpd, all reagent.1 are to conform
to the specifications established by the Committee on
Analytical ReogenU of the American Chemical Society,
where such specifications are available. Otherwise, use
the best available trade,
8.1 Sampling.
a 1.1 Fillers Same as Method 5, Section 3.1.1.
J.I. 2 Blllca Gel. Same as Method 6. Section 3.1.2.
3.1.3 Water. Delonlied, distilled to conform to A8TM
specification D11W-74, Type 3. At the option of the
analyst, the KMnOj test for ozldiiable organic matter
may be omitted when high concentrations of organic
matter are not eipected to be present.
1.1.4 Isopropanol. «0 Percent. Mil «00 ml of Isopro-
puol with 900 ml of delonlied, distilled water.
Noti.—Experience has shown that only A.C.B. (trade
Isopropanol Is satlsfartory. Tests have shown that
Isopropaool obtained from commercial sources occa-
caslooally has peroxide Impurities that will cause er-
roneously high rulfurlc acid mist measurement. Use
the following test for detecting peroildes In each lot of
laopropanol: Bbake 10 ml of the Isopropanol with 10 ml
of freshly prepared 10 percent potassium Iodide solution.
Prepare a blank by similarly treating 10 ml of distilled
water. After 1 minute, read the absorbance on a speetro-
pbotometer at 252 nanometers. If tho absorbanee exceeds
0.1. the Isopropanol shall not be used. Peroxides may be
removed from Isopropanol by redistilling, or by peonage
through a column of activated alumina. However, re-
agent-grade Isopropanol with suitably low peroxide levels
Is readily available from commercial sources; therefore,
rejection of contaminated lots may be more efficient
than following the peroxide removal procedure.
3.1 5 Hydrogen Peroxide, 3 Percent. Dilute 100 ml
of 30 percent hydrogen peroxide to 1 liter with deJonised,
dlatilled water. Prepare fresh dally.
8.1.11 Crushed Ice.
1.2 Sample Recovery.
3J.I Water. Same as 3.1.3.
8.2.2 Isopropanol, 80 Percent. Same as 3.1.4.
3.3 Analysis.
3.31 Water. Same as 3.1.3.
3 3.2 Isopropanol, 100 Percent.
3 3.3 Thorln Indicator. l-(o-arsonophenylaso)-2-napb-
thol-3. 6-dlsulfonJc acid, disodlum salt, or equivalent.
Dissolve 0 20« In 100 ml of delonlted. distilled water
1.3 4 Barium Perehlorale (0 0100 Normal). Dissolve
l.Kig of barium perchlorate trinydrate(Ba(C10<)>-3HiO)
In 200 ml detonlied. distilled water, and dilute to 1 liter
with Isopropanol: 1 23 g of barium chloride dlhydrate
(BaClf2HrO) may be used Instead of the barium per-
chlorale. Standardise wKh sulfurlc acid as In Section 9.2.
This solution must be protected against evaporation at
all times.
3.3.5 Sulfuric Acid Standard (0.0100 N). Purchase or
standardise to ±00002 N agamst 0.0100 N NsOK that
has previously been standardised against primary
standard potassium acid phthalate.
4. Prorrrfurc
4.1 Sampling.
4.1.1 Pretest Preparation Follow the procedure out-
lined in Method 5, Section 4.1.1; niters should be in-
spected, but need not be desiccated, weighed, or Identl-
nod. If the effluent gas ran be considered dry, I.e., mois-
ture free, the silica gel need not be weighed.
4.1.2 Preliminary Determinations. Follow the pro-
cedure outlined in Mot hod 5, Section 4 1.2.
4.1.3 Preparation of Collection Tram. Follow the pro-
cedure outlined in Method 5, Sertinn 4.1 3 (eicept for
the second paragraph and other obviously inapplicable
parts) and use r iirure 8-1 instead of Figure 5-1. Replace
the second pwnftiph with Place 100 ml of 80 percent
Isopropanol in the first Impmger, 100 ml of 3 percent
hydrogen peroxide in both the second and third 1m-
pingers: retain a portion of each reagent for use as a
blank solution. Place about 200g of silica gel In the fourth
iniDinaer.
PLANT.
LOCATION
OPERATOR
DATE
RUN NO
SAMPLE BOX NO..
METER BOX N0._
METER4H,?
C FACTOR
PITOT TUBE COEFFICIENT, Cp.
STATIC PRESSURE, mm H| (I*. H|)
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
ASSUMED MOISTURE, X
PROBE LENGTH, m (ft)
SCHEMATIC OF STACK CROSS SECTION
NOZZLE IDENTIFICATION NO
AVERAGE CALIBRATED NOZZLE DIAMETER, cm (in.).
PROBE HEATER SETTING
LEAK RATE, m3/min,(cfm).
PROBE LINER MATERIAL __
FILTER NO.
TRAVERSE POINT
NUMBEF,
TOTAL
AVERAGE
SAMPLING
TIME
(9), min.
VACUUM
mm H|
(in. H|)
STACK
TEMPERATURE
(Ts).
°C (*F)
VELOCITY
HEAD
(APS),
mrarl20
(in. HjO)
PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE
METER,
mmHjO
(in. HjO)
GAS SAMPLE
VOLUME.
m3 (ft3)
GAS SAMPLE TEMPERATURE
AT DRY GAS METER
INLET,
°C (°F)
Avg
OUTLET.
°C («FI
Avg
Avg
TEMPERATURE
OF GAS
LEAVING
CONDENSER OR
LAST IMPINGER.
oc (Op,
Figure 8-2. Field data.
-------
Section No. 3.7.10
Revision No. 0
Date May 1, 1979
Page 3 of 4
NOTI.—If molstun content Is to b« determined by
impinger analysis, weigh each of the first three implngers
(plus absorbing solution) to the nearest 0.5 g and record
these weights. The weight of the silica gel (or silica gel
plus container) must also be determined to the nearest
0.5 g and recorder.
4.1.4 Pretest Leak-Check Procedure. Follow the
basic procedure outlined in Method 5, Section 4.1.4.1,
noting that the probe heater shall be adjusted to the
minimum temperature required to prevent condensa-
tion, and also that verbage such as, plugging the
inlet to the ftlter holder • • '," shall be replaced by,
plugging the inlet to the first impinger • • V"
The pretest leak-check is optional.
4.1.5 Train Operation. Follow the baiie procedures
outlined In Method 9, Section 4.1.5, in conjunction with
the following special instructions. Data shall be recorded
on a sheet similar to the one In Figure W. The sampling
rat* shall not exceed 0.030 ra'/min (1.0 cfm) during the
run. Periodically during the test, observe the connecting
line between the probe and first impinger for slgnt of
condensation. If It does occur, adjust the probe heater
setting upward to the minimum temperature required
to prevent condensation. If component changes become
necessary during a run, a leak-check shall be done Im-
mediately before each change, according to the procedure
outlined In Section 4.1.4.2 of Method i (with appropriate
modifications; as mentioned In Section 4.1.4 of this
method); record all leak rates. If the leakage rated)
exceed the specified rate, the tester shall either void the
run or shall plan to correct the sample volume as out-
lined In Section 6.3 of Method 5. Immediately after com-
ponent changes, leak-checks are optional. If these
leak-checks are done, the procedure outlined in Section
4.1.4.1 of Method 5 (with appropriate modifications)
shall be used.
After turning off the pump and recording the final
readings at the conclusion of each run, remove the prone
from the stack. Conduct a post-test (mandatory) leak-
check as in Section 4.1.4.3 of Method 5 (with appropriate
modification) and record the leak rate. If the post-test
leakage rate exceeds the specified acceptable rate, the
tester shall either correct the sample volume, as outlined
in Section 8.3 of Method 5, or shall void the run.
Drain the tee bath and, with the probe disconnected,
purge the remaining part of the train, by drawing clean
ambient air through the system for 15 minutes at the
average flow rate used for sampling.
NOTI.—Clean ambient air can be provided by passing
air through a charcoal filter. At the option of the tester,
ambient air (without cleaning) may be used.
4.1.6 Calculation of Percent Isokinetic. Follow the
procedure outlined in Method 9, Section 4.1.9.
4.2 Sample Recovery.
4.2.1 Container No. 1. If a moisture content analysis
is to be done, weigh the first impinger plus contents to
the nearest 0.5 g and record this weight. ^
Transfer the contents of the first Impinger to a 250-ml
graduated cylinder. Rinse the probe, first impinger, all
connecting glassware before the filter, and the front half
of the filter holder with 80 percent Isopropanol. Add the
rinse solution to the cylinder. Dilute to 250 ml with 80
percent isopropanol. Add the filter to the solution, mix,
and transfer to the storage container. Protect the solution
against evaporation. Mark the level of liquid on het
container and identify the sample container.
4.2.2 Container No. 2. If a moisture content analysis
Is to be done, weigh the second and third Implngers
(plus contents) to the nearest 0.$ g and record these
weights. Also, weigh the spent silica gel (or silica gel
plus Impinger) to the nearest 0 J g.
Transfer the solutions from the second and third
Implngers to a 1000-ml graduated cylinder. Rinse all
connecting glassware (Including back half of filter holder)
between the filter and silica gel Impinger with deionlzed,
distilled water, and add this rinse water to the cylinder.
Dilute to a volume of 1000 ml with deionlied, distilled
water. Transfer the solution to a storage container. Mark
the level of liquid on the container. Seal and identify the
sample container.
4.3 Analysis.
Note the level of liquid In containers 1 and 2, and con-
firm whether or not any sample was lost during ship-
ment; note this on the analytical data sheet. If a notice-
able amount of leakage has occurred, either void the
sample or use methods, subject to the approval of the
Administrator, to comet the final results. •
4.3.1 Container No. 1. Shake the container holding
the Isopropanol solution and the filter. If the filter
breaks up, allow the fragments to settle for a few minutes
before removing a sample. Pipette a 100-ml aliquot of
this solution into a 250-ml Erlenmeyer flask, add 2 to 4
drops of thortn Indicator, and titrate to a pink endpolnt
using 0.0100 N barium perchlorate. Repeat the titration
with a second aliquot of sample and average the titration
values. Replicate tltntions matt agree within 1 percent
or 0.3 ml, whichever Is greater.
U.2 Container No. 2. Thoroughly mix tbe solution
In the container holding the contents of the second and
third Impinger*. Pipette a 10-ml aliquot of sample Into a
MO-inl Erlenmeyer flask. Add ml of Isopropanol. 2 to
4 drops of tborin Indicator, and titrate to a pink endpolnt
using 0.0100 N barium perchlorate. Repeat the titration
with a second aliquot of sample and average the titration
values. Replicate tltrations must agree within 1 percent
or 0.2 ml. whichever Is greater.
4.3.3 Blanks. Prepare blanks by adding 2 to 4 drops
of thortn Indicator to 100 ml of 80 percent isopropanol.
Titrate tbe blanks In the same manner as the samples.
o. CWttrottm
5.1 Calibrate equipment using the procedures speci-
fied In the following sections of Method 5: Section 5J
(metering system); Section S.S (temperature gauges);
Section 9.7 (barometer). Note that the recommended
leak-check of the metering system, described in Section
5.« of Method 9, also applies to this method.
5.2 Standardise the barium perchlorate solution with
25 ml of standard sulfurlc acid, to which 100 ml of 100
percent Isopropanol has been added.
Note.— Carry oat calculations retaining at least one
extra decimal figure beyond that of the acquired data.
Round off figures after final calculation.
(.1 Nomenclature.
X.- Cross-sectional ana of nostle, m> (ft1).
B..-Water vapor in the gas stream, proportion
by volume.
CHdOi-SuUuric acid (Including SOi) concentration,
g/dscm Ob/dscf).
CSOi-Sulfur dioxide concentration, g/dscm Ob/
dscf).
/•Percent of Isokinetic sampling.
W- Normality of barium perchlorate titrant, g
equivalents/liter.
^bar-Barometric pressure at tbe sampling site,
mm Eg (in. Hg).
P,-Absolute stack gas pressure, mm Hg (In.
Pstd- Standard absolute pressure, 760 mm Hg
(29.92 In. Hg).
7".- Average absolute drygas meter temperature
(aeeFlgure 8-2), • K (" R).
r.-Average absolute stack gu temperature (see
Figure 8-8), ° K <° R). _
TVtd- Standard absolute temperature, 213* E
(938s R).
V.- Volume of sample aliquot titrated, 100 ml
tor HiSOi and 10 ml for SOi.
V,, -Total volume of liquid collected In Impinge"
and silica gel, ml.
V.- Volume of gas sample as measured by dry
gas meter, ocm (dcf).
V.Cstd) -volume of gas sample measured by the dry
gas meter corrected to standard conditions,
oscm (dscf).
•.—Average stack gas velocity, calculated by
Method 2, Equation 2-9, using data obtained
from Method 8, m/sec (ft/sec).
Vsoln- Total volume of solution in which the
sulfurlr acid or sulfur dioxide sample is
contained, 2SO ml or 1,000 ml, respectively.
Vi- Volume of barium perchlorate titrant used
for the sample, ml.
Vn-Volume of barium perchlorate titrant used
lor tbe blank, ml.
y-Dry gas meter calibration factor.
AH- Average pressure drop across orifice meter,
mm (In.) HK>.
6 -Total sampling time, mln.
13.6-8peciflc gravity of mercury.
60-sec/mln.
100— Conversion to percent.
6.2 Average dry gas meter temperature and average
orifice pressure drop. See data sheet (Figure 8-2).
8.3 Dry Oas Volume. Correct the sample volume
measured by the dry gas meter to standard conditions
(20° C and 780 mm Hg or 68° F and 29.92 In. Hg) by using
Equation 8-1.
culate the moisture content of the stack gas, using Equa-
tion 9-3 of Method 5. Tbe "Note" in Section 6 5 of Method
9 also applies to this method. Note that if the effluent gas
stream can be considered dry, the volume of water vapor
and moisture content need not be calculated.
6.9 Sulfuric acid mist (including SOi) concentration.
--K,-
Equation 8-2
iv here:
lft-0.04904 g/milliequlvalent for metric unite.
-l.OSlXlO-Mb/meq for English units.
6.6 Sulfur dioxide concentration.
Cso,
Vm(tu
Equation 8-3
where:
iTi- 0.03203 r/meq for metric units.
-7.081X10-*lb?meq for English units.
6.7 Isokinetic Variation.
6.7.1 Calculation from raw data.
WtV.P.A,
Equation 8-4
where:
Jft-0.003464 mm Hg-m'/ml-'K for metric units.
-0.002676 In. Hg-ftVml-'R for English units.
8.7.2 Calculation from Intermediate values.
T.Vm(.u
P.v.A.ad-B..)
/>„,+ ( Ag/13.6)
- - -
Equation 8-1
where*
Jif^O.SgSS'K/mm Hg for metric units.
' -17.04 °R/i.n. Hg for English units.
NOTI.— If the leak rate observed during any manda-
tory leak-checks exceeds the specified acceptable rate,
the tester shall either correct the value of V. In Equation
8-1 (as described In Section M of Method 5), or shall
Invalidate tbe test run.
6.4 Volume of Water Vapor and Moisture Content.
Calculate the volume of water vapor using Equation
6-2 ft Method 5; the weight of water collected in the
Implngers and silica gel can be directly converted to
mllUliters (the specific gravity of water is 1 (/ml). Cal-
Equation 8-5
where:
£i-4.320 for metric units.
-0.09450 for English units.
6.8 Acceptable Results. If 90 percent
-------
Amendment to Reference Method 8; Correction*
Section No. 3.7.10
Revision No. 0
Date May 1, 1979
Page 4 of 4
In Method 8 of Appendix A, Sections
1.2, 2.32. 4.1.4, 4.2.1, 4.3.2, 6.1, and 6.7.1
we amended as follows:
1. In Section 1.2, the phrase "U.S.
EPA," is Inserted in the fifth line of
the second paragraph between the
words "Administrator," and "are."
Also, delete the third paragraph and
insert the following:
Filterable participate matter may be de-
termined along with SO, and SOt (subject to
the approval of the Administrator) by in-
•citing a heated glass fiber filter between
the probe and isopropanol impinger (see
Section 2.1 of Method 6). If this option is
chosen, particulate analysis is gravimetric
only; HiSO. acid mist Is not determined sep-
arately:
2. In Section 2.3.2, the word "Bur- i
rette" is corrected to read "Burette."
3. In Section 4.1.4, the stars "• • •"
are corrected to read as periods ". . .".
4. In Section 4.2.1, the word "het" on
the eighth line of the second para-
graph is corrected to read "the."
5. In Section 4.3.2, the number "40"
is inserted in the fourth line between
the words ."Add" and "ml."
6. In Section 6.1, Nomenclature, the
following are corrected to read as
shown with subscripts "CVW, C,o2.
P»«. P«d. T«*. VmUM), and V^."
7. In Section 6.7.1. Equation 8-4 is
corrected to read as follows:
100 T, [tt ¥,c • (VJT/T,)(%,,.•* iH/13.6)]
60 8 V. P. A.
(Sees. Ill, 114. 301(a), Clean Air Act
amended (42 U.S.C. 7411. 7414. 7601).)
CFR Doc. 78-7686 Filed 3-22-78; 8:45 am]
*Federal Register, Vol. 43, No. 57-March 23, 1978
-------
Section No. 3.7.11
Revision No. 0
Date May 1, 1979
Page 1 of 1
11.0 REFERENCES
1. Buchanan, J. W., and D. E. Wagoner. Guidelines
for Development of a Quality Assurance Program:
Volume VII - Determination of Sulfuric Acid Mist
and Sulfur Dioxide Emissions from Stationary
Sources. EPA-650/4-74-005-g. Environmental Pro-
tection Agency, Research Triangle Park, N.C.,
March 1976.
2. Hamil, H. F., D. E. Camann, and R. E. Thomas.
Collaborative Study of Method for the Determina-
tion of Sulfuric Acid Mist and Sulfur Dioxide
Emissions from Stationary Sources.
EPA-650/4-75-003, Environmental Protection Agency,
Research Triangle Park, N.C. 1974.
3. Driscoll, J., J. Becker, and R. Herbert. Valida-
tion of Improved Chemical Methods for Sulfur Oxide
Measurements from Stationary Sources.
EPA-R2-72-105. National Environmental Research
Center, Research Triangle Park, N.C.
4. Martin, R. M. Construction Details of Isokinetic
Source Sampling Equipment. Publication No.
APTD-0581. Air Pollution Control Office, Environ-
mental Protection Agency, Research Triangle Park,
N.C. 1971.
5. Rom, J. J. Maintenance, Calibration, and Opera-
tion of Isokinetic Source Sampling Equipment.
Publication No. APTD-0576. Office of Air
Programs, Environmental Protection Agency,
Research Triangle Park, N.C. 1972.
6. Fuerst, R. G., R. L. Denny, and M. R. Midgett. A
Summary of Interlaboratory Source Performance Sur-
veys for EPA Reference Methods 6 and 7 - 1977.
Available from U.S. Environmental Protection
Agency, Environmental Monitoring and Support
Laboratory (MD-77), Research Triangle Park, N.C.
27711.
7. Fuerst, R. G. and M. R. Midgett. A Summary of In-
terlaboratory Source Performance Surveys for EPA
Reference Methods 6 and 7 - 1978. Report in pre-
paration by U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory
(MD-77), Research Triangle Park, N.C. 27711.
-------
Section No. 3.7.12
Revision No. 0
Date May 1, 1979
Page 1 of 20
12.0 DATA FORMS
Blank data forms are provided on the following pages for
the convenience of the Handbook user. Each blank form has the
customary descriptive title centered at the top of the page.
However, the section-page documentation in the top right-hand
corner of each page of other sections has been replaced with a
number in the lower right-hand corner that will enable the
user to identify and refer to a similar filled-in form in a
text section. For example, Form M8-1.2 indicates that the
form is Figure 1.2 in Section 3.7.1 of the Method 8 Handbook.
Future revisions of these forms, if any, can be documented by
1.2A, 1.2B, etc. Sixteen of the blank forms listed below are
included in this section. Five are in the Method Highlights
subsection as shown by the MH following the form number.
Form Title
1.2 Procurement Log
2.3A and 2.3B Meter Box Calibration Data and Calculation
Form (English and metric units)
2.4A and 2.4B Posttest Meter Calibration Data Form
(English and metric units)
2.5 (MH) Pretest Sampling Checks
2.6 Nozzle Calibration Form
3.1 (MH) Pretest Preparations
4.1 Method 8 Field Data Form
4.2 Sample Label
4.3 Sample Recovery and Integrity Data
4.4 (MH) On-Site Measurements
5.1 (MH) Posttest Sampling Checks
5.2 Method 8 Analytical Data Form
5.3 Control Sample Analytical Data Form
5.4 (MH) Posttest Operations
-------
Section No. 3.7.12
Revision No. 0
Date May 1, 1979
Page 2 of 20
Form Title
6.1A and 6.IB Sulfuric Acid Mist Calculation Form
(English and metric units)
6.2A and 6.2B Sulfur Dioxide Calculation Form
(English and metricunits)
8.1 Method 8 Checklist to be Used by Auditors
-------
PROCUREMENT LOG
Item description
Qty.
Purchase
order
number
Vendor
Date
Ord.
Rec.
Cost
Dispo-
sition
Comments
Quality Assurance Handbook M8-1.2
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM
(English units)
Date
Barometric pressure, P,
in. Hg.
Meter box number
Calibrated by
Orifice
manometer
setting
(AH),
in. H20
0.5
1.0
1.5
2.0
3.0
4.0
Wet test
meter
fl3
5
5
10
10
10
10
Gas volume
Dry gas
meter
(vd),
ft3
Temperature
Wet test
meter
°F
Dry gas meter
Inlet Outlet Average
(t ), (t ), (t,),
di do d
°F °F °F
Time
(0),
min
Average
Y±
«d
AH
0.5
1.0
1.5
2.0
3.0
4.0
AH
13.6
0.0368
0.0737
0.110
0.147
0.221
0.294
Vw Pb(td -f 460)
i ~ AH
Vb + ife' «. + 46°>
4M . 0.0317 AH <«. + «°> 8
i P (t + 460i V
b v d H°vJ vw
If there is only one thermometer on the dry gas meter, record the temperature
under t,.
d
Quality Assurance Handbook M8-2.3A (front side)
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM
Nomenclature:
3
V = Gas volume passing through the wet test meter, ft .
3
V, = Gas volume passing through the dry test meter, ft .
t = Temperature of the gas in the wet test meter, F.
d. = Temperature of the inlet gas of the dry test meter, F.
d = Temperature of the outlet gas of the dry test meter, F.
t, = Average temperature of the gas in the dry test meter, obtained by the average t, and
td , F. i
o
AH = Pressure differential across orifice, in. t^O.
Y. = Ratio of accuracy of wet test meter to dry test meter for each run. Tolerance Y. =
1 Y +0.02 Y. 1
Y = Average ratio of accuracy of wet test meter to dry test meter for all six runs.
Tolerance Y = Y 40.01 Y.
3
AH@. = Orifice pressure differential at each flow rate that gives 0.75 ft /min of air at standard
conditions for each calibration run, in. H_0. Tolerance = AH@ +0.15 (recommended).
3
AH@ = Average orifice pressure differential that gives 0.75 ft /min of air at standard
conditions for all six runs, in. H»0. Tolerance = 1.84 +0.25 (recommended).
z
0 = Time for each calibration run, min-
P, = Barometric pressure, in. Hg.
Quality Assurance Handbook M8-2.3A (back side)
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM
(metric units)
Date
Barometric pressure, P
nun Hg.
Meter box number
Calibrated by
Orifice
manometer
setting
(AH),
mm H-O
10
25
40
50
75
100
wet test
meter
^w+273>
f(t + 273) 0
0.00117 AH w
^± - Pb (td + 273) 1^ Vw
If there is only one thermometer on the dry gas meter, record it under t
Quality Assurance Handbook M8-2.3B (front side)
-------
METER BOX CALIBRATION DATA AND CALCULATION FORM
Nomenclature:
V = Gas volume passing through the wet test meter, m .
W
Vd = Gas volume passing through the dry test meter, m .
t = Temperature of the gas in the wet test meter, °C.
d. = Temperature of the inlet gas of the dry test meter, °C.
d = Temperature of the outlet gas of the dry test meter, °C.
t. = Average temperature of the gas in the dry test meter, obtained by the average of t, and
t °C i
Li 9 V • I
0
0 = Time of calibration run, min,
AH = Pressure differential across orifice, mm H?0.
Y-J = Ratio of accuracy of wet test meter to dry test meter for each run. Tolerance Y^ =
Y +0.02 Y.
Y = Average ratio of accuracy of wet test meter to dry test meter for all six runs.
Tolerance Y = Y +0.01 Y.
AH@. = Orifice pressure differential that gives 0.021 m of air at standard conditions for each
1 calibration run, mm H?0. Tolerance AH@^ = AH@ +3.8 mm H?0 (recommended).
AH@ = Average orifice pressure differential that gives 0.021 m3 of air at standard conditions
for all six runs, mm H^O. Tolerance AH@ = 46.74 +_6.3 mm H2U (recommended).
P. = Barometric pressure, mm Hg.
Quality Assurance Handbook M8-2.3B (back side)
-------
POSTTEST METER CALIBRATION DATA FORM (English units)
Test numbers
Date
Meter box number
Plant
Barometric pressure, P,
in. Hg Dry gas meter number
Pretest Y
Orifice
manometer
setting,
(AH),
in H20
Gas volume
wet test
meter
(v>
3
ftJ
10
10
10
Gas volume
dry gas
meter
(vd)
ftJ
Temperature
Wet test
meter
-------
POSTTEST METER CALIBRATION DATA FORM (metric units)
Test numbers
Date
Meter box number
Plant
Barometric pressure, P,
mm Hg Dry gas meter number
Pretest Y
Orifice
manometer
setting,
(AH),
mm H20
Gas volume
wet test
meter
-------
NOZZLE CALIBRATION
Date
Calibrated by
Nozzle
identification
number
Dr
mm, (in.)
D2'
mm, (in.)
D3'
mm, (in. )
AD,
mm, (in.)
avg
where:
D, ,»,_,= nozzle diameter measured on a different diameter, mm (in.)
Tolerance = measure within 0.25 mm (0.001 in.).
AD = maximum difference in any two measurements, mm (in.).
Tolerance = 0.1 mm (0.004 in.).
D
avg = average of D,, D_, D_,
Quality Assurance Handbook M8-2.6
-------
METHOD 8 FIELD TFST DATA FORM
Plant
Location
Operator
Date
Run number
Sample box number
Meter box number
Meter AH@
Meter calibration
Pitot tube CP
Probe length
Probe liner material
Probe heater setting
Ambient temperature
Barometric pressure
Assumed moisture
Static pressure
C factor
Reference AP
Maximum AH
Sheet
of
Nozzle identification number
Nozzle diameter
Final leak rate
Vacuum during leak check
Remarks:
Traverse point
number
Total or
Avg
Sampling
time
(9) ,
min
Clock
time
24 h
Vacuum,
mm Hg
(in. Hg)
Stack
temperature
«*&!•
Velocity
head
(AP > ,
mm H,O
(in. H20)
Pressure
differential
across
orifice
meter,
mm H,O
(in. H20)
Gas sample
volume,
m3 (ft3)
Gas sample temperature
at dry gas meter
*?ft)
Outlet,
*C (8F)
Temperature
of gas
leaving
condenser or
last impinger,
5C (°F)
Quality Assurance Handbook M8-4.1
-------
SAMPLE LABEL
Plant _ City _
Site _ Sample type _
Date _ Run number _
Front rinse D Front filter D Front solutionD
Back rinsed Back filter Q Back solutionD
Solution _ Level marked D w
Volume: Initial Final
Cleanup by _
-------
Plant
SAMPLE RECOVERY AND INTEGRITY DATA
Sample location
Field Data Checks
Sample recovery personnel
Person with direct responsibility for recovered samples
Sample
number
1
2
3
Blanks
Sample
identification
number
H2S04
so2
Date
of
recovery
Liquid
level
marked
Stored
in locked
container
Remarks
Signature of field sample trustee
Laboratory Data Checks
Lab person with direct responsibility for recovered samples
Date recovered samples received
Analyst
Sample
number
1
2
3
Blanks
Sample
identification
number
H2S04
so2
Date
of
analysis
Liquid
at marked
level
Sample
identified
Remarks
Signature of lab sample trustee
Quality Assurance Handbook M8-4.3
-------
METHOD 8 ANALYTICAL DATA FORM
Plant
Date
Sample location
Volume and normality of
barium perchlorate
Analyst
1.
2.
Blank
ml Ba(C10.)_
H t.
ml Ba(ClO,)^ N =
H /
ml Ba(ClO,)~
V
soln
Sulfur Trioxide Analysis
- Total volume of solution in which the
sulfuric acid sample is contained, ml
V - Volume of sample aliquot, ml
3.
V - Volume of barium perchlorate
titrant used for sample, ml
1st titration
2nd titration
Average
Run 1
Run 2
Run 3
V * - Volume of barium perchlorate 1st titration
titrant used for blank, ml 2nd titration
Average
1st titration = gg • titration _ 2nd titrationl < 0.2 ml
2nd titration ' ' —
Sulfur Dioxide Analysis
V 1 - Total volume of solution in which the
n sulfur dioxide sample is contained, ml
V - Volume of sample aliquot, ml
SL
V - Volume of barium perchlorate
titrant used for sample, ml
1st titration
2nd titration
Average
v , * - Volume of barium perchlorate 1st titration
titrant used for blank, ml 2nd titration
Average
Run 1
Run 2
Run 3
1st titration
2nd titration
Signature of analyst
= 0.99 to 1.01 or 11st titration - 2nd titration| £0.2 ml
Signature of reviewer or supervisor
Volume of blank and sample titrated should be the same; otherwise a
volume correction must be made.
Quality Assurance Handbook M8-5.2
-------
Plant
CONTROL SAMPLE ANALYTICAL DATA FORM
Date analyzed
Analyst
N.
Ba(Cl04)2
Weight of ammonium sulfate is 1.3214 gram?
Dissolved in 2 S, of distilled water?
Titration of blank ml Ba(ClO4)?
(must be less than the 0.5 ml titrant)
Control
Sample
Number
Time of
Analysis
24 h
Titrant volume
1st
2nd
3rd
ml
Ave.
(Two consecutive volumes must agree within 0.2 ml)
ml Ba(C10 ) x N , . = 25 ml x 0.01N
v 4'2 (control sample) (control sample)
ml x
N =
(must agree within +3J£, i.e., 0.233 to 0.268)
Does value agree? yes no
Signature of analyst
Signature of reviewer
Quality Assurance Handbook M8-5.3
-------
Sulfuric Acid Mist (Including S03) Calculation Form
(English units)
Sample Volume
V = . ft3, Tm = ._ °R, Pbar = . in. Hg
Y = _. , AH = _. in. H20
Equation 6-1
P
- 17.64 VY = . ft
std
Sulfuric Acid Mist (Including SO.,) Concentrations
N = . g-egA, V. = . ml, Vtfa = _. ml
V n = . ml, V = . ml, V = . ft3
soln a m
Equation 6-2
CH S0 = 1.081 x 10~4\ „• f= . X 10"* Ib/dscf
2 ' mstd '
Quality Assurance Handbook M8-6. 1A
-------
Sulfuric Acid Mist (Including SO-) Calculation Form
(metric units)
Sample Volume
Vm = -'
' Tm - --- •- K' Pbar
_ _ _•_ ^^ ^9
Y = . , AH = . mm. H.,0
*"" ' — " ~~~ """" ~~" """"
Equation 6-1
V = 17.64 V Y
m
std
m
bar
m
m
Sulfuric Acid Mist (Including S03) Concentrations
N = ._
soln
g-eg/£, V
. ml, V
ml, vtb = _. ml
3. ~~ ~"~ *"*
. ml, V.
m
m
std
Equation 6-2
= 0.04904
2 4
N(Vt -
v
m
std
Quality Assurance Handbook M8-6.1B
-------
Sulfur Dioxide Calculation Form
(English units)
Sample Volume
Vm =
ft3,
in. Hg
Y = _. , AH = _. in. H20
V = 17.64 VY
mstd m
bar
m
Equation 6-1
^3
Sulfuric Acid Mist (Including SCO Concentrations
N = ._
soln
_ _ g-eg/A, Vt
. ml, V
; Vtb = _._ _ ml
a
ml,
Equation 6-2
Cco = 7.061 x 10
ovJ«
-5
V
m
std
x 10 4 Ib/dscf
Quality Assurance Handbook M8-6.2A
-------
Sulfur Dioxide Calculation Form
(metric units)
Sample Volume
Vm = -••
Y = .
mT = TC
_ ' m _*_ '
, AH = .mm H~o
mm Hg
Equation 6-1
V = 0.3858 V Y
m
std
m
Pbar + (AH/13.6)
m
m
SO2 Concentration
N = .
V
g-eg/A, Vt
. ml, V.
ml, V.. = _. ml
soln ' '""' va '-
ml,
C_ = 3.203 x 10
-2
V
Equation 6-2
= _._ _ _ g/dscm
m
std
Quality Assurance Handbood M8-6.2B.
-------
METHOD 8 CHECKLIST TO BE USED BY AUDITORS
Presampling Preparation
Yes No Comment
1. Knowledge of process conditions
2. Calibration of pertinent equipment, in particular,
the dry gas meter, prior to each
field test
On-site Measurements
3. Leak-testing of sampling train after sample run
4. Preparation and addition of absorbing solutions
to impingers
5. Isokinetic sampling
6. Purging of the sampling train and rinsing of the
impingers and connecting tubes to recover the
sample
7. Recording of pertinent process condition during
sample collection
8. Maintaining the probe at a given temperature
Postsampling
9. Control sample analysis - accuracy and precision
10. Sample aliquotting techniques
11. Titration technique, particularly endpoint
precision
12. Use of detection blanks in correcting field
sample results
13. Calculation procedure/check
14. Calibration checks
15. Standard barium perchlorate solution
General Comments
Quality Assurance Handbook M8-8.1
-------
TECHNICAL REPORT DATA
/Please read Inunctions on the reverse before completing
1 RE=OHT MO
EPA-600/4-77-027b
3. RECIPIENT'S ACCESSI Of* NO.
4. TITLE AMD SUBTITLE
QUALITY ASSURANCE HANDBOOK FOR AIR POLLUTION MEASURE-
MENT SYSTEMS, VOLUME III - STATIONARY SOURCE SPECIFIC
METHODS
5. REPORT DATE
May 1979
6. PERFORMING ORGANIZATION CODE
Darryl J. von Lehmden, U.S. EPA, RTP, NC
William G. Dewees, PEDCo-Environmental, Inc., Cin., OH
Carl Nelson. PEDCo-Environmental, Inc., Cincinnati. OH
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
U.S. Environmental Protection Agency, Environmental
Monitoring & Support Laboratory, RTP, NC 27711, and
PEDCo-Environmental, Inc., Cincinnati, Ohio 45246
10. PROGRAM ELEMENT NO.
IAD 800
11. CONTRACT/GRANT NO
68-02-2725
12. SPONSORING AGENCY NAME AND ADDRESS
Environmental Monitoring & Support Laboratory, QAB
Office of Research and Development
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
The Handbook will be reoroduced in the current format (3-ring
binder) and maintained up-to-date by a document control system operated by EMSL/RTP.
Distribution will be to personnel In EPA, and its contractors, state and selected
air pollution control agencies in foreign countries.
16. ABSTRACT
This Handbook includes quality assurance guidelines on stationary source emission
measurements. Regardless of the scope and magnitude of the stationary source emission
measurement program, there are a number of common considerations pertinent to the
production of quality data. These common parameters are discussed in Section 3.0 of
Volume III and include quality assurance guidelines in the areas of: (1) planning the
test program; (2) general factors in stationary source testinq; (3) chain-of-custody
procedure; and (4) traceability protocol for gases used for continuous source emission
monitors. The remainder of Volume III contains pollutant-specific quality assurance
guidelines. Initially Volume III includes guidelines for the following oollutant-
specific measurement systems: Section 3.5 Method 6 - determination of sulfur dioxide
emissions from stationary sources, Section 3.6 Method 7 - determination of nitrogen
oxide emissions from stationary sources, and Section 3.7 Method 8 - determination of
sulfuric acid mist and sulfur dioxide from stationary sources. Source testers and
managers responsible for stationary source emission measurements will find Volume III
useful in planning quality assurance.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Group
Quality assurance, source testing, perfor-
mance and system audits, chain-of-custody,
traceability protocol, sulfur dioxide
emission method, nitrogen oxide emission
method, sulfuric acid mist emission method
13. DISTRIBUTION STATEMENT
RELEASE TO PUBLIC
19. SECURITY CLASS {This Report/
Unclassified
21. NO. OF PAGES
404
20. SECUFflTY CLASS (This page)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
•frU.S. GOVERNMENT PRINTING OFFICE: 1979-61+0- 01? 3 9 0 9 REGION NO. 4
------- | |