-------
UTAH:
Lynn Menlove «*- Cl, «t
Bureau of Air Quality
Utah Div. of Health
150 W. N. Temple
P.O. Box 2500
Salt Lake City, Utah 84110
Telephone: (801) 533-6108
FTS: 588-*#t» fSdc
WYOMING:
Charles Collins
Air Quality Div.
Wyo. Dept. of Environmental Quality
Hathaway Bldg.
Cheyenne, Wyo. 82002
Telephone: (307) 777-7391
FTS: 328-9391
WYOMING AREA OFFICES
Lander Area:
ue
Mr. Woody Russel ^
Department of Environmental Quality
933 Main St.
Lander, Wyoming 82520
Telephone: (307) 332-3047
Sheridan Area:
Mr. Richard Schrader
Department of Environmental Quality
30 E. Grinnel St.
Sheridan, Wyoming 82801
Telephone: (307) 672-6488
-------
AUGUST 1978
LISTING OF PRINCIPAL TECHNICAL CONTACTS FOR
STATIONARY SOURCE COMPLIANCE TESTING ACTIVITIES
IN EPA HEADQUARTERS, RTP AND REGIONAL OFFICES
Full Address:
OFFICE OF ENFORCEMENT
Louis Paley
Technical Support Branch
Division of Stationary Source Enforcement (EN-341)
Environmental Protection Agency
Washington, D. C. 20460
Telephone: (202) 755-8137
FTS: 755-8137
Kirk Foster
Technical Support Branch
Division of Stationary Source Enforcement ^D-7)
Environmental Protection Agency
Research Triangle Park, N.C, 27711
Telephone: (919) 541-4571
FTS: 629-4571
OFFICE OF AIR QUALITY PLANNING AND STANDARDS
Roger Shigehara, Chief
Test Support Section
Emissions Measurement Branch (MD-19)
Emissions Standards & Engineering Division
Environmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-5276
FTS: 629-5276
Joseph McCarley, Chief
Field Testing Section
Emission Measurement Branch
Emission Standards & Engineering Division (MD-13)
Environmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-5245
FTS: 629-5245
-------
COMPLIANCE TESTING CONTACTS LIST (W>
OFFICE OF AIR QUALITY PLANNING & STANDARDS (continued)
James Dealy
Air Training Institute
Manpower & Technical Information Branch
Control Programs Development Division (MD-17)
Environmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-2401
FTS: 629-2401
0< James Jahnke, Section Manager
Northrup Services, (MD-20)
Environmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-2766
FTS: 629-2766
OFFICE OF MONITORING & TECHNICAL SUPPORT
Rodney Midgett, Chief
Source Methods Section
Quality Assurance Branch (MD-77)
Encironmental Monitoring & Support Laboratory
Environmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-2196
FTS: 629-2196
William Mitchell
Source Methods Section
Quality Assurance Branch (MD-77)
Environmental Monitoring & Support Laboratory
Encironmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-2769
FTS: 629-2769
-------
COMPLIANCE TESTING CONTACTS LIST eartt
OFFICE OF MONITORING & TECHNICAL SUPPORT (continued)
Tom Logan, Continuous Monitoring
Source Methods Section
Quality Assurance Branch (MD-77)
Environmental Monitoring & Support Laboratory
Environmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-2580
FTS: 629-2580
OFFICE OF AIR, LAND & MATER USE
James Homolya, Chief
Gaseous Emissions Research Section
Stationary Source Emissions Research Branch (MD-46)
Environmental Protection Agency
Research Triangle Park, N.C. 27711
Telephone: (919) 541-3085
FTS: 629-3085
OFFICE OF ENERGY, MINERALS & INDUSTRY
Bruce Harris
Process Measurement Branch (MD-62)
Industrial Environmental Research Laboratory
Environmental Protection Agency
Research Triangle Park, N.C. 27711
. Telephone: (919) 541-2557
FTS: 629-2557
Larry Johnson
Process Measurement Branch (MD-62)
Industrial Environmental Research Laboratory
Environmental Protection Agency
Research Triangle Park, N.C, 27711
Telephone: (919) 541-2557
FTS: 629-2557
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Gary Young
National Enforcement Investigations Center
Box 25227, Bldg. 53
Denver Federal Center
Denver, CO. 80225
Telephone: (303) 234-2336
FTS: 234-2336
-------
COMPLIANCE TESTING CONTACTS LIST-WESTERN REGIONS
REGION IV
Jerry Rom
Air Engineering Branch
Air & Hazardous Materials Division
Environmental Protection Agency
345 Courtland Street, N.E.
Atlanta, GA. 30308
Telephone: (404) 881-5552
FTS 257-2786
NORTH CAROLINA:
Michael Aldridge
Air Quality Section
North Carolina Dept. of Natural & Economic Resources
P.O. Box 27687
Raleigh, North Carolina 27611
Telephone: (919) 731-4740
WEST VIRGINIA:
Dale Farley
West Virginia Air Pollution Control Comm.
1558 East Washington St.
Charleston, West Virginia 25311
Telephone (304) 345-4022
FTS: 885-402 2
REGION V
Edwin Zylstra
Air Surveillance Branch
Surveillance & Analysis Division
Environmental Protection Agency
203 South Dearborn
Chicago, Illinois 60604
Telephone: (312) 353-2303
FTS: 353-2303
REGION VI
Phil Schwindt
Surveillance Branch
Surveillance & Analysis Division
Environmental Protection Agency
1201 Elm Street
Dallas, Texas 75270
Telephone: (214) 749-7126
JTS: 749-7126
-------
WESTERN REGIONS, (continued)
TEXAS:
Charles Goerner, Acting Chief
Source Evaluation Section
Texas Air Control Board
8520 Shoal Creek Blvd.
Austin, TX 78758
Telephone:
REGION VII
(512) 451-5711
FTS: 734-5011
Dwayne Durst, Chief
Air Surveillance Section
Surveillance & Analysis Division
Environmental Protection Agency
D6 faHtteun'Rul. «- — —- * —
Kansas City, Kansas WB
Telephone:
(816) 374-4461
FTS: 758-4461
— - JM:
•jjH -
3
, pspi
,iU 5f-
At***
REGION VIII
John Floyd
Air Surveillance Section (8S-S)
Surveillance & Analysis Division
USEPA
1860 Lincoln St.
Denver, CO 80295
Telephone: (303) 837-4261
FTS: 3 27-4261
REGION IX
WMStaNMh, Chief (or Ken Kitchingman)
Air Investigation Section
Surveillance & Analysis Division
Environmental Protection Agency
215 Fremont St.
San Francisco, CA 94105
Telephone: (415) 556-8752
FTS: 556-8752
REGION X
.arry Sims or Paul Boys
Surveillance & Investigation Branch
Surveillance & Analysis Division
Environmental Protection Agency
1200 Sixth Avenue
Seattle, Washington 98101 Telephone: (206) 422-1106 FTS: 399-1106
-------
t/l4
REVISED LISTING
STACK SAMPLING FIRMS KNOWN TO WORK IN REGION VIII
For additions, deletions or corrections contact: John R. Floyd, U. S.
Environmental Protection Agency, Surveillance Branch (8S-S), 1860
Lincoln Street, Denver, Colorado 80295. Phone FTS: 327-4261, Commercial
303-837-4261.
COLORADO Coors/Spectro - Chemical Laboratory
Division of Coors Porcelain Company
Frank B. Schweitzer, Dan Briggs
P. 0. Box 500
Golden, Colorado 80401
303-279-6565
linviro - Test, Ltd.
Liam S. Geer, Jr.
P. 0. Box 15325
8545 West Colfax Avenue
Lakewood, Colorado 80215
303-233-4082
Impact, Ltd.
Ronald Battles, R. Stephen Schermerhorn
1409 Larimer Square
Denver, Colorado 80202
303-571-1300
Stearns-Roger Corp.
Environmental Sciences Division
Dave Osborn
P. 0. Box 5888
Denver, Colorado 80217
303-758-1122 exf 3bO\
STW Testing, Inc.
Tom Fuson Q;(l
P. 0. Box 26212
1480 Hoyt
Lakewood, Colorado 80226
303-232-3299
-------
COLORADO U.S. Array - Environmental Health A.
Capt. James Stratta; Lt. Peterson
U.S. - AEHA, Rgn. Division - West
Fitzsimons Army Medical Center (FAMC)
Aurora, Colorado 80240
303-341-8881
York Research Corporation - West
Lou Grothier
7100 Broadway, Building 3A
Thornton, Colorado 80221
303-426-1582
MONTANA Yapuncich, Sanderson, and Brown Laboratories (EERC)
Ed Waddington, Dean Arthun
13 North 32nd, P.O. Box 593
Billings, Montana 59103
FTS: 585-6011, Commercial 406-252-6325
Ecology Audits, Inc.
Casper Office - Greg Smith
P.O. Box 2956
Casper, Wyoming 82602
FTS: 328-5330 (307-266-1356) Wyo.
FTS: 749-1011, Commercial 214-350-7893 - Bill Harris
Engineering-Science, Inc.
M. Dean High, Don Holtz
150 N. Santa Anita Avenue
Arcadia, California 91006
FTS: 8-508-445-7560, Commercial 213-445-7560
SOUTH Wilson Wright, Inc.
Clair C. Wilson
Pollution Division
P.O. Box 2526
Tulsa, OK 74101
FTS: 736-7011, Commercial 918-584-5819
'WYOMING
WEST
-2-
-------
EAST Corning Laboratories, Incorporated
Robert N. Corning, Gary Ochs
1922 Main Street, P. 0. Box 625
Cedar Falls, Iowa 50613
FTS: 863-2011, Commercial 319-277-2401
David Brasslau Associates, Incorporated
David Brasslau
2829 University Avenue, S.E.
Minneapolis, Minnesota 55414
FTS: 725-4242, Commercial 612-331-4571
Environmental Research Corporation
William Bosin
3725 North Dunlap Street
St. Paul, Minnesota 55112
FTS: 725-4242, Commercial 612-484-8591
Interpoll, Incorporated
Perry Lonnes, Larry Jennings
1996 West County Road C.
St. Paul, Minnesota 55113
FTS: 725-4242, Commercial 612-636-6866
Midwest Research Institute (MRI)
Paul Constant
425 Volker
Kansas City, Missouri 64110
FTS: 758-7212, Commercial 816-753-7600
Northstar Research, Division of MRI
A. E. Vandergrift
3100 38th Avenue South
Minneapolis, Minnesota 55406
FTS: 725-4242, Commercial 612-721-6373
-3-
-------
EAST (Cont.) Particle Data Laboratories, Ltd.
Meryl Jackson
115 Hohn Street
P. 0. Box 265
Elmhurst, Illinois 60126
FTS: 8-409-832-5658, Commercial 312-832-5658
Pollution Curbs, Incorporated
Frank Belgea
502 North Prior Avenue
St. Paul, Minnesota 55104
FTS: 725-4242, Commercial 612-647-0151
Research-Cottrell, Incorporated
Norm Troxell
P. 0. Box 750
Bound Brook, New Jersey 08805
FTS: 342-5500, Commercial 201-885-7000
Stephen W. Upson, Associates, Incorporated
Stephen W. Upson
2361 Wehrle Drive
Buffalo, New York 14221
FTS: 432-3311, Commercial 716-634-2105
Clean Air Engineering
835 Sterling Avenue
Palatine, IL 60067
FTS: 8-312-991-3300
Bill Walker, Pres.
-4-
-------
STACK SAMPLING CONTACTS
Bovay Engineers, Inc.
5009 Caroline St.
Houston, Texas 77004
David Braslau Associates, Inc.
2829 University Ave., S.E.
Minneapolis, MN 55414
Bucher & Willis Consulting
Engineers, Planners and
Architects
605 W. North St.
Salina, Kansas 67401
Leo A. Daly Company
8600 Indian Hills Dr.
Omaha, Nebraska 68114
Ekono, Inc.
410 Bellevue Way, S.E.
Bellevue, WA 98004
Frankfurter, Inc.
201 Elliott Ave. W.
Seattle, WA 98119
Manchester Laboratories
105 N. Franklin St.
Manchester, Iowa 52057
Wenzel & Company
4035 10th Ave., S.
Great Falls, MT 59403
Zurn Environmental Engineers
Zurn Industries, Inc.
150 North Santa Anita Ave.
Arcadia, California 91006
Pollution Curbs, Inc.
502 North Prior Ave.
St. Paul, MN 55104
Environmental Research Corp.
3725 North Dunlap St.
St. Paul, MN 55112
Interpol 1, Inc.
1996 West County Road C
St. Paul, MN 55113
Enviro-Test, Limited
1086 South Reed St.
Lakewood, CO 80226
Research-Cottrell
Box 750
Bound Brook, NJ 08805
Yapuncich, Sanderson and
Brown Laboratories
13 North 32nd
Billings, MT 59101
Coors/Spectro-Chemical Lab.
Div. of Coors Porcelain Co.
P. 0. Box 500
Golden CO 80401
ATTN: Frank B. Schweitzer
Testing & Engineering Co.
2000 E. 40th Avenue
Denver, CO 80205
Entropy Environmentalists
P. 0. Box 12291
Research Triangle Park,
NC 27709
ATTN: Walter Smith
Midwest Research Institute
425 Volker Blvd.
Kansas City, MO 64110
ATTN: A. E, Vandergrift
Particle Data Labs. Ltd.
P. 0. Box 265
Elmhurst, IL 60126
ATTN: Eric Ansley
STW Testing, Inc.
1480 Hoyt
Denver, CO 80215
Wilson Wright, Inc.
Pollution Division
Box 2526
Tulsa, OK 74101
ATTN: Clair C. Wilson
York Research Corp.-West
7100 Broadway, Bldg. 3A
Denver, CO 80221
Sierra Research Corp.
Box 3007
Boulder, CO 80302
Stearns-Roger
Environmental Sciences Div.
Box 5888
Denver, CO 80217
ATTN: Don S, Packnett
Alan M. Vorhees & Assoc.Inc.
1751 Williams St.
Denver, CO 80218
The Ken R. White Co.
3955 E. Exposition Ave.
Suite 300
Denver, CO 80209
IMPACT, Ltd.
1409 Ltd.
Denver, CO 80202
ATTN: Ronald Battles
Stephen W. Upson,
Associates, Inc.
2361 Wehrle Drive
Buffalo, NY 14221
ATTN: Stephen W. Upson
Capt. James Strada
US AEHA - West
Fitzsimons Army Medical
Center
Denver, CO 80240
n/i5/76 £
-------
^«0,x
\
? UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
» "V
WASHINGTON. D.C. 20460
August 18, 1977
MEMORANDUM
SUBJECT: Transmittal of Technical Reports on New Developments in
Emission Measurement Methodology
TO: Regional and State Compliance Testing Contacts
This mailing is the start of what hopefully will be a continuing
program of direct information exchange between the headouarters and
research offices of EPA, and the technical staffs of EPA regional
offices and state air pollution control agencies involved in monitoring
or conducting emission tests of stationary sources for compliance
purposes. Emission testing has been aptly characterized as a highly
dynamic and changing field that is raDidlv becoming less of an art and
more of a science. A large-scale research and study effort is carried
on by the EPA offices in Research Triangle Park, North Carolina, for the
purposes of developing better test methods and techniques for more re-
liable and rapid emission measurements. The technical data and infor-
mation gained from this major research program are used in making
continued improvements and refinements to the EPA reference methods
and procedures for performance testing.
It is important that field enforcement personnel stay abreast of
new developments and changing concepts in emission measurement method-
ology. Timely receipt of EPA reports and publications dealing with
test methodology research should be helpful to the regional and state
source-testinq staff in this regard. Comments received from persons
attending the Compliance Testing Workshops held by the Regional offices
and the Division of Stationary Source Enforcement confirm the need for
a better flow of information to field personnel. The workshops have
also helped us identify key persons responsible for the review and
evaluation of performance or complia.ice tests in each of the EPA Regional
offices and the majority of the state agencies. A mailing list has been
compiled of the names and addresses of those individuals serving as the
principal coordinators for stationary-source compliance-testing activities
in each of the offices. In turn, the various EPA offices engaged in
test method development and evaluation have agreed to make a concerted
effort to include the persons listed as Compliance Testing Coordinators
in the initial distribution of both in-house and contract technical re-
ports judged to be of possible interest to field enforcement personnel.
Henceforth, on a monthly basis, if possible, these reports will be sent
to the designated persons as copies become available. Conversely, any
comments or suggestions that the field personnel would care to make
concerning the reported information or other research needs in this
technical area would of course be appreciated and welcomed by the RTP
programs.
-------
- 2 -
In receiving the technical reports, it must be remembered that
the majority of them are prepared by EPA contractors or other non-
EPA organizations working under EPA's general direction and guidance.
Although the reported data are usually thoroughly reviewed by the
sponsoring EPA program, the findings may not necessarily reflect or
represent the views or policies of the agency. For example, it is
common for the sponsoring program to release one or more "interim
report" documents when the study is complex and lengthly in order to
make the data and preliminary findings immediately available to the
technical community. Naturally, the conclusions or findings contained
in these preliminary reports may be subject to change in the final
report. Moreover, as with all scientific publications the technical
soundness and overall acceptability of a report or research paper can
only be determined over a period of time bv further examination and
testing by knowledgeable persons in the emission measurement field.
Nevertheless, having access to current and update information, even if
not time-tested, should aid field enforcement personnel in their
application of reference test methods and interpretation of results,
particulary where other guidance is not readily available for handling
novel and difficult sampling situations frequently encounted in the field.
If the proper person in your organization is not receiving the
technical reports, please notify either Kirk Foster, DSSE (MD-7), EPA
Research Triangle Park, N. C. 27711, Telephone: (919) 541-4571 / FTS:
629-4571; or Lou Paley, DSSE (EN-341), EPA, 401 M. Street, Washington,
D. C. 20460, Telephone: (202) 755-8137 / 755-8137.
We encourage you, as the primary person selected to receive this
information for your program, office or agency, to make every effort
to see that the information is promptly circulated to other "persons in
your organization having a need to know. Usually, only limited quantities
of these publications are printed by the sponsoring EPA program, and
generally only one copy can be made available to each recipient.
Technical Support Branch Staff
Division of Stationary Source Enforcement
-------
COMPLIANCE TESTING INFORMATION No. 1 / AUGUST 1977
CONTENTS
Item Title or Description of Material
1 Transmittal Memorandum
2 List of reports issued by Quality
Assurance Branch, Environmental
Monitoring and Support Laboratory
3 A Study on the Accuracy of Type S Pitot
Tube, EPA 600/4/77-030, June 1977
4 Effective Sampling Techniques for Parti-
culate Emissions from a typical Stationary
Sources (Interim Report), EPA 600/2-77-036,
February 1977
5 Stack Sampling Technical Information (collection)
of papers prepared by Emission Measurement Branch,
Emission Standards and Engineering Division)
6 Evaluation of Stationary Source Particulate Measure-
ment Methods - Volume II. Oil-Fired Steam Generators,
February 1977
Next Month
. Revised EPA Test Methods 1.-8
. Collaborative Study of EPA Method 13A and Method 13B
. and other reports
c
-------
COMPLIANCE TESTING INFORMATION
No. 2 / SEPTEMBER 1977
Contents
Item Title or Description of Material
1 Revision to Reference Methods 1-8,
(August 18, 1977 FR) (additional copies
available on request)
2 Public Comment Summary (in response to
proposed revision to Reference Methods
1-8 [June 8, 1976 FR])
3 Guideline for Evaluating Compliance Test
Results (Isokinetic Sampling Rate Criterion)
4 How EPA validates NSPS Methodology (reprint
from July 1977 issue of ES&T)
5 Standardization of Stationary Source Method
for Vinyl Chloride, EPA 600/4-77-026, May 1977
6 Determination of Hydrogen Sulfide in Refinery
Fuel Gases, EPA 600/4-77/007, Januarv 1977
7 Standardization of Method 11 at a Petroleum
Refinery: Volume I and II, EPA 600/4-77-008a
and b
8 HP-65 Programmable Pocket Calculator applied to
Air Pollution Measurement Studies: Stationary
Sources, EPA 600/8-76-002, October 1976
9 Pollution Control Technology and Environmental
Assessment (overview of measurement methodology
studies sponsored by Process Measurement Branch,
IERL/RTP)
Next Month
. HP-25 Programmable Pocket Calculator Manual
. IERL-RTP Procedures Manual - Level 1 Environmental Assessment
-------
COMPLIANCE TESTING INFORMATION
No. 3 / OCTOBER 1977
Item CONTENTS
1 HP-25 Programmable Pocket Calculator Applied
to Air Pollution Measurement Studies: Stationary
Sources
2 List of Reports Issued By Process Measurements
Branch, Industrial Environmental Research Laboratory,
EPA/RTP
3 Process Measurements for IERL/RTP Environmental
Assessment Programs
4 Methodology for Measurement of Polychlorinated
Biphenyls in Ambient Air and Stationary Sources:
A Review, EPA 600/4-77-021, April 1977
5 Highlights of August 18, 1977 EPA Test Method
Revisions 1-8
6 Determination of Optimum Number of Traverse Points:
An Analysis of Method 1 Criteria, April 1977 (A Paper
Prepared By Entropy Environmental for DSSE Compliance
Test Workshops!"
7 Isokinetic Particulate Sampling in Non-Parallel Flow
Systems - Cyclonic Flow, October 1977 (A Draft Paper
Prepared by Entropy Environmental for DSSE Compliance
Test Workshops - Comments are invited)
8 Selecting a Stack Sampling Consultant (Reprint from
June 1977 issue of Pollution Engineering)
9 EPA National Emission Standards1for Hazardous Air
Pollutants, EPA 340/1-77-020, June 1977 (A Compilation
of Federal Regulations)
10 An Evaluation of the Current EPA Method 5 Filtration
Temperature - Control Procedure, (Unpublished Paper
Prepared by Emission Measurement Branch, Emission
Standards and Engineering Division, EPA/Durham)
Next Month
. Measurement of Polycyclic Organic Materials and Other Hazardous Organic
Compounds in Stack Gases: State of the Art
-------
COMPLIANCE TESTING INFORMATION
No. 4 / NOVEMBER 1977
ITEM CONTENTS
1 Preliminary List of Corrections to August 10, 1977
Revisions to Reference Methods 1-8
2 Comment on Spurious Acid Mist Values and Their Cause
(Reprint from August 1977 Issue of Stack Sampling News)
3 Number of Sampling Points Needed for Representative
Source Sampling, October 1976 (A paper by K. Knapp,
EPA/ESRL presented at 4th Energy & The Environment
Conference)
4 Measurement of Polycyclic Organic Materials and Other
Hazardous Organic Compounds in Stack Gases - State of
the Art: EPA No. 600/2-77-202, October 1977
5 EPA Standards of Performance for Stationary Sources,
EPA—340/1-77-015, November 1977 (A Compilation of NSPS
Regulations as of October 1, 1977)
Next Month
. Source Testing Manual: Observation and Evaluation of Performance Tests at
Asphalt Concrete Plants (Draft)
-------
COMPLIANCE TESTING INFORMATION
NO. 5 / DECEMBER 1977
Item CONTENTS
1 Determination on Including Soot Blowing
Periods in Performance Tests for New Fossil -
Fuel Fired Steam Generators
2 Listing of Stationary Source Enforcement Series
Publications Through December 1977 (DSSE)
3 Collaborative Studv of EPA Method 13A and Method
13B, EPA-600/4-77-050, December 1977 (QAB/EMSL
report)
4 Development, Observation and Evaluation of
Performance Tests at Asphalt Concrete Plants
(Draft report prepared for DSSE - Comments are
Invited}
5 Revised Technical Guide for Review and Evaluation
of Compliance Schedules for Air Pollution Sources
EPA 340/1-77-017 (DSSE report - reference source
for industrial process information)
NEXT MONTH
• Revised EPA-Reference Method 11
•Instrumental Sensing of Stationary Source Emissions
-------
COMPLIANCE TESTING INFORMATION NO. 6 / January 1978
Item CONTENTS
1 Remote Sensing of Gaseous Pollutants by Infrared
Absorption and Emission Spectroscopy (Paper by ESRL
presented at the Joint Conference, New Orleans, La.)
Nov. 6, 1977). i
2 Instrumental Sensing of Stationary Source Emissions
(Reprint from October 1977 issue of Environmental
Science and Technology.)
3 Legal Aspects of Remote Sensing and Air Enforcement
{.Reprint from February 1978 issue of APCA.)
4 Methods for Determining the Polychlorinated Biphenyl
Emissions from Incineration and Capacitor and Trans-
former Filling Plants, EPA-600/4-77-048, November 1977
CEMSL)
5 Development and Laboratory Evaluation of a Five-Stage
Cyclone System, EPA-600/7-78-008, January 1978 (IERL/
RTP)
6 Particulate Sampling Support: 1977 Annual Report
EPA-600/7-78-009, January 1978, (Report on IERL/RTP
source sampling activities.) !
7 Application of Remote Techniques 1n Stationary Source
Air Emission Monitoring, EPA-340/1-76-005, June 1976
(DSSE)
8 Continuous Emissions Monitoring Conference Dallas, Texas;
February 15-17, 1977, EPA-340/1-77-025, December 1977
(DSSE)
-NEXT MONTH
•Revised EPA Reference Method 11 (January 10, 1978 Federal Registar)
•NAPA Stack Sampling Manual
-------
COMPLIANCE TESTING INFORMATION NO. 7 FEBRUARY 1978
Item CONTENTS
1 Abstract of Study Report on Evaluation of
EPA Method 5 Probe Deposition and Filter
Media Efficiency. {Reprinted from NTIS
March 7, 1978 Envir. & Poll. Contr. abstract
summary)
2 February issue of Source Evaluation Society
Newsletter containing, 1) Corrections and
Revisions to EPA Methods 1-8, and 2) Procedure
for Calibrating and Using Dry Gas Volume Meters
as Calibration Standards, (ESED paper).
3 Survey of Techinques for Monitoring Sewage Sludge
Charged to Municipal Sludge Incinerators, EPA
340/1-77-016A, (DSSE Report).
4 NAPA Environmental Inspection and Testing Manual
for Asphalt Plants (A trade association publication).
5 Regulations and Resource File of Continuous Emission
Monitoring Information, EPA 340/1-78-002, (DSSE
report prepared for regional & state CEM workshops).
6 Control of Particulate Emissions for Wood-Fired
Boilers, EPA 34/1-77-026, (DSSE technical report
useful as background information on testing this
type of source).
7 October 1977 issue of Stack Sampling Newsletter
containing article entitled "It's The Old Condensible
Trick." (copies supplied by Technomic)
NEXT MONTH
•Municipal Incinerator Enforcement Manual
c
-------
COMPLIANCE TESTING INFORMATION
No. 8 / MARCH-OUNE 1978
ITEM CONTENTS
1 General Notice and Comment Regarding Draft
Quality Assurance Guidelines for EPA Methods
6, 7 & 8 and Revised;Soot Blowing Procedure
2 Request for Comments on ESED/OAQPS Tentative
oo = Recommendation to Allow Use of EPA Method 17
a 22 § (In-Stack Filter) on Combustion Sources With
^ a Stack Temperatures of 320°F or Less.
O CO
=* « Thermocouple Calibration Procedure Evaluation,
June 1978 Ca paper prepared by ESED).
=5
—) to
4 Process Measurements Review, First Quarter, 1978
CA newsletter issued quarterly by PMB/IERL on
development of process measurement techniques)
5 Information Memorandum - Substitution of 10 Percent
H?02 for 3 Percent HgOg in Method 6 Analysis, May 1978
(Prepared by ESED).
6 Operating Stoker-Fired Boilers at High Efficiencies
& Burning Clean Fuel Together with Coal Reduces Emissions.
(Two articles reprinted from February 1977 issue of Power
which gives background information on techniques for
adjusting and fine tuning industrial boilers for minimizing
emissions).
7-11 Resource Manuals for Implementing NSPS Continuous Emission
Monitoring (CEM) Requirements. (Issued by DSSE).
Vol. 1 - Source Selection and Location of CEM Systems
(EPA 340/1-78-005a)
Vol. 2 - Preliminary Activities for CEM System Certi-
fication (EPA 340/1-78-005b)
Vol. 3 - Procedures for Agency Evaluation of CEM Data
and Excess Emission Reports (EPA 340/1-78-005c)
Vol. 4 - Source Operating and Maintenance Procedures for
CEM Systems (EPA 340/1-78-005d)
Next Month
• Municipal Incinerator Enforcement Manual
• Updated NESHAP Regulation Compilation Manual
• Revised Soot Blowing Procedure
• Particulate Sampling Strategies for Large Power Plants (June 1976 - A Reprint)
c
-------
COMPLIANCE TESTING INFORMATION NO. 9 / July-August 1978
ITEM CONTENTS
Notice on Delay In Issuing Sool blowing
Procedure
Information Memorandum - Method 8 Test for
Peroxfde Impurities in Isopropanol, August
8, 1978 (Issued By ESED)
Municipal Incinerator Enforcement Manual,
EPA 340/1-76-013, January 1977. (reprint)
(Technical Guideline Issued by DSSE which
gives background Information on testing this
type of sourceJ
Particulate Sampling Strategies for Large Power
Plants Including Non Uniform Flow, EPA 600/2-76-
170, June 1976". (reprint) (ESRL publication)
Technical Manual: A Survey of Equipment and Methods
for Particulate Sampling in Industrial Process Streams,
EPA 600/7-78-043, March 1978. (IERL publication)
Controlled and Uncontrolled Emission Rates and Applicable
Limitations for Eighty Processes, EPA 340/1-78-004.
(reprint - the original report was issued September 1976
by CPDD) (a reference for background information on a
variety of industrial processes).
Next Month
• Updated NESHAP Regulation Compilation Manual
• Paper on Procedure for Including Soot Blowing Run in Performance Test
• EPA Performance Test Methods and Data Forms (in standard size type and fully corrected)
• Industrial Guide for Air Pollution Control (general sampling guide)
C
-------
COMPLIANCE TESTING INFORMATION
NO. 10 / September-October 1978
ITEM CONTENTS
1 Technical Paper - Source Sampling at Steam
Generators with Intermittent Soot Blowing,
October 1978. (Recommended NSPS performance
testing procedure prepared by Entropy Environs-
mental for DSSE)
2 Information Memorandum - Methods for Collecting
and Analyzing Gas Cylinder Samples, September
1979. (Issued by ESED)
3 National Emission Standards for Hazardous Air
Pollutants - A Compilation as of April 1, 1978,
EPA 340/1-78-008, April 1978. (DSSE publication)
4 EPA Performance Test Mpt.hnds - Parts I and II.
EPA 340/1-78-011, August 1978. (A reprint of current
reference methods in full size type including re-
commended data forms). (DSSE publication)
5 Progress Report on Process Measurement Methods
Research - High Temperature, Particulate Sampling,
Inorganic Analysis, Quality Assurance, Fugitive
Emissions, Organic Analysis and Biological Analysis,
June 1978. (IERL report)
6" Industrial Guide for Air Pollution Control, EPA
625/6-78-004, June 1978. (Technology Transfer;
Officelpublication). (See Chapter 5 for industrial
source testing procedures)
7 Descriptive Brochure on Using EPA Library Services
for Air Pollution Literature Searches and Documents.
(Issued by Research Triangle Park. EPA Library)
Next Period
• Roundup on Sampling Procedures for Cyclonic Flow (three most recent
technical papers on the subject)
• Final NSPS Determination for Handling Soot Blowing
• Procedures Manual for Fabric Filter Evaluation
£
-------
COMPLIANCE TESTING INFORMATION
No. 11/November-December 1978
ITEM CONTENTS
1 Listing of EPA Reference Methods for NSPS
Performance Tests. (All test methods -
tentative, proposed or promulgated - that
have been assigned a reference number as
of December 1, 1978)
2 Sampling of Tangential Flow Streams, (paper
appearing in August 1978 issue of AIHA Journal
based on study done under ESRL grant to
University of Florida)
3 A Method for Stack Sampling Cyclonic Flow, June
1978. (paper by Texas Air Control Board Staff
presented at 1978 Houston APCA meeting)
4-7 Stack Sampling Technical Information - Volumes
I - IV, October 1978. (A collection of mono-
graphs and papers prepared by ESED staff on NSPS
test methods and equipment)
8 Sensitized Fluorescence for the Detection of
Polycyclic Aromatic Hydrocarbons, EPA 600/7-
78-182, September 1978. (Simplified spot test
for rapid detection and semi-quanitative measure-
ment of PAH's) (IERL report)
9 Informational Memorandum - An Alternative Method
for Stack Gas Moisture Determination, December
28, 1978. (Issued by ESED)
10 Proposed Changes to NSPS Appendix B - Performance
Specifications I, II and III. (Recent draft of
proposed changes to continuous source emission
monitoring requirements and specifications)
(Released by ESED for information purposes)
11 Listing of NSPS Process Monitoring Requirements,
December 1, 1978. (A brief background review
and summary list prepared by EMSL) (Interested
comments solicited)
(Continued)
-------
COMPLIANCE TESTING INFORMATION
ity
NO. 12 / January-February 1979
ITEM CONTENTS
1 Listing of EPA Reference Methods for NESHAP
Compliance Tests. (All test methods, tentative,
proposed or promulgated, that have been assigned
a reference number as of January 1, 1978)
2 Amendment to EPA Reference Method 16 (TRS emissions)
published January 12, 1979 in 44 FR 2578. (Requires
use of scrubber to prevent potential interference
from high SO2 concentrations)
3 Precision Estimates for EPA Test Method 8 - SO2
and H2SO4 Emissions from Sulfuric Acid Plants.
(EMSL paper published 1n January 1979 issue of
Atmos. Envir.)
4 Announcement and Conference Program for Engineering
Foundations Ninth Stack Sampling and Stationary
Source Emission Evaluation Conference, April 1-6,
1979 at Asilomar (Calif.). (The program emphasis
is on continuous monitoring and organic measurement
methods.)
5 Measuring Inorganic and Alkyl Lead Emissions from
Stationary Sources, November 1978. (Paper by EMSL)
6 Procedure for Determining Inorganic Lead Emissions
from Stationary Sources, November 1978. (Paper by
EMSL)
7 Procedure for Determining Alkyl Lead Emissions from
Alkyl Lead Manufacturing Plants, November 1978.
(Prepared by EMSL)
8 A Data Reduction System for Cascade Impactors, EPA
600/7-78-132a, July 1978. (IERL report)
9 The Use of Tedlar Bags to Contain Gaseous Benzene
Samples at Source - Level Concentrations, EPA
600/4-78-057, September 1978. (EMSL report)
10 Colaboratlve Testing of EPA Method 106 (Vinyl Chloride),
EPA-600/4-78-058, October 1978. (EMSL report)
11 Measurement of Volatile Organic Compounds, EPA 450/2-
78-041, October 1978. (ESED Guideline Series)
-------
COMPLIANCE TESTING INFORMATION
'NO. 12 / January-February 1979
Next Period
• Update (February 1, 1979) of NSPS regulations manual
• Primary sulfate emissions from combustion sources (measurement methods)
• Ultraviolet video technique for visualization and measurement of
stack plumes (particulate and SO )
2
-------
H-
LISTING OF ifte
EPA REFERENCE METHODS FOR ' <"
NSPS PERFORMANCE TESTS
APPENDIX A - REFERENCE METHODS
Method 1 - Sample and velocity traverses for stationary sources
Method 2 - Determination of stack gas velocity a^d volumetric flow
rate (type S pi tot tube)
Method 3 - Gas analysis for carbon dioxide, excess air, and dry
molecular weight
Method 4 - Determination of moisture in stack gases
Method 5 - Determination of particulate emissions from stationary sources
Method 6 - Determination of sulfur dioxide emissions from stationary
sources
Method.7 - Determination of nitrogen oxide emissions from stationary
sources
Method 8 - Determination of sulfuric acid mist and sulfur dioxide
emissions from stationary sources
Method 9 - Visual determination of the opacity of emissions from
stationary sources
Method 10 - Determination of carbon monoxide emissions from stationary
sources
Method 11 - Determination of hydrogen sulfide emissions from stationary
sources
Method 12 - Determination of inorganic lead emissions from stationary
sources
Method 13A - Determination of total fluoride emissions from stationary
sources - SPADNS Zirconium Lake method
Method 13B - Determination of total fluoride emissions from stationary
sources - Specific Ion Electrode method
Method 14 - Determination of fluoride emissions from pot room roof monitors
of primary aluminum plants
Method 15 - Determination of hydrogen sulfide, carbonyl sulfide, and
carbon disulfide emissions from stationary sources
Method 16 - Semicontinuous determination of sulfur emissions from
stationary sources
Method 17 - Determination of particulate emissions from stationary
sources (In-Stack Filtration Method).
-------
Method 18 - Determination of total gaseous nonmethane organic compound
emissions from stationary sources
Method 19 - Determination of sulfur dioxide removal efficiency and
particulate, sulfur dioxide and nitrogen oxide emission
rates from utility steam generators
Method 20 - Determination of nitrogen oxides, sulfur dioxide, and
oxygen emissions from stationary gas turbines
* Method 21- Determination of nitrogen oxide emissions from stationary
reciprocating internal combustion engines
* Method 22 - Visual Determination of Fugitive Emissions from Material
Processing Sources
~Have not been proposed, as of 10/25/78.
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY ^ 6
Office of Air Quality Planning and Standards
Research Triangle Park, North Carolina 27711
subject: Corrections to Reference Methods 1-8 date: DEC 1 S1Q77
from: Roger T. Shigehara, Chief, Test Support Section RECfivrn
Emission Measurement Branch, ESED (MD 19)
T0: See Below *1 '978
s A A DJVSION
Please find enclosed a list of corrections to the "Revision
to Reference Methods 1-8," published 1n the August 18, 1977
Federal Register. Note that this 1s an abreviated 11st, containing
only those changes that significantly affect the procedural and/or
analytical aspects of the methods, and therefore may have an import
tant bearing on the test results. A complete list of corrections to
Methods 1-8 will be published and distributed at a later date.
€PA ferm 1320-6 (R>«. 4-72)
&
-------
ABBREVIATED LIST OF CORRECTIONS TO
REFERENCE METHODS 1-8
1. In Section 6.2 of Method 3, page 41771, Equation 3-1 is
corrected to read as follows:
SEA
%02 - 0.5% CO
0.264 %HZ - (%02 - 0.5% CO)
100
2. In Section 3.1.8 of Method 4, page 41774, delete all of first
paragraph except the first sentence and insert the following:
Leak check the sampling train as follows: Temporarily insert a
vacuum gauge at or near the probe inlet; then, plug the probe inlet and
pull a vacuum of at least 250 mm Hg (10 in. Hg). Note the time rate of
change of the dry gas meter dial; alternatively, a rotameter (0-40 cc/min)
may be temporarily attached to the dry gas meter outlet to determine the
leakage rate. A leak rate not in excess of 2 percent of the average
sampling rate is acceptable. Note: carefully release the prots inlet
plug before turning off the pump,
3. In Section 2.1.12 of Method 6, page 41783, the phrase "and
Rotameter." is inserted after the phrase "Vacuum Gauge" and the phrase
"and 0-40 cc/min rotameter," is Inserted between the words "gauge" and "to."
4. In Section 4.1.2 of Method 6, page 41784, delete the last sentence
of the last paragraph. Also delete the second paragraph and Insert the
following paragraphs Instead:
Temporarily attach a suitable (e.g., 0-40 cc/m1n) 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
-------
2
and note the flow rate as indicated by 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 leak-check shall precede the leak check of the
sampling train described immediately above; 1f 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-impinger
assembly. Place a vacuum gauge at the Inlet to either the drying tube or
the pump, pull a vacuum of 250 mm (10 1n.) 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 seconds.
5. In Section 4.1.3 of Method 6, page 41784, 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 sample volume for the leakage."
-------
£*# A
July 197B
Nov,1978 (rev)
COMPANY:
VISIBLE EMISSION EVALUATION FORM
REGION VIII - DENVER
Iff
ADDRESS OF SOURCE:
TYPK OK FACILITY
STACK NAME:
ORSERVER:
Sky Condition (% clouds rt.
-------
Page
H*
FORM A
OBSERVATION RECORD
i IMP ANY:
UX jVl'ION:
IIATI::
OBSERVER:
n:sT mumhi:r.-
TACK I.D. NO.
MIN
SECONDS
0
15
30
45
I)
1
J
3
4
5
0
7
3
0
LO
II
i:
13
II
...15..
Ji<
i /
13
19
:u
n
23
>4
25'
\li
¦'> 1
.
1
___L
REMARKS
TYPI: OP PACII.ITY:
COWTROI. DEVICE:
Olc.crvod whilo on < < >m 11; i r i y iiropt tIv: y>
TIME: HEIUN KND
MIN
SECONDS
0
15
30
45
30
31
32
33
34
3S
36
37
38
39
40
41
42
4.5
44
|
45
¦Id
1/
48
49
50
51
*
52
1
|
53
1
54
55
1
5f>
1
r "•
1
_ !,M
V.I
REMARKS
-------
?ORM A PAGE 3 of 3
SKETCH: Indicate within the figure provided below: 1) Point of Evasion (Draw a small circle indica-
ting the emission point being evaluated, including its distance and direction fran the observer. The
position of the observer is located in the center of the circle, at the intersection of the quadrant
lines. Orient the sketch in accordance with the North arrow shown. Include specific features such
as buildings, streets, .etc., which will positively identify the location of the emission source being
evaluated. If more than this single emission source are .located in the inmediate area, identify the
evaluated source, and indicate its distance from the adjacent emission.sources.) 2) Direction of
Plume Travel (Draw an arrow, originating at the emission point being evaluated, pointing in the
airection of plume travel.) 3) Sun Position (Use an asterisk to show the sun's position with respect
to its height above the horizon and the observer's location. A sun, low in the sky, should be drawn
sear the dashed horizon circle, whereas a midsumner noon sun, mgh in the sky, should be shown
directly above the observer, etc. Insure the sun is properly oriented within the 140° sector at the
observer's back.)
X
/
\
\
\
f
/
i
)
I
/
/
I S
Wet or Dry Plume (circle one) If wet, is it attached or detached? (circle one)
If detached, estimate breakpoint distance fran stack- ft.
Persons present during evaluation:
Name: Name:
Title: Title:
Copy of mi," Visible Emissions Observation (VEO) Given: Date Time _________
k^'Name: Nans:
Title: Title:
Signature: (Company person receiving data):
Date:".
Title:
-------
USEPA REGION VIII DENVER
Visible Emission Evaluation
Field Tnvrat.ifintion
Work Shoot.
I'l.irit. N.'irn^: Date:
Mime of Company:
Address:
Type of Facility:
1. Applicable Visible Emission Regulation:
FO!^y»>-
¦July 1078
Nov,!978 (rev)
2. Prior Notification to Company:
a. Notified by: d. Time of Notification
b. Name of Official Notified: e. Date of Notification.
c. Title:
3. Plant Process:
a. Based on company information, did any type of plant process upset occur duririp,
the visible emission evaluation? If so, explain. If no upset occurred, did
the company Rive any reason for the violation?
b. What was the approximate plant production rate at the time of inspection? Is
this rate above or below the normal production rate?
c.. In general, what products utilized in the production process are responsible for
the visible emissions? Are these the same products that wore utilized during
your visible emission evaluation?
(I. Whc'ti was the observed :;ource constructed or last modified?
e. Were Uinm any opacity proMomn identified from fugitive rsources (road, transfer'
points, etc)? If so, where and to what extent?' Was the source operating a re-
cording transmissometer on the stack that was evaluated?
-------
C. Whnt. w.'i:'. t.hc r^riorvi'l eorrvl.it ion of t.ho instrument. (t.rNin:irtiL:'.:'.ONH t<-r) cl;it.;i .1::
compared to the visible emissions observations taken concurrently? AtInch
a copy of the concurrent transmissometer data if available.
I'ollnUori Control Kfiuiprrient:
a. What type of pollution control device(s) are utilized on the stack evaluated?
If low-sulfur coal is used, what is the value of the most-recent analysis
(BTU, Ash, and Sulfur %, on Dry Basis)?
b. Itiaeri on company reports or your porsonnl inspection, were the control device::;
mentioned above operating properly? If not, explain.
c. If the facility was equipped with a flue gas monitoring system (SO2, N0X, etc.)
was this system operable? If so, what compliance or operation and maintenance
condition of the control system did the data indicate? Attach a copy of this
data if available.
d. If an EPA Method 5 stack test was done during this Method 9 evaluation,
what was the run number and time of this Method 5 test?
Miscellaneous Remarks: (any other unusual circumstances mentioned by company
personnel or observed by field inspector; comments made by state or local pollution
control officials; your comments, if any, concerning appropriateness of initiating
nn enforcement action).
Source of information for above information (items 1-5):
a. Name: Telephone Number:
b. Title: Mailing Address:
-------
THE NUMBER OF SAMPLING POINTS NEEDED FOR REPRESENTATIVE SOURCE SAMPLING
Introduction - One of the major problems in stationary source emissions measure-
ments Is getting a representative sample to the measuring device. The number
and location of the sampling points to be used depends greatly on the flow of
the gas stream being sampled. Not only are good representative sampling points
needed for the pollution measurements, but they are also needed for accurate
volumetric flow rates for total emission determinations. This paper presents
some of the results obtained from work done in the development of source sam-
pling strategies for sampling In large ducts.
Test Program - EPA Method 1 gives the EPA procedure for selecting the location
of sampling sites for stationary source emission measurements. It recommends
the selection of a sampling site at least eight stack or duct diameters down-
stream and two diameters upstream from any flow disturbance. Twelve sampling
points are required for such a location. When such a sampling site 1s not
possible* sampling sites closer to disturbances may be selected, but more sam-
pling points are required. At the minimum recommended downstream distance of
two diameters, 48 points are required. In large modern installations, few have
reasonable sampling sites that are at least eight diameters downstream of a
flow disturbance. In those Installations which have complicated flow fields
influenced by one or more disturbances but designed with turning vanes, etc. to
minimize draft losses, the flow may be relatively uniform, thus requiring less
than the indicated number of sampling points for representative sampling. To
define this and similar flow situations and to establish good sampling strate-
gies for these types of installations, EPA contracted Flutdyne Engineering
Corporation to make a study of the gas flow and particulate distribution in the
ducts and stacks of large power plants. This study had as its prime objectives:
(1) Determine the effects of duct and stack geometries on velocity profiles
and particulate distributions.
(2) Establish sampling strategy guidelines which describe the expected flow
profiles and the magnitude of errors caused by the proximity to mechanical
disturbances.
(3) Identify geometric flow configurations in large Dower Dlants which
generate cyclonic flow.
(4) Study the effect of emission levels at part-load operation and scale
these measurements to the full-load case.
A detailed report on the findings of this study has been prepared by Hanson
"Superior numbers refer to similarly-numbered references at the end of this paper?
K. T. Knapp
Environmental Protection Agency
Research Triangle Park, N, C. 27711
et al.
563
-------
%>/(>
The study was conducted in several phases. After a literature review, a survey
of large power plants was made. Several of these plants were chosen as test
sites, and many tests by EPA Methods 2 and 5 were conducted for both gas velo-
city and particulate loading measurements at different duct and stack geometries
near mechanical disturbances. These tests included many runs with as many as 84
sampling points. In addition to these tests, a 1/10 scale test model of the
precipitator and stack breeching of one of the power plants was constructed.
The test model had removable turning vanes and many measurements were made with
and without the turning vanes.
Results and Discussion - From the test data obtained at the power plants and
from the model, simulated profiles for both velocity and particulate distribu-
tion were constructed. Figures 1 and 2 Illustrate examples of velocity distri-
butions found near flow disturbances. In the Hanson report*1* 26 illustrations
for rectangular ducts and 6 for round ducts are given. Both velocity distribu-
tions and particulate concentration distributions are presented. Table I 1s
part of an evaluation of these data giving the percent error in the measurement
as a function of the number of traverse points for a given matrix. Table II 1s
the average error from 21 tests of the total volumetric flow rate for certain
matrices. These data are also shown 1n Figure 3. In an independent study,
Brooks et al(2) obtained the same kind of results. The results of both studies
showed a definite leveling off of the percent error after 16 sampling points
with a symmetrical matrix.
Conclusions - The conclusion that may be drawn from the data presented here 1s
that no appreciable Improvement 1n gas flow measurement can be obtained with
symmetrical matrices of more than 16 traverse points 1n rectangular ducts of
large power plants. In addition, good results can probably be obtained from a
matrix with only 12 traverse points provided that at least 3 points are in each
direction. Results for similar conclusions are given 1n the report by Hanson*1'
for gas flow in round ducts and for particulate concentration distributions 1n
botl^types of ducts. These conclusions.are supported by the work of Brooks et
Acknowledgments - The author wishes to acknowledge the fine work of Fluidyne,
especially that of Dr. H. A. Hanson. The author also wishes to thank Ed Brooks
for his helpful comments.
References
1. Hanson, H. A., R. J. Davlni, J. K. Morgan and A. A. Iversen, Particulate
Sampling Strategies for Large Power Plants Including Nonuniform Flow,
EPA-600/2-76-170, June 1976".
2. Brooks, E. F. and R. L. Williams, Flow and Gas Sampling Manual,
EPA-600/2-76-203, July 1976.
564
P
-------
Figure 1. Velocity Distribution Simulating Profiles for Measurements Near Two
Disturbances at a Large Power Plant
r
2.'
we
tife)
Gas Velocity ["" '
C. VXocity [j^Sp-]
565
F
-------
H1
Figure 2. Velocity Distribution Simulating Profiles for Measurements Near Two
Disturbances at a Large Power Plant 1
Gas Velocity [jEt/secj
L «/«ecJ
>-Y
f
X
_flo_
jL(84,»)
\
ft/sec
566
f
-------
TABLE I
Part of the Evaluation of Various Equal Area Sampling Strategies
for a Velocity Distribution Measured at a Large Power Plant( '
Number of traverse points along x axis
^—Number of traverse points along y axis
n
4X3
% Error in Measured
Total Number of Total Volumetric
Matrix Traverse Points Flow Rate
1x1 1 -78.90
1x2 2 -21.42
2x1 2 -55.12
1x3 3 -26.28
3x1 3 -42.29
1x4 4 -27.19
2x2 4 - 8.48
4x1 4 -40.33
1x5 5 -27.39
5x1 5 -39.99
1x6 6 -27.44
2x3 6 - 5.71
3x2 6 - .95
6x1 6 -39.97
1x7 7 -27.44
1x8 8 -27.43
2x4 8 - 5.48
4x2 8 .40
3x3 9 - .95
2x5 10 - 5.51
5x2 10 .74
2x6 12 - 5.56
3x4 12 - 1.06
4x3 12 - .05
567
-------
TABLE II
Average Percent Error of Total Volumetric Flow Rate
from 21 Tests as a Function of Traverse Points
Traverse Points
Matrix Number of Average Percent Error
X Y Points 21 Tests
1
1
1
14.90
2
2
4
4.01
3
3
9
0.92
2
5
10
2.39
2
6
12
2.36
3
4
12
0.62
4
3
12
0.72
4
4
16
0.47
5
5
25
0.33
6
6
36
0.25
I Mi
12.
i a,
%
Error
MJ
Figure 3 Dependency of Error in Total Volunetric
Flow Rate on Number of Traverse Points
. Equal no. of points X and Y
+ Other
H, IB. IZ IB. 2B. 2H. 26.
Number of Traverse Points
568
-------
It
SAMPLING LOCATION FOR GASEOUS POLLUTANT MONITORING IN
COAL-FIRED POWER PLANTS
R. T. Shigehara*
Introduction
"Performance Specification 2 - Performance Specifications and
Specification Test Procedures for Monitors of S0? and NO from
1 x
Stationary Sources" requires that continuous monitoring systems
for S02 and NOx emitted from coal-fired power plants be "...In-
stalled at a sampling location where measurements can be made
which are directly representative or which can be corrected
so as to be representative of the total emissions from the
affected facility." The specification provides two alternatives
for locating the monitoring points:
1. At sampling locations 8 or more equivalent stack diameters
downstream of any air 1n-leakage or where stratification of the
pollutant gas 1s demonstrated not to exist, any point of average
concentration no closer than 1.0 meter to the stack or duct
wall may be monitored (with extractive systems), or (with 1n-
sltu systems) any path of average concentration may be monitored.
"Stratification," according to the specification, 1s "a
condition Identified by a difference 1n excess of 10 percent
between the average concentration in the duct or stack and the
concentration at any point more than 1.0 meter from the duct or
stack wall."
~Emission Measurement Branch, Emission Standards and Engineering
Division, Office of Air Quality Planning and Standards, Environ-
mental Protection Agency, Research Triangle Park, N.C., July 1978.
-------
2. At sampling locations less than 8 equivalent diameters
or where stratification of the pollutant gas 1s shown to exist,
a. a single point no closer than 1.0 meter to the
stack or duct wall or a path may be used provided that a diluent
monitor (COg or Og) 1s used with the pollutant monitor or
b. a multipoint sampling probe or a path that yields
an average pollutant concentration may be used.
Data from seven power boilers (six coal-fired and one coal/oil
mixed fuel-fired units ranging from 125 to 800 Mw) were examined
1n light of the above alternatives and Subpart D*which requires
the use of a diluent monitor to convert the pollutant concentration
into units of the emission standards. The data were obtained
2
by the Exxon Research and Engineering Company, under EPA sponsor-
ship. This paper presents the conclusions of the data evaluation.
Sampling Locations
A summary of the sampling locations for the seven boilers (1n
terms of the distances from the nearest upstream and downstream
disturbances) Is given 1n Table 1. Note that, in all Instances,
the sampling locations were downstream of the rotary air pre-
heater. The Navajo unit stack location was more than 8 equivalent
2
diameters downstream from the ID fan, a source of air 1n-leakage,
and was the only location that met the requirement of alternative
(1) above (see Introduction). The duct location of the Navajo
plant was estimated to be about 6 to 7 equivalent diameters
from the preheater, another source of air 1n-leakage.
-------
TABLE 1. SUMMARY
Unit
Sampling location
Widows Creek
Unit 5
Widows Creek
Unit 7
E.C. Gaston
Unit 5
Downstream of rotary air pre-
heater and fly ash collection,
just upstream of l.D. fan
Downstream of rotary air pre-
heater, just upstream of
electrostatic precipitator
Just downstream of the rotary
air preheater
Barry Unit 4
Downstream of air preheater and
electrostatic precipitator,
just upstream of stack
Barry Unit 5
Morgantown
Unit la
Navajo
Unit 1
Downstream of rotary air pre-
heater, just upstream of
electrostatic precipitator
Downstream of rotary air pre-
heater, just upstream of
electrostatic precipitator
Downstream of rotary air pre-
heater, just upstream of l.D.
fan
350 ft up stack
Navajo
Unit 1
(in stack)
acoal/oil mixed fuel fired
SAMPLING LOCATIONS
Equivalent Distance from nearest
diameter, disturbance, ft
ft downstream upstream
11.6 *1 1/2 *5 1/2
15.0 1.35 *4
13.5 Sampling ports located
at the start of an
expansion section
15.3 Sampling ports located
at the end of a com-
pression section
immediately before a
90° bend
14.7 Sampling ports located
at the start of an ex-
pansion section
13.4 Sampling ports located
at the start of an
expansion section
19.5 *70 *7
25.0
*350
*350
-------
4
Location of Data Points
For each boiler, the pollutant and diluent concentrations
were measured at the points shown 1n the figures in the Appendix.
For each unit, a "run" consisted of measuring the pollutant
and diluent concentrations at each of the traverse points.
Data Reduction
For each run, the SOg and N0X data were reduced on the
basis of both 02 and C02 diluent measurements as follows:
1. All pollutant and diluent point values were expressed
1n terms of the standard (I.e., mass per unit calorific value).
Then the "overall average" emission rate was calculated.
2. The emission rate at each traverse point, located at
least 1.0 meter from the stack wall, was compared to the overall
average emission rate. The percentage deviation of each of these
points from the overall average was calculated.
3. The average pollutant and diluent concentrations along
various sampling paths were calculated; then, the average con-
centrations were converted to emission rates and the results
were compared to the overall average emission rate. For rectangular
stacks, the path averages were, for simplicity, calculated on
the basis of the "rows" and "columns" used in the data gathering
process; in most cases, at least one sample path passed through
the centroid. (The centrold is defined as a concentric area
that is geometrically similar to the stack cross section and
no greater than 1 percent of the total cross-sectional area).
-------
5
The percentage deviation of each path average emission rate from
the overall average emission rate was calculated.
[The reduced data for Items 1, 2, and 3 are presented in
the Appendix; the numerical values shown are the plus or minus
percentage deviations of the point or path average emission rates
from the overall average. The percentage deviations are "paired,"
each pair of numbers corresponding to a particular sampling
run. The first number of each ea1r of deviations was deter-
mined on the basis of Og measurements; the second number (in
parentheses) was determined by use of COg measurements.]
4. The percentage deviations for all runs in a given
duct or stack were then averaged. They are summarized in Table
2. Table 2 lists only the maximum negative percentage deviations
from the overall average emission rate values, because they
Indicate the amount by which a tester could have underestimated
the overall emission rate by using a particular measurement
strategy. In those cases where there were no measurements in
the centroid or where no sample path passed through the centroid,
the data were interpolated to obtain the centroid and centroid
path values.
Discussion and Data Evaluation
Theoretically, at the locations selected for monitoring 1n
power plants, S02 and N0X should be well mixed and stratification,
if any, should only come from air infiltration. This would be
true more so for SO^ than for N0X> However, the data obtained in
-------
TABLE 2. SUMMARY OF PERCENTAGE DEVIATIONS FROM AVERAGE AT SELECTED SAMPLING POINTS
so2
NOx
Sampling
1-Meter"
Centroid"
Other"
1-Meter®
Centroid"
Other"
point
Centroid
Poi nt
Path
Path
Centroid
Poi nt
Path
Path
WC-5A
-K-l)
-4(-l)
-l(-l)
-2(-4)
-K-D
-2(+2)
-K-l)
-2(-2)
5B
-2(-4)
-6(-7)
-4(-3)
-2(-2)
o(-l)
+K-1)
-K-l)
-K-4)
7A
-6(-7)
-K-l)b
-12(-14)
-2(-3)b
-6(-7)
-K-l )b
-4(-6)
7B
+2(+l)b
-7(-10)
0(-2)b
-2(-4)
-l(-l)b
-3(-5)
-K-2)b
-4(-6)
G-5A
+7(+3)b
•
-6(-4)
0(-2)b
-10(-6)
+2(-2)b
-2(-4)
0(-2)b
-7(-8)
5B
+7(+2)
-4(-2)
o(-i)b
-5(-6)
0(-2)b
-2(-4)
+K-i)b
-2(-2)
B-4A
0(-2)b
-l(-4)
0(-l)b
-2(-2)
-2(-3)b
-10(-12)
-2(-2)b
-4(-4)
4B
0(-l)
-2(-2)
0(-2)b
-2(-2)
o(-Db
-6(-8)
0(-l)
—2(-4)
5A
+4(+2)
-2(-2)
+K-1)
-2(-2)
+4(+2)
-4(-4)
+K+1)
-2(-3)
5B
+l(-2)
-10(-4)
+K-U
-10(-7)
+1(-1)
-8(-6)
+K-1)
-6(-2)
M-1A
+K-l)b
-
-K-3)
-3(-4)
-3(-4)b
-
-2(+l)
-6(-4)
IB
0(+l)b
-
-K+i)
-3(-2)
-1(0) b
-
-K+2)
-8(-8)
N-1A
-3(-3)
-ll(-ll)
0(—2)
-7(—8)
-K-l)
-4(-4)
o(-l)
-4(-4)
IB
-3(-3)
-4(-3)
-3(-2)
-11(-10)
-4(-3)
-4(-4)
-1(0)
-3(-4)
1C
+3(0)
-7(-7)
+K+1)
-7(-8)
+1(-1)
-5(-6)
o(-l)
-2(-3)
ID
+7(+9)
0(+3)
-2(-l)
-22(-23)
0(0)
-6(-5)
-K-2)
-K-2)
S
-2(-2)
-4(-7)
-K-2)
-K-2)
0(-l)b
-4(-7)
0(0)
0(0)
a Maximum negative values
b Interpolated values
-------
7
the cited test program did not reflect this theory. A likely explana-
tion is that the data included temporal variations and measurement
errors.
In the test program, sampling was conducted from two ducts.
The analyses at each traverse point were performed by the same set of
instruments, and the samples from the two ducts were alternately
measured by means of two probes and a switching valve. The time at
each point was about 1 to 2 minutes. A complete traverse was con-
ducted twice and the entire test usually lasted 3 to 5 hours. The
duplicate measurements at each traverse point for most plants differed,
which strongly indicates temporal variations or, possibly, instrument
drift. Thus, the data evaluation below would be based on data that
include both temporal and instrument drift variations. However, the
conclusions drawn from the data would be conservative ones and should
serve as adequate guidelines for the selecting of representative
measurement locations.
The results of the data reduction demonstrate the following:
1. By measurement of emission rates at the centroid of the stack
or along a path that passes through the centroid, there is only a .
5-percent chance that the tester would have underestimated the average
emission rate by as much as 4 percent.
2. By selective monitoring of the pollutant and diluent concen-
trations at a single point (located 1 meter or more from the stack
wall), which yields the lowest emission rate, there is a 95-percent
chance that the tester could have underestimated the average emission
6
-------
8
rate by as much as 11 percent.
3. By selective monitoring of the pollutant and diluent concen-
trations along a path (other than one passing through the centroid)
that yields the lowest emission rate, there is a 95-percent chance that
the tester could have underestimated the average emission rate by as
much as 17 percent.
4. The Navajo data show that stratification can exist at sampling
locations that are 8 or more diameters downstream from the nearest point
of air in-leakage. Stratification also existed in the Navajo duct loca-
tion that was 6 to 7 equivalent diameters from the air preheater.
Conclusion
In light of the above, the following conclusions are drawn:
1. The "8 equivalent diameter" criterion of alternative 1 (see
Introduction) 1s not necessarily a reliable indicator of the presence
or absence of stratification. Therefore, this criterion is not viable
for coal-fired power plants.
2. The tester will not necessarily be prevented from significantly
underestimating the average emission rate by the use of both pollutant
and diluent monitors to monitor the emission rate (a) at a single point
(other than the centroid), located at least 1 meter from the stack wall,
or (b) along a path other than one passing through the centroid. There-
fore, alternative 2a (see Introduction) is not viable for coal-fired
power plants.
3. Even when stratification is present, monitoring the emission
-------
9
rate at the centroid of a coal-fired power plant duct or stack (or
along a path passing through the centroid) will yield emission rate
numbers that are either correct, biased high, or biased very slightly
(4 percent) low.
References
1. Federal Register, Vol. 40, No. 194. Monday, October 6,
1975. p.46250-46271.
2. Crawford, A. R., M. W. Gregory, E. H. Manny, and W. Bartok.
Magnitude of S02, NO, C02, and 02 Stratification in Power PLant Ducts.
EPA-600/2-75-053. September 1975.
-------
10
APPENDIX
Legend
1. The paired numerical values shown in each figure are
percentage deviations from the overall emission rate for a
particular measurement strategy. Percentage deviation values are
given for (a) all traverse points located 1.0 meter or more from
the stack walls (these points are within the boundaries of the
dotted lines 1n each figure) and (b) various measurement paths,
some of which pass through the centroid and some of which do
not (the percentage deviation values for these paths are out-
side the boundaries of the stack cross section in each figure).
2. The first value of'each numerical pair is based on Og
measurements.
3. The second value (in parentheses) 1s based on CO2
measurements.
4. Each pair of percentage deviation values corresponds
to a particular run.
5. For further explanation and example, see the figure
on page 11 for Widows Creek Units 5A and 5B.
-------
WIDOWS CREEK UNITS 5A AND 5B
1: +1(+2)
2: +6 (+6)
' Duct A
+K+2)
-3(-3)
¦2(-4)
¦2(-4)
Column Averages
r
"I
i .+2<+1!
1 -3(-2) ,
I ,
| -3(0) 1
i I'5!*1' .j
n
^ 1 meter
Run 1 Run 2
+4(+4) +1(0)
+2(+2) 0(-l)
-l(-2) +3 (+1)
-3(-3) -2(0)
-l(-i) -l(-i)
+K-D
+10(+10)
+ +1
:
Duct B
+3(+5) +1(-1)
+1 (-4) 0(+2)
2(0) +2(+2)
-1-1 +1-1)
0+1) -2(-2)
-------
WIDOWS CREEK UNITS 5A AND SB
NOx
+K+2)
-2(+l)
-2(-2)
+1(0)
+1(0)
+1(0)
•
•
•
+2(+2)
+1(0)
•
1
—
•
1
i
-K-2)
-3(-3)
•
| . -4-5
1 +3(+4)
1
1
1 •
1
+1(0)
+1(0)
•
•
1 "3<
L_ J-]!
•
1
t
_ J
«
-l(-l)
+1(0)
+K-3)
-l(-l)
+3(+2)
-HO)
-1(0)
0(-1)
-2(-2)
0(0)
•
•
•
+l(+2)
+1(0)
•
1
•
"1
I
+H-3)
+2(-4)
•
•
•
; •»
! -si
%
%
1
1 .
1
1
•
_j
•
0(+2)
-2(-2)
+2(+2)
-K-l)
+2(0)
-2(-2)
-------
UIDOUS CREEK UNITS 7A AND 7B
so2
-21 (-20) -K-5) -2(-l) -5(-7) +3(0) -6(-4) +l(+2) +15(+15)
-2 (-9) —6(-10) -2(-5) +3(+4) +7(+10) +l(+6) 0(+4) -1(+1)
+3(+l) +3(+4)
0(+l) +2(+2)
-3(-3) -l(-l)
+K-1) +1 (+1)
-12(-12) -3(-4)
0(-2) -l(-4)
=3(=S) =?(-n
»4(-9) •*-6(-9)
=9(-W --7H)"
• 0(+4) H-5(+8)
.-2(-l) .r5(-l) ,+6(-3) .-K-5)
-6(-ll) 0(-3) +3(+l) +7(+8)
I 1
-et-7
-5(-2) -+3(+0)
-7(-7) ,+2(+£)
_+li+8) j
+3(+2) +5(+4) +3(+l) -3(-5) +l(-6) +9(-12) +6(-4) +8(+7)
+4(0) —3(—6) +1(-1) +4(+3) +8(+9) +l(+3) -7(-2) -8(-5)
+3(+l) +3(+2)
0(-l) +2(+3)
0(-l) +1(0)
0(—5) 0(0)
o(-l) -3(-3)
0(-2) -3(-2)
r
i _
±6(=fc6) _+4(+2} =3(=5) —0(-=3) .
.+3(-2) ,+l(-l) #+4(+3) #+9(+9)
,+3(+2) .+4(+l) -5(-5) +2 .
3(-7) +2(-l) +3(0) +7(+9)
-a(-i2)
0(+2)
•10(-17
-4(-2) '
-7i^9i) #
-6H4) .
331 •
OS
-------
WIDOWS CREEK UNITS 7A AND 7R
N0X
-4(-4) -5(-7) —4(-4) +1(-1) +1(0) +2(+3) 0(-l) +10(+10)
0(-7) +2(-2) -4(-6) -1(0) -6(-4) +3(+8) +4(+8) 0(+3)
• •
•
0(-l)
-1(+1)
- ' -7(-9) —8(-9)
i i-13(+10)t +2(-l)
|
-5(-7) *-2(-2)
-3(+l) -5(-2)
»
+Hoy
. +3(+6)
+5ft3)
+9(fl3).
+5(+6)
0(-l)
-1(0)
+2(+3)
1
1 • -2(-3) •-3(+l)
L . +9(^+3) -1 (-4)
^l+ii "J}-?}
• +4(+5)
+51+12)
ail);
+K-1)
+3(0)
• •
#
-4(-4)
-3(-4)
• *
0
-2(-3)
-l(-3)
—9(-8) —4(—3) -4(-4) -1(0) +l(-3) +6(+5)
+l(-3) +3(0) -2(-4) -l(-2) -3(-2) +3(+5)
0(+5) +7(+8)
-l(+4) 0(+3)
-6(-4) -4(-3) -3(-3)
+9(+5) . +2(-l) « 0(-l)
~4(-3) . -4(-5) f 0(+2)
+5(+l) -2(-5) +2(-l)
+1(-1)- +8(+7) +8f+8)
-3(-3) . +4(+6) . +2(|4)
+1 . +5(-l) „+3(}2)
-3(-2) +5(+7) +2(f6)
-2(-2)
-2(-3)
-1(0)
-1(0)
o(-D
+K-1)
+l(-2)
+2 (+2)
+2(+2)
+2(+2)
0(+l)
-1(0)
-------
(L+)Z+
(Z~)L+
(e-)i-
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BARRY UNITS 5A AND 5B
+2(0) —1(-4) -2(-2) 0(-3) +1(+1) 0(+2) 0(+3) -2(+3)
-5(+l) 0(+l) +3(+l) +3(+l) +!(-!) 0(-l) 0(-2) -2(-2)
-3(-3) -2{-2)
0(0) 0(+l)
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0(0) -2(-l)
•
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L_-9(-A)
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+l(+2) _+2(+]i
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f
0(+2)
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1 1
1
+9(+5) -1(-4) -2(-7) 0(-3) +5(+4) +7(-3) -3(+5) -14(0)
+2(+5) +2(+l) 0(-7) +2(-l) +2(0) 0(-l) -2(-l) -5(-l)
-2(-2) +1(+1)
+1(0) +1(+1)
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140RGANT0UN UNITS 1A AND IB
0(-l) -5(-7) -4(-5) -1(-2) -2(-4) +2(-5) -l(-l) +2(0) +2(+3) +2(+5) +3(+5) +4(+9)
+1(-1) 0(0) -2(-2) +1(-1) +4(+2) +1(-1) +2(-3) -3(-2) -l(-l) -1(0) +2(+4) -3(+2)
f • • f
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0(0)
~,—. _ •_ --
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0(-l) -1(+2) 0(+5)
0(-2) 0(0) +l(-3)
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MORGANTOWN UNITS 1A AND IB
i!+JI ~3!+!l "1S+11 ~3!"3) ~6(_2) +4<*7) +6(+i3) -k+7) +6(+in +4(+i3)
-3(0) -3(+l) -5(-l) -4(-l) +2(+4) 0(+3) -5(-6) +5(+10) +2(+8) +l(+6) +7(+14) +2(+12)
+5(+9) +l(+6)
0(+2) +3(+6)
0(+2) -4(0)
-4(+3) -1(+5)
"5HI "7("8} "7f"8! "7!"7) °H} _2{°) _4(+1) +5(+1) +5(+5) +8(+9) +4(+6> +13(+8)
¦4(-6) -8(-8) —5(—4) -4(-5) -l(-4) +l(-4) +2(+2) 0(+l) +8(+7) +11(+11)+8(+10) -4(0)
+3(+2)
0.(0)
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-1(0)
ro
o
r
L
~ 1
_ _ J
-1(-2)
0(0)
+K+1)
0(0)
-------
+10(+10) +6(+5)
+4 (+3) +7(+6)
+2(-l) +8(+7)
+l(+2) -4(-4)
NAVAJO UNITS 1A, IB, IC, AND ID
S09
c
Ducts
0(0)
-2(—2)
0(-2)
-7(-8)
-3(-3)
-3(-3)
A
-2(-3)
+2(+2)
-3(-2)
+2(+l)
—2(—2)
-6(-5)
B
0(-l)
-2(-3)
+1(+1)
-7(-8)
+2(+2)
—3(—3)
C
-4(-3)
+2(+2)
-2(-1)
+2(+4)
+2(+5)
+3(+4)
D
•
• •
«
•
•
t •
•
1 ~
1 +5(+4)
' +5(+4)
. ' +10(^6) f
1 +10(+10)
-3(-3)
+4(+4)
+6(+6)
+3(+5)
-3(—2)
.-3(-3)
-2(-3)
+7{+9)
-ll(-ll)
. +4(+3)
+3(0)
0(+3)
-3(-3)
+5(+4)
+6(+4)
+8(+13)
1
-3(-3)
+4(+9)
' +11(+11)
+11 (+11)
1 * +14(+11)*
1 +6(+9)
—3(—3)
+8(+7)
+6(+4)
+6(+8)
—3(—2)
. +7(+7)
-6(-7)
+11(+12)
—3(—3)
. —3(—3)
+3(0)
+7(+9)
+2(0)
.+7(+7)
+3(0)
+8(+10)
-3(-3).
+5(+6)l .
+3(+2)
0(+5)|
•
+3(+2)
+11 (+11)
| ' +10(+8) '
+2(+3)
+4(+4)
+6(+4)
-7(-2)
+5(+6)
-3(-2)
+4(+4)
•-6(-7)
+7(+7)
+3(+2)
—4(—3)
*+1(0)
+15(+16)
-3(-3)
.+2(0)
-5(-7)
+12 (+14)
-3(-3)
-1 (-2)1 .
-1 ("2)1
+3(+7)
1
1
•
• •
•
•
f
• •
Ducts
+2(+2) A
-11(-10) B
-4(-4) C
-22(—23) D
-u-i)
+4(+4)
+5(+4)
+7(+9)
Note: Only 1 run
was made per duct.
0(0)
+5(+5)
+4(+2)
+10(+13)
+l(+2)
+4(+3)
-l(-2)
+9(+11)
-3(-3)
0(-l)
-3(-4)
-5(-5)
-------
NAVAJO UNITS 1A, IB, 1C, AND ID
NO..
-4(-4)
-3(-4)
+3(0)
-l(-2)
-l(-l)
0(0)
SRI'
—3(—2)
+1(0)
-2(-3)
+1(0)
0(-l)
-10)
0(0)
¦1("2)
+2(+2)
0(0)
+1(0)
+l(+i)
+3(+2)
+4(+4)
-l(-l)
0(+2)
+3(+3)
+l(+2)
0(0)
+2(+2)
Note: See Navajo Unit
S0~ data sheet for
change In notation.
a
+4(+2)
+4(+l)
-H-1)
+3(+4)
0(0)
+4(+l)
+1 (+1)
+K+1)
+1(0)
-1(0)
0(0)
-K+D
+l(-D
o(+i)
+1(0)
-l(-2)
+1(0)
-1(0)
0(0)
0-1)
0(0)
+1(0)
ro
ro
-------
NAVAJO UNIT 1 - STACK
+4(+4)
+1(+1)
0(0)
+K+1)
-l(-6
+U-3
+3(+6)
Sft
•+4(+l)
+2(+l)
SIS)
1—7(—6)
-1(-1)
0(-6)
-l(-6)
-K-D
-2(0)
o(+i)
-i(-i)
o(-l)
+3(+10)
+2(+6)
l(-3)
-8(-15)
+3(-3)
-0(+l)'
-3(—4)
0(0)
o(-l)
+l(+7)
+3(+8)
-3(-3)
+2(+D
-------
NAVAJO UNIT 1 - STACK
:S>'
ofo)
-l(-2)
-3(-9
+1C-2
+6(+9
-3(-10)
+l(-4)
+8(+10)
+1(+8)
+1(-2)
+4(+3)
+9(+12)
+l(+5)
-6-6)
+4(+3)
-14(-21)
-l(-7)
'+8 (+8 J
-2(-3)
+4(+8)
-2(+2)
-2-4)
-6(-7)
+15(+20)
0(+5)
-3(-4)
—5(-6)
-2(-2)
0(-l)
0(0)
+2(+2)
ro
-f*
VI
-------
6/ix/ys
THERMOCOUPLE CALIBRATION PROCEDURE EVALUATION
Kenneth Alexander*
Introduction
The Federal test methods^published in the August 18, 1977,
Federal Register require that thermocouple-potentiometer systems
be calibrated after each field use. Above 405°C, an NBS calibrated
reference thermocouple-potentiometer system or an alternative
reference, subject to the approval of the Administrator, is
specified for the comparison. Since the calibration procedure
requires the use of high temperatures in the laboratory and the
use of expensive reference thermocouples, a study was conducted
to determine whether extrapolated values from low-temperature
calibrations would provide sufficiently accurate values at the
high temperatures.
The purpose of this paper is to report the findings of the
study and to establish a simplified calibration procedure.
Equipment and Procedure
Six chrome!-alumel (type K) thermocouples and one potentiometer
with readout were selected for calibration. ASTM mercury-in-glass
reference thermometers and an NBS calibrated platinum-rhodium
(type S) thermocouple-potentiometer were used as the temperature
references.
*Emission Measurement Branch, ESED, OAWPS, EPA, Research Triangle
Park, May 1978.
-------
The following procedures were used in calibrating the thermo-
couples:
1. For the ice point (32°F) calibration, crushed ice and
liquid water were placed in a Dewar vessel to form a slush. The
thermocouples were placed in the slush to a depth of not less than
2 inches, and care was taken so that they did not touch the sides
of the vessel.
After a 3-minute wait for the system to reach thermal equi-
librium, the readout on the potentiometer was. observed and recorded.
Eight readings were taken in 1-minute intervals. When necessary,
ice was added and excess liquid drained off to maintain a temp-
erature of 32°F.
2. For the boiling point calibration a hot plate and a
Pyrex beaker filled with deionized water and several boiling chips
were used. After the water reached a full boil, the thermocouples
were placed in the water to a depth of no less than 4 inches and
the system was allowed to equilibrate for 3 minutes. Eight
potentiometer readings were obtained in successive 1-minute in-
tervals and recorded. Barometric pressure was also recorded
periodically. The temperature of the boiling water was measured
concurrently with a reference thermometer to obtain the correct
temperature of the water.
3. For higher temperature calibrations, a tube furnace and
ASTM reference thermomuters (up to 7C0°F) or the NBS calibrated
platinum-rhodium reference thermocouple (above 760°F) were employed.
-------
3
The tube furnace had a heated cylindrical volume approximately
13 inches in length and a 1-inch I.D.; the volume at either end
was opened to the atmosphere.
The highest and most stable temperature was found to be
at the center of the oven volume. This is where the tip of the
reference device and the tip of the thermocouple were placed.
The test and reference thermocouples were inserted into the
furnace at least 4 inches. The ASTM reference thermometers,
however, which were designed for full immersion, could not be
totally immersed 1n the furnace. A temperature correction
was made, therefore, for the length of the mercury shaft that
was exposed to the outside of the furnace.
To minimize temperature fluctuations, the furnace was
heated 509 to 100° above the desired calibration temperature
and then allowed to cool at a rate that the slower responding
device could accommodate. When it was clear that both devices
were responding to the temperature drop at the same steady rate,
temperature readings were recorded at 1-minute Intervals until
eight readings were obtained. The average of all eight readings
was taken as. the calibration temperature. Several high-temperature
calibrations were made in the range of 600° to 1600°F.
To determine whether the thermocouples lose any of their
accuracy or precision at low temperatures after repeated
exposure to high temperatures, three thermocouples were successive-
ly calibrated at.the 1ce point, boiling point, and approximately
1600°F.
-------
4
Discussion_of Results
Results of all tests are summarized in Tables 1, 2, and 3.
Table 1 lists the temperature observed. Table 2 shows the results
of constructing an extrapolated curve from only the ice point and
boiling point data found in Table 1 by using the least-squares
method. The final column in Table 2 shows the percent error be-
tween extrapolated and actual values to be always less than 1.1
percent. This is well within the specified accuracy^ of 1.5 percent
of the measured absolute temperature. Table 3 summarizes the tests
made to determine the retention of calibration by thermocouples
after repeated cycling between high and low temperatures. The
percent error between the observed and reference temperatures 1s
never more than 1 percent and rarely above 0.5 percent. Thus,
there seems to be no indication that any loss of precision or
accuracy occurs by cycling the thermocouples between temperature
extremes.
Recommended Procedure
The following procedure is recommended for calibrating thermos'
couples for field use:
1. For the ice point calibration, form a slush from crushed
ice and liquid water (preferably deionized, distilled) 1n an
insulated vessel such as a Dewar flask.
Taking care that they do not touch the sides of the flask,
insert the thermocouples into the slush to a depth of at least
2 inches. Wait 1 minute to achieve thermal equilibrium, and
record the readout on the potentiometer. Obtain three readings
-------
taken in 1-minute intervals. (Longer times may be required to
attain thermal equilibrium with thick-sheathed thermocouples.)
2. Fill a large Pyrex beaker with water to a depth of no
less than 4 inches. 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 thermocouple(s) in the boiling water to a
depth of at least 2 inches, taking care not to touch the sides
or bottom of the beaker.
Alongside the thermocouple(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
p
will be required to give the correct reference temperature.
After 3 minutes both instruments will attain thermal
equilibrium. Simultaneously record temperatures from the ASTM
reference thermometer and the thermocouple-potentiometer three
times at 1-minute intervals.
3. From the calibration data obtained in the first two
steps of the procedure, plot a linear curve of observed temperature
versus reference temperature. Extrapolate a linear curve from
these two points using the least-squares method, and the result will
be a calibration curve for higher temperatures (up to 1500°F)
accurate to within 1.5 percent on the absolute temperature scale.
4. For even greater accuracy 1n constructing a calibration
curve, it is recommended that a boiling liquid (such as cooking
oil) be used for a calibration point in the 300°- 500°F range.
-------
6
References
1. "Standards of Performance for New Stationary Sources,
Revisions to Methods 1 - 8," Title 40, Part 60. Federal Register,
Vol. 42, No. 160 August 18, 1977.
2. Weast, Robert C., Handbook of Chemistry and Physics,
54th Edition, CRC Press, Cleveland, Ohio, 1973, pp. D158.
-------
Table 1: DATA SUMMARY OF THERMOCOUPLE CALIBRATION
I.D. NO.
101-'
I.D.
NO.'
02
I.D. NO.
103
_ Test
temperature,°R
Reference
temperature. °R
Test
temperature?R
Reference
temperature,°R
Test
temperature, °R
Reference
temperature. °R
494
492 (32°F)
. 494
492
493
492
676
675 (216°F)
676
675
674'
.672
1113
1108 (648°F)
1295
1292
il!8
1114
1261
1260 (800°F)
1596
1583
1276
1273
1664 .
1658 (1196°F)
1537
1537
1969
1972 •
I.D.
11
NO.
38
I.D. NO.
110
I.D
1"
NO. .
1
Test
temperature.°R
Reference
temperature. °R
Test
temperature?R
Reference
temperature,°R
Test
temperature. °R
Reference
temperature, °R
: 493 •
492
493
492
-• 493
• ¦ 492
674
fi7?
- fi7?
674
672.....
:v/C
O / ®T
1107
1104
1298
1295
1293
1285
1304
TpQQ *
. 1618 ...
1624
1609 •
1598
1590
2074
2064
- - - ¦ * . " ¦
2012
2018
-------
Table 2: TRUE REFERENCE TEMPERATURES VERSO'S EXTRAPOLATED REFERENCE TEMPERATURE
I.D. NO.
Observed
temperature,
°R
Reference*
temperature,
°R
Reference Temperature
Extrapolated From 32°,
212° F (1), R°
% Error Between Actual
: Reference*. And
Extrapulated Reference
101
1261
1260
1263
0.24
101
1663
1658
1667
0.54
102
1295
1292
1297
0.39
102
1596
1583
1600
1.07
103
1276
1273
1271
0.16
103
1537
1537
1530
0.46
103
1969
1972
1960
1.0
108
1304
1298
1298
0
108
1598
1530
1591
0.06
" ; 108
' 2012
2018
2003
. '1.0
110
1298
1295
1293
0.15
110
1628
1618
1621
0.18
no
2074
2064
2064 •
. o
in
1293
1235
1288
0.23
in
1624
1509
1617
0.50
-------
Table J: EFFECTS OF REPEATED CYCLING BETWEEN HIGH MD LOW TEMPERATURES
I:b: No;
no
I.D. No.
103
I.D. No.
108
Run
Test
temoei-dture
' °R
Reference
tepo^rature,
' °R
% Error
Test
temperature,
°R
Reference
temperature,
.?R
XError
Test j
temperature,
Or
Reference
temperature,
°R
% Error
1
493
492
0.2
493
492
0.2
493
4Q?
n ?
2
493
492
0.2
493
492
0.2
4Q4
4Q?
ft 41
3
493
492
0.2
494
492
0.41
494
4Q?
n ai
4
493
492
0.2
494
492
0.41
494
4Q?
n di
5
493
492
0.2
494
492
0.41
494
492
0.41
6
494
492
0.41
494
492
0.41
494
4Q?
n-4i
1
675
672
0.45
674
672
0.3
674
672
n 3
2
674
672
0.3
674
672
0.3
674
67?
n 3
3
674
672
0.3
674
672
0.3
674
67?
0 3
4
674
672
0.3
674
672
0.3
674
67?
0.3
5
675
672
G.45
674
672
0.3
674
672
0.3
6
675
672
0.45
674
672
0.3
674
' 672
n.3
1
2090
2074
0.77
2076
2053
0.63
2069;:
2063
n ?q
2
2110
2100
0.48
2097
2090 '
0.33
2038
2032
n.3
3
2068
2056
0.39
2063
2056
0.34
2064
2056
0.39
4
2096
2085
0.53
2092
2086
0.29
2094.
2087
0.34
- 2382
2374
0.34
2381
2373
0.34
2378
2373
0.21
|6
' 2079
2075
0.19
2080
2074
0.29
2079
2073
0.29
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Office of Air Quality Planning and Standards
Research Triangle Park, North Carolina 27711
subject: Stack Sampling Technical Information
DATE: MAR 101978
pROM: Roger T. Shigehara, Chief, Test Support Section
Emission Measurement Branch, ESED (MD 19)
T0: See Below
&
RECEIVED
MAR 16 1978
S & A DiVSION
The present procedures in EPA Reference Methods 4, 5, 6, 11 and
13 specify that a wet test meter be used as the calibration standard
for volume measurements. A recent study has shown, however, that a
properly calibrated dry gas meter may be used in lieu of a wet test
meter. The enclosed stack sampling technical document, "Procedure
for Calibrating and Using Dry Gas Volume Meters as Calibration
Standards," sets forth the procedure for their use.
The reference test methods will be revised at a later date to
specifically allow the use of standard dry gas meters as an alterna-
tive. In the meantime, the enclosed procedure may be used.
Enclosure
Addressees:
John Feldman, Region I
Robert Kramer, Region III
Richard S. DuBose, Region IV
Jerome J. Rom, Region IV
Ed Zylstra, Region V
Phil Schwindt, Region VI
William A. Spratlin, Region VII
Lee Daniels, Region VIII
Arnold Den, Region IX
Robert D. Harp, Denver Federal Center, NEIC
Louis Paley, EG 341
Rodney Midgett, (MD 77)
Directors, Enforcement Division, Regions I-III, V-X
Director, S. & A Division, Region X
I
-------
PROCEDURE FOR CALIBRATING AND USING
DRY GAS VOLUME METERS AS
CALIBRATION STANDARDS
P. R. West!in and R. T. Shigehara
INTRODUCTION
Method 5,^ "Determination of Particulate Emissions from Sta-
2
tionary Sources," and APTD-0576, Maintenance, Calibration, and
Operation of Isokinetic Sampling Equipment, specify that a wet
test meter be used as the calibration standard for volume measure-
O
ments. A recent study has shown, however, that a properly cali-
brated dry gas volume meter may be used in lieu of a wet test
meter for calibrating Method 5 equipment. The procedure below
outlines the proper calibration steps for preparing a dry gas
volume meter as a calibration standard. In addition, the proce-
dures outlined in APTD-0576 for calibration of a dry gas meter
in the Method 5 sampling train are modified to reflect the find-
ings of the above mentioned study•
CALIBRATING THE STANDARD DRY GAS METER
The dry gas meter to be calibrated and used as a secondary
reference meter should be of high quality and have a scale of
3 liters/rev (0.1 ft /rev). A spirometer (400 liter or more capacity)
may be used for this callbratipn, although a wet test meter is
usually more practical. The wet test meter should have a scale
of 30 liters/rev (1 ft /rev) and capable of measuring volume to within
<_ 1.0 percent; wet test meters should be checked against a spiro-
meter or a liquid displacement meter to ensure the accuracy of
the wet test meter. Spirometers or wet test meters of other sizes
-------
may be used, provided that the specified accuracies of the proce-
dure are maintained.
Set up the components as shown in Figure 1. A spirometer may
be used in place of the wet test meter in the system. Run the ,pump
for at least 5 minutes at a flow rate of about 10 liters/min
(0.35 cfm) to condition the interior surface of the wet test meter.
The pressure drop indicated by the manometer at the inlet side of
the dry gas meter should be minimized [no greater than 100 mm HgO
(4 in. H20) at a flow rate of 30 liters/min (1 cfm)]. This can be
accomplished by using large-diameter tubing connections and straight
pipe fittings.
The data collected for each run include: approximate flow rate
setting, wet test meter volumes, dry gas meter volumes, meter
temperatures, dry gas meter inlet pressure, barometric pressure,
and run time. Figure 2 shows an example data sheet that may be used
in data collection. Repeat runs at each orifice settings at least
three times.
Repeat the calibration runs at no less than five different
flow rates. The range of flow rates should be between 10 and
34 liters/min (0.35 and 1.2 cfm).
Calculate flow rate, Q, for each run using the wet test meter
gas volume, Vw, and the fun time, ©. These calculations are as
follows:
2
-------
thermometers!
CONTROL'
'VALVES
U-TUBE
MANOMETER
THERMOMETER(V
MANOMETER
I WET TEST METER
PUMP I
DRY GAS METER
Figure 1. Equipment arrangement for dry-gas meter calibration".!
-------
DATE:.
DRY GAS METER IDENTIFICATION:
BAROMETRIC PRESSURE (Pb>: in. H|
APPROXIMATE
FLOW RATE
(a)
cfm
SPIROMETER
(WET METER)
GAS VOLUME
(Vs)
ft3
DRY GAS
METER
VOLUME
(Vdg)
ft3
TEMPERATURES
DRY GAS
METER
PRESSURE
(Ap)
in. H2O
TIME
(0)
min.
FLOW
RATE
(a)
cfm
METER
METER
COEFFICIENT
(Yds)
AVERAGE
METER
COEFFICIENT
('j.)
SPIROMETER
(WET METER)
W
°F
DRY GAS METER
INLET
(ti)
°F
OUTLET
(t0)
°F
AVERAGE
(td>
"F
0.48
0.6B
¦
0.80
1JOO
1.20
-
V, (tj + 460) ^
Vdg (ts + 460) {Pfa + ^).
Figure 2. Example data sheet for calibration of a standard dry gas meter for method 5 sampling equipment (English unitsj.
a
Yds
-------
P V
Q - 0.3855 (t * gy3y / (SI units)
w
P V
Q " 17-65 (t' + 460) r (English)
w
Equation'1
Calculate the dry gas meter coefficient, Y^, for each run as
follows:
Vw (t .e + 273) P.
Yjc ¦ w— "rr—units)
d. Vds (tw ~ 273)
Equation 2
Vw (*,
-------
determine the maximum and minimum values. The difference between
the maximum and minimum values at each flow rate should be no
greater than 0.030. Extra runs may be made in order to complete
this requirement. If this specification cannot be met in six
successive runs, the meter is not suitable as a calibration stan-
dard and should not be used as such. In addition, the meter coef-
ficients should be between 0.95 and 1.05. If these specifications
are met, average the three values at each flow rate resulting
in five average meter coefficients,
Prepare a curve of meter coefficient, versus flow fate,
Q, for the dry gas meter. This curve shall be used as a reference
when the meter is used to calibrate other dry gas meters an4 to
determine whether recallbration is required.
USING THE STANDARD DRY GAS METER AS A CALIBRATION STANDARD
The sampling dry gas meter shall be calibrated as it will be
used In the field; therefore, 1t shall be Installed Into the field
meter box, if applicable, prior to calibration. Set up the com-
ponents as shown in Figure 3. Run the pump 1n the meter box about
15 minutes to warm the pump apd other components. Select three
equally spaced flow rates for calibration that cover the range of
flow rates expected in the field. Then collect the data for cali-
bration. These daw include approximate flow rate, orifice setting,
initial and final standard dry gas meter volumes, initial and final
meter box gas meter volumes, meter temperatures, barometric pres-
sure, and run time. Repeat the runs at each flow rate at least twice.
4
-------
I UMBILICAL'
ITHERMOMETERS
O
V
i
METER BOX
CALIBRATION
I DRY TEST METER |
Figure 3. Meter box calibration set-up.|
-------
The range of flow rates will depend somewhat on the use of
the meter in the field. That is, if the meter is to be used at
flow rates between 10 and 34 liters/min (0.35 and 1.2 cfm), then
duplicate calibrations should be run at three equally spaced flow
rates between these two values.
Determine the flow rate for each run using the standard dry
gas meter volume, V^.
Using the curve of versus flow rate established earlier for
P V
Q - 0.3855^-4-273) I8,
(SI units)
Equation 3
(English)
the standard dry gas meter, determine the meter coefficient. Y^,
at each orifice setting, AH, as follows:
vds (td + 273> pb
-------
Calculate an average Yd over the range of operation and calci" i.e
a standard deviation for all the calibration runs. The maximum ^i.in-
dard deviation should not exceed a value of + 0.020. Figure 4 shows
an example data sheet that may be used for these calibrations with
the necessary calculations. The average Y^ should be marked on the
calibrated meter box along with, the date of calibration and aH«, the
19
orifice setting that corresponds to 21 liters/min (0.75 cfm) at 20° C
and 760 mm Hg (68° F and 29.92 in. Hg).
RECALIBRATION OF STANDARD DRY 6AS METER
3
In a recent study a dry gas meter under controlled conditions in
a laboratory maintained its calibration within about 1 percent for
at least 200 hours of operation. It is recommended that the standard
dry gas meter be recalibrated against a wet test meter or spirometer
annually or after every 200 hours of operation, whichever comes first.
This requirement is valid provided the standard dry gas meter is kept
in a laboratory and, 1f transported, cared for as any other laboratory
instrument. Abuse to the standard meter may cause a change In the
calibration and will require more frequent recalibrations.
As an alternative to full recallbration, a two-point calibration
check may be made. Follow the same procedure and equipment arrange-
ment as for a full recallbration, but run the meter at only two flow
rates [suggested rates are 14 and 28 liters/min (0.5 and 1.0 cfm).
Calculate the meter coefficients for these two points, and compare
the values with the meter calibration curve. If the two coefficients
are within £ 1.5 percent of the calibration curve values at the same
flow rates, the meter need not be recalibrated until the next date for
6
-------
DATE: CALIBRATION METER IDENTIFICATION:
METER BOX IDENTIFICATION:. BAROMETRIC PRESSURE (Pb): in. Hg
APPROXIMATE
FLOW
RATE
(Q)
cfm
ORIFICE
READING
(AH)
in. H2O
CALIBRATION
METER
3AS VOLUME
Wdj)
ft3
METER BOX
METER
GAS VOLUME
(Vd)
ft3
TEMPERATURE
TIME
(0)
tnin.
METER BOX
METER
COEFFICIENT
(Yd>
(AH@)
CALIBRATION METER
METER BOX METER
INLET
(tda)
®F
OUTLET
(tdso)
-°F
AVERAGE
°F
INLET
W
•f
OUTLET
(W
°F
AVERAGE
(td)
°F
0.40
0.80
UO
-
AVERAGE
*
„ Vds ffjj + 460) Pk
y* * Yds tif i
Vd (tdj+460J (Pb + jJJl !
I
t
0.0317 AH (tijj + 460)Q~2 I
AHa = [— 1
Pb(tj + 460) Vdj 1 >f
\
WHERE: AH@ = ORIFICE PRESSURE DIFFERENTIAL THAT GIVES 0.75 cfm OF AIR AT 70° F AND 29.92 inches OF MERCURY, In. H2O.
TOLERANCE-±0.15 pM
Figure 4. Example data sheet for calibration of meter box gas meter against a calibration dry gas meter [English units).
%
-------
a recalibration check.
CALIBRATING THE DRY GAS METER FOR METHOD 6 SAMPLING
Method 6,^ "Determination of Sulfur Dioxide Emissions from
Stationary Sources," requires a meter box with a flow rate of
about 1 liter/min (2 cfh). A dry gas meter may be used as a stan-
dard volume meter for this application, if it has been calibrated
against a wet test meter (1 liter/min) or spirometer in the prdper
flow rate range. For this purpose, a dry gas meter standard need
be calibrated at 1 liter/min (2 cfh) and the meter box should be
calibrated against the standard dry gas meter at the same flow rate.
The calculations are similar to the ones described earlier. Again,
the calibrations of the standard meter should be repeated three times
against the wet test meter or spirometer. The calibration of the
meter box gas meter should be repeated twice. Example data sheets
for these calibrations are shown in Figures 5 and 6.
SUMMARY
A dry gas volume meter 1s calibrated against a spirometer or
a wet test meter under controlled conditions. A curve of peter
coefficient versus meter flow rate is established and kept with the
dry gas meter. The calibrated dry gas meter is then used as a
reference meter in the calibration of meters used in field testing.
REFERENCES
1. "Standards of Performance for New Stationary Sources,
Revisions to Methods 1-8," TitTe 40, Part 60. Federal Register.
Vol. 42, No. 160. August 18, 19-77.
7
-------
2. Rom, Jerome J. Maintenance. Calibration, and Operation
of Isokinetic Source Sampling Equipment. Environmental Protection
Agency, Research Triangle Park, N. C. APTD-0576. March, 1972.
3. Wortman, Martin, Robert Vollaro, and Peter Westlin.
Dry-Gas Volume Meter Calibrations. Environmental Protection Agency
monograph. Research Triangle Park, N. C. February, 1977.
8
-------
DATE: .
DRY GAS METER IDENTIFICATION:
BAROMETRIC PRESSURE (Pb): I in. Hg
APPROXIMATE
FLOW RATE
ft3
DRY GAS
METER
VOLUME
(Vdg)
ft*
TEMPERATURES
DRY GAS
METER
PRESSURE
(AP)
in.H20
TIME
(0)
min.
FLOW
RATE
(Q)
cfh
METER
COEFFICIENT"
(Yds)
SPIROMETER
(WET METER)
W
•f
DRY GAS METER
INLET
fcdi)
•f
OUTLET
(tdo)
°F
AVERAGE
(trf)
"F
2.0
AVERAGE
Vs Fb
Q - 1063
e (tf+460)
Vs {td + 46QJ Ph
VdS"v^ (tj + 460) "(ph+_^L,
Figure 5. Example data sheet for calibration of a standard dry gas meter for method 6 sampling equipment (English units).
-------
DATE: CALIBRATION METER IDENTIFICATION.
METER BOX IDENTIFICATION
BAROMETRIC PRESSURE {Pbh. m.Hg
APPROXIMATE
FLOW
RATE
(Q)
eft
ORIFICE
READING
(AH)
IlL-lljO
CALIBRATION
METER
GAS VOLUME
(Vds)
ft3
METER BOX
METER
GASVOLUME
®F
INLET
(tdi)
°F
OUTLET
ftdo)
•f
AVERAGE
(td)
°F
AVERAGE
Vds. fid + *60) Pb
«¦ ds V,
Figure 6. Example data sheet for calibration of meter box gas meter against a calibration dry gas meter {English units).
-------
AN ALTERNATIVE METHOD FOR STACK
GAS MOISTURE DETERMINATION
Jon Stanley and Peter R. West!in*
U(as(7&
Introduction
Reference Method 4, "Determination of Moisture Content in Stack
Gases," in Appendix A of Title 40 CFR Part 60, Standards of Performance
for New Stationary Sources, describes two sampling methods - a reference
method and an approximation method. The reference method employs
Smith-Greenburg Impingers; the approximation method uses midget
impingers. A study was conducted to determine whether the approximation
method sampling train and procedure could be modified and be used as
an alternative method. In addition, a similar study was conducted
with the Reference Method 6 train to determine whether the procedure
could be modified to simultaneously measure moisture content and S02
concentration.
Test results showed that the midget implnger sampling train can
be used for accurate moisture determination. This paper describes the
two alternative moisture measurement methods and presents a summary and
analysis of results of the field tests with the methods.
Test Method
1. Apparatus. The sampling equipment is the same as specified
for the moisture approximation method in Reference Method 4 and in
Reference Method 6, except for the addition of a silica gel trap.
(See Figures 1 and 2). The silica gel trap 1s a midget bubbler with
* Emission Measurement Brianch, Emission Standards and Engineering Division
Office of Air Quality Planning and Standards, Environmental Protection
Agency, Research Triangle Park, North Carolina 27711, August, 1973
-------
2
a straight tube.
2. Reagents
a. For the modified approximation Method 4, add 10 ml of
water to each of the first two implngers and approximately 15 g of
silica gel in the bubbler.
b. For the Modified Reference Method 6 train, add 15 ml of
80 percent isopropanol to the first impinger, 15 ml of 3 percent
hydrogen peroxide in the next two impingers, and approximately 15 g
of silica gel in the final bubbler,
3. Procedure
a. Apply silicone grease as necessary to the grou.id glass
fittings of the impinger halves. Wipe any extra grease from the ball
joint fittings and the outside of the impingers and weigh all the
impingers at one time to the nearest 0.05 gram. Record the weight.
b. Assemble the train as shown in Figure 1 or Figure 2.
c. Perform a leak check by disconnecting the first Impinger
from the probe and, while blocking the impinger Inlet, activating the
pump and opening the needle valve. An acceptable leak check is
achieved when the rotameter indicates no flow, the dry gas meter is
stationary for 1 minute, and bubbling in the impingers is limited to
less than one bubble per second. Release the impinger inlet plug
slowly, turn off the pump, and reconnect the probe.
d. Read the record the dry gas meter volume. Ice down
the impingers and heat the probe as necessary. Read and record the
barometric pressure.
-------
3
SILICA fi£L TUfiE
VALVc
rilTeR (CLASS WOOL)
J i: i uj/^oo
L !: >° *
I i,. i o o
i '•} i •
-Cj
o
ICE BATH
0«Y GAS METER
MIDGET IMPING EOS
Figure 1. Modified Approximation Method 4 train.
SILICA GELTU8E
R—-J^Qi
HEATEDPROBE
VALVE
lUI
fIL'Efl (GLASS WOQU
ICE HATH
/VIIOUST IWINGEftS
DAY GASMETEfl
Figure 2. Modified Reference Method 3 train for moisture determination.
7
-------
e. Start the sample pump and adjust the sample flow, .\ain-
tain the flow for the modified approximation Method 4 between 1 and
4 Hters/min and the flow for Reference Method 6 at 1 1pm.
f. Continue the sampling for 20 minutes or other appro-
priate sampling time. (The total moisture catch must be at least
1.0 gram to. maintain measurement accuracy.) Read and record the dry
gas meter temperature every 5 minutes during the sampling run.
g. At the end of the sample run, stop the pump and record
the final volume reading on the dry gas meter. Conduct a leak check
as specified in Part 3c.
h. Remove the impingers from the ice bath, cap them, and allow
them to warm to ambient temperature.
1. Wipe any moisture from the outside of the Impingers and
re-weigh thera in the manner specified in Part 3a.
Calculations
The following calculations are used to determine the moisture
content of the.stack gas:
0)
V, - 1.336 x 10'3 AW
Yfv
Where: Vwc ¦ Volume of water vapor condensed, corrected to
standard conditions, sera.
AW ¦ Total weight gain of the condenser and silica
gal trap assembly, g.
(2)
- 0.3855 Y * Pm * V„
y— m
-------
5
Where: V ¦ Dry gas volume measured by meter, corrected
mstd
to standard conditions, dscm.
Y • Meter calibration coefficient, dimensionless.
P ¦ Absolute meter pressure, mm Hg.
m
Tm ¦ Absolute temperature at meter, °K.
Vm ¦ Dry gas volume measured by meter, dent.
V.
(3) 3 - y x 100
wc mstd
Where: Bwe ¦ Water vapor content in stack gas, percent.
W5
Discussion and Summary of Test Results
A series of test runs was completed using the procedures
described in this paper on the exhaust of a gas-fired Incinerator.
Initial tests were made using trains based on the condensation
principle of Reference Method 4, but using midget impingers and
up to three silica gel traps 1n each train. A separate weighing of
these extra silica gel traps showed that complete (> 95 percent)
moisture collection was possible with the condensation train and
one silica gel trap. An error analysis showed that the moisture
collection must be at least 1 g to maintain the absolute accuracy
required of the method (see Recommendations).
Each test run consisted of two identical test trains (except
Run MA-19) operated simultaneously and the results were calculated
-------
from data collected by each train. The repeatability of the results
was determined by comparing the results of the two trains run side
by side. Table 1 shows a summary of test results, which includes
a brief description of the trains for each run.
Analysis of the results shows that either modified moisture
method is precise, can be used with no loss of accuracy, and can
be used as an alternative moisture method. Of the 13 duplicate
runs shown in Table 1, all but one yielded + 0.5 percent absolute
agreement or better between the results of the paired trains.
Error Analysis
The minimum moisture catch should be at least 1 g to assure
accurate results. An error analysis illustrates the importance of
the recommendation. For example, for a moisture weight gain of
0.60 g, a balance with an accuracy of + 0.05 g coyld produce results
-2
between 0.55 and 0.55 g, For a gas volume of 1.51 x 10 dscm,
these two values correspond to moisture levels of 4.6 and 5.4 percent,
respectively. Sampling the same stack gas until 1.0 g was collected
•2
would require 2.54 x 10 dscm of sample gas. A similar measurement
error of + 0.05 g in the sample weight gain would produce moisture
levels between 4.8 and 5.2 percent.
References
40 CFR Part 60, Standards of Performance for New Stationary
Sources, Federal Register. Vol. 42, No. 160, August 18, 1977.
-------
TABLE 1. SUMMARY OF RESULTS
Run
number
MA-2
MA-6
MA-7
MD-8
MO-9
MA-10
MA-12
MA-14
MA-15
Flow
rate
liters/min
4
1
1
2
2
2
3
3
3
Moisture
calculated
from
train 1
percent
3.6
7.6
7.1
5.9
6.7
6.0
6.4
5.2
4.8
Moisture
calculated
from
train 2
percent
4.1
8.0
7.2
6.0
6.6
5.9
6.3
5.2
4.9
Difference
0.5
0.4
0.1
0.1
0.1
0.1
0.1
0.0
0.1
Description
of
trains
1 water impinger
3 silica gel traps
2 water impingers
2 silica gel traps
2 water impingers
2 silica gel traps
2 water impingers
2 silica gel traps
2 water impingers
2 silica gel traps
2 water impingers
2 silica gel traps
2 v/ater impingers
2 silica gel traps
2 water impingers
2 silica gel traps
2 three percent perox
impingers
2 silica gel traps
Oq
-------
TABLE 1.
Roisture
calculated
Flow from
Run rate train 1
number 1 iters/min percent
MA-16 3 6.6
MA-17 3 6.9
HA-ie 3 4.8
MA-19
3
6.4
SUntlARY OF RESULTS
(Continued)
Roisture ~
calculated
from
train 2
percent
6.5
5.1
4.9
6.6
Difference
0.1
1.8
0.1
0.2
Description
of
trains
2 three percent
peroxide impingers
2 silica gel traps
2 three percent
peroxide impingers
2 silica gel traps
1 80 percent isoproperie
impinger
2 3 percent peroxide
impingers
1 silica gel trap
Train 1
1 80 percent
isopropanol
Impinger
2 3 percent perox-'
impingers
1 silica gel trap
Train 2
2 water impingers
2 silica gel traps
&
-------
Reprinted from American Industrial Hygiene Association
Journal, August 1978, Study funded by Environmental
Science and Research Laboratory, Environmental Protection
Agency, Research Triangle Park, N.C. 27711.
The causes and characteristics of tangential flow in industrial stacks are described. Errors
induced by tangential flow in the determination of volumetric flow rate and particulate
concentration are analyzed. Experiments were conducted at the outlet of a cyclone
collector in order to investigate the effect of tangential flow on the determination of
emission rates. Straightening vanes were found to be useful in the reduction of error in
flow rate measurements.
Sampling of tangential flow streams
DALE A. LUNDGREN'. MICHAEL D. DURHAM', and KERRY WADE MASON2
'Dept. of Environmenfal Engineering Sciences, University of Florida, Gainesville,
Florida 32611; 'South Carolina Dept. of Health and Environmental Control. Columbia,
South Carolina 29201
sources of tangential flow
Tangential flow is the nonrandom flow in a
direction other than that parallel to the duct
center line direction. It is often encountered in
industrial stacks and provides a difficult
situation for obtaining a representative
particulate sample and for accurate determina-
tion of flow rate. In an air pollution control
device, whenever centrifugal force is used as the
primary particle collecting mechanism,
tangential flow will occur. Gas flowing from the
outlet of a cyclone is a classic example of
tangential flow and a well recognized problem
area for accurate particulate sampling.
Tangential flow can also be caused by flow
changes induced by ducting. If the duct work
introduces the gas stream into the stack
tangentially, a helical flow will occur. Even if the
flow stream enters the center of the stack, if the
horizontal velocity is high compared to the
upward gas velocity, a double vortex flow
pattern will occur. In all of these cases, in a
cylindrical stack the flow will be characterized
by one or two primary vortices spiraling up the
stack. Since any other eddies produced in the
stack will be of a much smaller magnitude, there
will be very little interference and dissipation of
the primary vortex and thus, the spiraling flow
can be maintained the entire length of the stack.
Therefore, satisfying the requirement of
sampling 8 stack diameters downstream from a
flow disturbance will not eliminate the
tangential flow sampling problem.
errors caused by tangential flow
Types of errors that are introduced by tangential
flow are particle concentration gradients, nozzle
misalignment, and invalid flow rate and
concentration measurements. Concentration
gradients occur because the rotational flow in
the stack acts somewhat as a cyclone. The
centrifugal force causes the larger particles to
move toward the walls of the stack, causing
'higher concentrations in the outer regions.
The bias due to misalignment of the probe is
similar to that caused by superisokinetic
sampling. In this situation the nozzle velocity is
greater than the flow stream velocity and
therefore the sampled area will be greater than
the nozzle area. As the flow stream converges
into the nozzle some of the larger particles,
because of their inertia, will be unable to make
the turn and will not be collected. Therefore, the
particle concentration in the gas that is collected
will be less than the actual concentration. When
the nozzle is at an angle to the flow stream, the
projected area of the nozzle is reduced by a
factor equal to the cosine of the angle between
the flow direction and the nozzle axis. Even
though the nozzle velocity is equal to the flow
stream velocity, a reduced concentration will be
obtained because some of the larger particles will
be unable to make the turn in the nozzle.
Therefore, whenever the nozzle is misaligned,
the large particle concentration will always be
less than when the nozzle is aligned.
Previous investigations relating to
anisokinetic sampling have primarily dealt with
the bias induced when free stream velocity was
not equal to the suction velocity. This bias. A, is
defined as:
A=C,/Co (D
where Ci 35 volumetric particulate concentra-
S40
Am Intl. Hyg. Assoc J (39)
August. 1978
-------
tion in the nozzle, and
Co = volumetric concentration in the gas
stream.
It has been determined from experimentation
that the anisokinetic sampling bias. A, is a
function of two parameters: the inertial
impaction parameter, K, and the velocity ratio,
R. The parameters K and R can be defined by:
K - (CppV0DpJ)/(18^D1) (2)
where C = Cunningham correction factor,
pp = particle density,
V0 = duct velocity,
Dp = particle diameter,
H = gas viscosity, and
Di — nozzle diameter.
R - V./V, (3)
where Vi = probe inlet velocity.
The sampling bias is related to K and R by the
following expressions:"*2'
A - 1 + (R—I) /3(K) (4)
where £(K) is a function of both K and R.<2>
Sampling error associated with the nozzle
misalignment due to tangential flow has not
been adequately evaluated in past studies
because the sampled flow Held was maintained
or assumed constant in velocity and parallel to
the duct axis. The studies that have been
performed on the effect of probe misalignment
do not provide enough quantitative information
to understand more than just the basic nature of
the problem. Results were produced through
investigations on the effect of the nozzle
misalignment on the collection efficiency of 4,
12, and 37 urn particles.11' In a study on the
directional dependence of air samplers,<4> it was
found that a sampler head facing into the
directional air stream collected the highest
concentration. Although these results coincide
with theoretical predictions (i.e., measured
concentration is less than or equal to actual
concentration and the concentration ratios
decrease as the particle size and the angle are
increased), the data are of little use since two
important parameters, free stream velocity and
nozzle diameter, are not included in the analysis.
Particles of 0.68,6.0 and 20 pm diameter were
sampled'5' at wind speeds of 100, 200, 400, and
700 cm/sec with the nozzle aligned over a range
of angles from 60 to 120 degrees. A
trigonometric function was then used to convert
equation (4) to the form:
See equation S below
This function only serves to invert the velocity
ratio between 0 and 90 degrees and does not
realistically represent the physical properties of
the flow stream. In fact, equation (S) becomes
unity at 45 degrees regardless of what the
velocity ratio or particle size is. This cannot be
true since it has been shown that the
concentration ratio will be less than or equal to
unity, and will decrease inversely with angle and
particle diameter.
A more representative function can be
determined in the following manner: Consider
the sampling velocity V* to be greater than the
stack velocity V0. Let at be the cross sectional
area of the nozzle of diameter Di. The stream
tube approaching the nozzle will have a cross
sectional area a<> such that:
¦oV. = aiVi (6)
If the nozzle is at an angle 6 to the flow stream,
the projected area perpendicular to the flow is an
ellipse with a major axis Di, minor axis Dicos0,
and area (DiJ rrcos#)/4. The projected area of the
nozzle would therefore be a,cosfl. It can be seen
that all the particles contained in the volume
Voaicos0 will enter the nozzle. A fraction /3'(K) of
the particles in the volume (ao — a,cos0)Vo will
leave the stream tube because of their inertia and
will not enter the nozzle. Therefore, with Co, the
actual concentration of the particles, the
measured concentration in the nozzle would be:
c „„ C.a,cos0Vo[+ l-fl'(K)](ao-a,cosfl)VaC.
a,V, (7)
Using equations (6) and (3), this may be
simplified to:
A®11 + 0(K)[(V,sin0 + Vocos0)/(V.cosfl + Vosinfl)- I] (5)
American Industrial Hygiene Association JOURNAL (39) 8/78
641
-------
A = C/C. = I + J3'(K.) (Rcosfl—I) (8)
/J'(K) would be a function of the velocity ratio R
and the inertia! impaction parameter K,lJI and
would also be a function of the angle 6 because as
the angle increases, the severity of the turn that
the particles must make to be collected is also
increased. For small angles the sampling
efficiency will be of the form:'4'
A = 1 - 4sin(nK/0) (9)
Errors in the measurement of tangential flow
velocity and subsequent calculations of flow rate
are due primarily to the crudeness of the
instruments used in source sampling. Because of
the high particulate loading that exists in source
sampling, standard pitot tubes cannot normally
be used to measure velocity. Instead, the S-type
pitot tube is used because it has large diameter
pressure ports that do not easily plug. This type
of pitot tube can give an accurate velocity
measurement, but is quite insensitive to flow
direction. It can be misaligned up to about 45
degrees in either direction of the flow and still
read approximately the same velocity head. This
means that the S-type pitot tube cannot be used
in a tangential flow situation to accurately
measure the velocity in a particular direction.
The velocity in a rotational flow field can be
broken up into an axial and radial component.
The magnitude of the radial component relative
to the axial component will determine the degree
of error induced by the tangential flow. The
radial velocity component does not affect the
stack gas flow rate but does affect the measured
velocity because the S-type pitot tube lacks
directional sensitivity. If the maximum velocity
head were used to calculate the stack velocity,
the resultant calculated flow rates would be off
by a factor of 1/cosd. Aligning the probe parallel
to the stack centerline will reduce but not
eliminate this error because a large part of the
radial velocity component will still be detected.
Therefore, the actual stack gas flow rate cannot
normally be determined by an S-type pitot tube
in tangential flow because neither the radial
velocity Vr nor the axial velocity V. can be
measured directly. Also, V, increases in
magnitude as the probe is moved from the stack
center to the walls. Complicating analysis of the
subject is the fact that tangential flow is
sometimes accompanied by a reverse flow at the
stack center. One method to greatly reduce the
error in velocity measurement and flow rate
calculation is the use of in-stack flow
straighteners upstream from the sampling port.
These can eliminate the radial component of
velocity and allow a true flow rate to be
determined.
emission rate measurements obtained
from sampling the outlet of a cyclone
The outlet of a small industrial cyclone was
tested to determine the errors that arise from
sampling tangential flow.1" The previous
discussion suggests that sources of error induced
by tangential flow are: concentration gradients
across the stack, sampling bias due to
misalignment of the probe, and inaccurate
measurements of flow through the stack.
Experiments were also run to determine what
effect an in-stack flow straightener would have
on the measurement error.
experimental procedure
The major components of the experimental set
up included a dust feeder, fan, cyclone collector,
sampling equipment, and two stack extensions.
The test dust was a crushed gypsum rock with a
40 Atm mass median diameter (MMD). A
standard design, high efficiency cyclone
collector with a body diameter of 45 cm was used
as the collector. Dust leaving the cyclone had a
MMD of 2.7 nm. Two sampling trains were used
in the experiments: an Andersen cascade
impactor was used for particle size distribution,
and an EPA Method 5 train was used for particle
concentration and emission rate. The stack
extensions included a straight vertical stack
placed on the outlet of the cyclone; a second
extension turned the flow 90 degrees into a
horizontal duct section which contained a one-
foot long, cross type straightening vane.
Four types of tests were performed to
determine the errors involved in sampling
tangential flow: 1) velocity traverses at various
locations; 2) concentration measurements at
various probe angles; 3) emission rate
measurements at different locations; and 4)
particle size distribution measurements across
the dust traverse. Velocity traverses used for
determining volumetric flow rates were obtained
using an S-type pitot tube positioned parallel to
642
Am. Ind. Hyg. Assoc. J (39} August. 19/8
-------
the stack wall for one traverse and then rotated
to the point of maximum velocity head for
another traverse. A third velocity traverse was
performed in the section of duct following the
straightening vanes. To determine the effect of
sampling at various angles, four apparent
isokinetic samples were taken at 0,30,60, and 90
degrees with respect to the axis of the duct.
Emission rates were determined by sampling
downstream of the flow straighteners and
upstream in the straight stack extension. In the
straight stack extension, measurements were
made with the sampling nozzle aligned parallel
to the stack wall and also with the nozzle rotated
to the angle of maximum velocity head. Probes
were washed with acetone so wall losses were
included as collected particulate matter. Actual
emission rates were determined by subtracting
the collected dust in the cyclone from the dust
feed rate.
results
To determine the emission rate from a source, it
is necessary to determine the flow rate. Results
of flow rates determined at different locations of
the cyclone discharge indicated serious errors
can result in cases of tangential flow. A
maximum error of 212% (three times actual
flow) occurred when the pitot tube was rotated
to read a maximum velocity head. Sampling
parallel to the stack wall produced a flow rate
determination error of 74%. When sampling
downstream of the flow straightening vanes, the
flow rate error was reduced to 15%.
Dust concentration measurements were ma
-------
solution may not be feasible in large stacks
because of installation problems, cost, and
increased pressure drop created by the flow
straighteners.
acknowledgement
This research was funded in part by an
Environmental Protection Agency Research
Grant No. R803692.
references
1. Badzioch, S.: Collection of Gas-Borne Dust Particles
by Means of an Aspirated Sampling Nozzle. Sr. J.
App. Phys. 10:26(1959).
2. Betyaev, S. P. and L. M. Levin: Techniques for
Collection of Representative Aerosol Samples. J
Aerosol Sci. 5:325 (1974).
3. Watson, H. H.: Errors Due to Anioskinetic Sampling
of Aerosols. Am. Ind. Hyg. Assoc. J. 15:1 (1954)
4. GUuberman, H,: The Directional Dependence of Air
Samplers. Am. Ind. Hyg. Assoc. J. 75:1 (1954).
5. Ray nor. G. S.: Variation in Entrance Efficiency of a
Filter Sampler with Air Speed. Flow Rate, Angle, and
Particle Size. Am. Ind. Hyg. Assoc. J. 31:294(1970)
6. Fuchs, N. A.: Sampling of Aerosols. Atmos £nvir
9:697(1975).
7. Mason. K. W.: Location of the Sampling Nozzle in
Tangential Flow. M.S. Thesis, University of Florida.
Gainesville, Florida (1974).
Accepted February 15, 1978
844
Am. Ind. Hyt. Assoc. J (39)
August. 1978
-------
tjis
A METHOD FOR STACK SAMPLING CYCLONIC FLOW
Charles L. Goerner
Fred H. Hartraann
James B. Draper
Texas Air Control Board
Austin, Texas
Charles L. Goerner, B.S., M.S., P.E.
Engineer
Fred H. Hartmann, B.S., P.E.
Engineer
James B. Draper, B.S., P.E.
Engineer
Texas Air Control Board
8520 Shoal Creek Boulevard
Austin, Texas 7 8 758
-------
78-35.2
Abstract
This paper presents a method for particulate sampling in
stacks with cyclonic flow. Specific procedures and quantita-
tive adjustments to sampling parameters are described. Sam-
pling is performed isokinetically with the nozzle and pitot
tubes aligned parallel to the direction of flow and with sam-
pling time at each point weighted by the cosine of the flow
angle at that point. The method is specifically applicable
to particles with tangential velocity components without con-
sideration of radial velocity components. Comments are made
concerning the behavior of particles with radial velocity com-
ponents as applicable to the accuracy of this method.
-------
78-35.2 1
Introduction
Accurate sampling results cannot be obtained with conventional
sampling procedures from stacks with severe cyclonic flow,
i.e. flow with tangential velocity components. Cyclonic flow
may exist after cyclones, tangential stack inlets, or other
configurations that tend to induce swirling.
Several papers have been written describing and evaluating
various procedures for sampling cyclonic flow. This paper
presents a method that is currently being used by the Texas
Air Control Board staff. One inherent characteristic of this
method is that adjustments to the nozzle and pitot tube posi-
tion are made for tangential velocity components (yaw) but no
adjustments for radial velocity components (pitch) are made.
This fact and its possible effect on the accuracy of the meth-
od are discussed.
The generally accepted criteria for acceptable flow conditions
for stack sampling requires that the direction of flow be
within - 10° of the stack axis. If the flow direction is out-
side this range, special sampling procedures are needed to
obtain unbiased results. The angle between the longitudinal
axis of the stack and the plane of the pitot tubes when
aligned parallel to the flow direction is referred to as the
flow angle. It has the same magnitude as the angle between a
plane perpendicular to the stack axis and the plane of the
pitot tubes at the null (zero manometer reading) position.
The basic attempt of this paper is to describe the method as
applicable to determination of pollutant mass flow rates.
This requires determination of pollutant concentration as well
as volume flow rate. The procedure is not as complex if only
pollutant concentration is needed.
Particulate Sampling
A particulate stack sample must be extracted isokinetically at
each sampling point, and the volume extracted must be propor-
tional to the stack exit volume from each area increment.
If particulate sampling is performed with the nozzle and pitot
tubes in any position other than parallel to the flow stream,
various sources of bias are introduced. Distortions of nozzle
area and variations of pitot tube reading with flow angles
other than zero are sources of bias.l The method presented is
offered as a procedure to reduce biasing effects.
V
-------
H9
78-35.2
2
The volume extracted at a sampling point may be expressed as
Varying nozzle area (An) from point to point is not feasable,
and nozzle velocity must be equal to the velocity of the flow
stream. Therefore, sampling time at each point must be
adjusted so that the volume extracted at each sampling point
is proportional to the stack exit volume from each area incre-
ment. This is accomplished by weighting the sampling time at
each point according to the vertical component of velocity at
that point (cosine of the flow angle).
Suggested Procedure
Sampling parameters for cyclonic flow sampling are set up in
the same manner as for non-cyclonic flow. Preliminary velocity
traverse readings are taken with the pitot tubes aligned paral-
lel to the flow at each sampling point. The direction of flow
at each point is determined by locating the null position of
the pitot tubes (zero manometer reading) and then rotating the
pitot tubes 90° to obtain velocity measurements. The flow
angle at each sampling point is recorded during the preliminary
velocity traverse.
Isokinetic sampling is performed at each sampling point in the
normal manner except with the nozzle and pitot tubes aligned
parallel to the flow and with sampling time weighted according
to the cosine of the flow angle at each point. This may be
accomplished by selecting a basic sampling time for each point
which may be multiplied by the cosine of the previously mea-
sured flow angle for each point. Inspection of the planned
sampling times is necessary to insure that total sampling time
and volume are sufficient, and that the shortest sampling time
is long enough for accurate measurement and recording.
Calculations
Emission calculations on a concentration basis are
Vn = (A„) (vn) (t)
(1)
where:
Vn » Nozzle volume extracted at the point
An = Area of the nozzle
vn = Nozzle velocity at the point
t = Sampling time at the point
C - M/V
(2)
where:
C = Particulate concentration
M = Mass of particulate caught
V » Volume of gas extracted
-------
78-35 .2
3
The results are directly applicable to stack emission concen-
tration since the mass of particulate caught (M) and the vol-
ume of gas extracted (V) have been weighted according to the
stack exit volume from each area increment.
Emission calculations on a pollutant mass rate basis are
P - (M/V) (vs) (As) (COS F) (3)
where:
p = Mass flow rate of particulate
M - Mass of particulate caught
V * Volume of gas extracted
vs * Average measured stack velocity
As = Area of the stack
COS F = Average of the cosines of the flow angles
The emission concentration (M/V) is weighted according to the
stack exit volume from each area increment, and the average
measured stack velocity (vs) is measured with the pitot tubes
aligned parallel to the flow at each sampling point. There-
fore, the average velocity must be multiplied by the average
of the cosines of the flow angle at each point to obtain the
exiting component.
Calculations of isokinetic variation are made in the normal
manner. Since sample volume becomes weighted when sampling
time is weighted, no additional adjustments are necessary, and
input values to the isokinetic calculation are directly used
as measured.
Accuracy Considerations
According to sampling terminology, a large particle is one
that is influenced more by its own inertial characteristics
than by the flow stream. Therefore, when the nozzle is paral-
lel to the flow direction of a cyclonic flow stream it may not
be parallel to the flow direction of large particles in the
stream. This problem is not necessarily peculiar to cyclonic
flow streams. The effect of particle paths not parallel to
the nozzle is a smaller effective nozzle area resulting in
high isokinetic variation which in turn tends to induce a low
bias to the sample.1 The effects of this type bias have not
been quantitated but this sampling method is an attempt to
keep such bias to a minimum.
The sampling method presented is limited to flow streams with
tangential components of flow. The following exercise shows
that adjustments for radial flow components are unnecessary if
the sampling ports are at least two stack diameters downstream
from the stack inlet or disturbance.
-------
H
78-35.2
Consider a particle in a stack with a vertical velocity compo-
nent, v, a tangential velocity component, vt, and a radial
velocity component, vr, at a distance R from the center of the
stack.
The radial acceleration (Ar) of the particle due to centrifu-
gal effects of vt is
Ar = vt2/R (4)
If the particle starts from rest at the center of. the stack
(most restrictive case) and accelerates at Ar, the time (t)
required to reach the position, R distance from the center, is
t « R/(ivr) (5)
and vr - (*) (6)
Substituting (4) and (5) into (6)
vr » (vt2/R)(R/ivr)
Simplifying vr2 = 2 vt2 (7)
At the initial occurence of cyclonic flow (flow 10° from axial)
vt/v = tan 10°
or vt - v tan. loo (8)
Substituting (8) into (7)
Vr2 " v2(2 tan2 10°)
or vr = (0•25)v (9)
which shows that at the smallest flow angle at which cyclonic
flow exists, the radial velocity of a particle is one fourth
the vertical velocity# Therefore, if the sampling ports are
at least two diameters from the entrance to the stack, the
particle will reach the stack wall before reaching the ports
because it will travel half a diameter in a radial direction
while it travels two diameters in a vertical direction. If
the particle reaches the stack wall before reaching the ports,
no radial component of velocity is possible, and no pitch
adjustment of the probe is necessary. This is substantiated
by the cyclonic flow wock described by Phoenix and Grove 2
"Two 24-point traverses were chosen but, in most cases, points
1, 2, 23, and 24 were not sampled because of an excessive
amount of particulate and water droplets at the wall". If the
average flow angle in the stack is greater than 10^, the par-
ticle reaches the stack wall before travelling two diameters
-------
78-35.2
vertically. If the average flow angle in the stack is less
than 10°, sampling is performed in the normal manner with no
adjustments necessary.
-------
78-35.2
References
1. J. W. Peeler, "Isokinetic particulate sampling in non-
parallel flow systems - cyclonic flow", Entropy Environ-
mentalists, Inc., (1977) (Draft).
2. F. J. Phoenix and D. J. Grove, "Cyclonic flow - character
ization and recommended sampling approaches", Entropy
Environmentalists, Inc., EPA Contract 68-01-4148, (Novem-
ber, 1977) (Draft).
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Environmental Research Center
Research Triangle Park, North Carolina 27711
January 19, 1978
MEMORANDUM
SUBJECT: Clarification of How Soot Blowing is to be Included in
Performance Tests for New Power Plants
FROM: Kirk Foster
Technical Support Branch, DSSE
TO: Regional and State compliance testing coordinators
Requests for determination of applicability or other clarification
of the NSPS regulations are usually directed to" the Division of Stationary
Source Enforcement. DSSE prepares and periodically issues summaries of
NSPS determinations that have been made by the agency. These determinations
often involve questions related to compliance testing.
The attached determination, abstracted from the May 26 - September
16, 1977 Summary Report, addresses the problem of how periods of soot
blowing are to be included in the compliance test in a manner representa-
tive of their contribution to overall emission levels. If you have anv
questions regarding application of this technique, please contact vour
EPA Regional Office coordinator.!
pun**-
Al
-------
DETERMINATIONS OF APPLICABILITY OF NEW SOURCE PERFORMANCE
STANDARDS - MAY 26 - SEPTEMBER 16, 1977 SUMMARY REPORT
DETERMINATION CODE NO.: D-78
REFERENCE:
QUESTION:
Memo to R-VII (E. Reich
to R. Markey) 29 JUN 77
How is soot blowing to be included
in performance tests for fossil
fuel fired steam generators which
have non-automatic, non-contin-
uous soot-blowing?
AFFECTED REGULATION: 60.8
DETERMINATION:
Units which do not blow soot continuously must
have the effect of soot-blowing included b>/
performance testing in the normal manner,
provided that the following precautions are
taken: 1) soot-blowing is permitted only
during one of the test runs, 2) this soot-
blowing is representative of the plant's
typical cycle, and 3) the test run in which
the soot-blowing occurs is properly weighted
wh^n averaging with the other two test runs.
The soot-blowing performance test run should
include as much of the soot-blowing cycle as
possible. The weight of the soot-blowing
performance test run may be determined b.v the
following generalized equation. This equation
insures proper weighting of a soot-blowing
performance test run regardless of whether the
soot-blowing lasts the entire time of the test
run, and also regardless of the number and
duration of the non soot-blowing test runs
made while performance testing a fossil fuel-
fired steam generator.
WHERE:
W = ST/ (AR-SB)
R = the average number of
hours of operation per
24 hours day.
-------
S = the average number of
hours of soot-blowing
operation per 24 hour
day.
T = the total test time of
the non soot-blowing per-
formance test runs
(hours).
A = the time spent blowing
soot during the soot-
blowing performance
test run (hours).
B = the time spent not
blowing soot during the
soot-blowing perfor-
mance test run (hours).
Multiply the soot-blowing test run by W be-
fore taking the arithmetic mean of the per-
formance test runs as required by Section
60.8 (f).
-------
PARTICULATE SOURCE SAMPLING AT
STEAM GENERATORS WITH
INTERMITTENT SOOT BLOWING
OCTOBER 1, 1978
PREPARED FOR:
KIRK FOSTER
DIVISION STATIONARY SOURCE ENFORCEMENT
PREPARED BY:
JAMES W. PEELER
ENTROPY ENVIRONMENTALISTS, INC.
-------
PARTICULATE SOURCE SAMPLING AT
STEAM GENERATORS WITH INTERMITTENT
SOOT BLOWING
Introduction
At fossil-fuel fired steam generators which utilize intermit-
tent soot blowing practices, a major contribution to the total
particulate emissions from the facility often occurs during
relatively short duration soot blowing periods. Since emissions
during soot blowing periods can be quite significant, a procedure
is needed for conducting performance tests and weighting the
test results in a manner which will accurately reflects the
total emissions from the source. The major problem areas encount*
ered in developing such a procedure include: CI) establishing
a workable definition of "representative" emission values which
is directly comparable to the applicable emissions standard;
(2) determining representative source operation conditions for
conducting the performance test, (both for normal operating
conditions and soot blowing conditions); and (3) collecting
particulate samples which accurately reflect the emissions for
both source operating modes. This paper discusses these problem
areas and outlines methods which may be employed to determine
representative emission values for fossil-fuel fired steam gen-
erators with intermittent soot blowing. It should be noted that
some control agencies enforce emission standards which are effec-
tively "never to exceed" emission limitations. In this situation*
sources must comply with the emission standards during soot
blowing and testing must be conducted to reflect the maximum emis-
sions from the source. Other control agencies may exclude soot
blowing from all performance tests as a non-representative opera-
ting condition. This paper does not attempt to address either of
these issues.
*
-------
3opC>
Soot Blowing Practices / Effluent Characteristics
Soot blowing practices are highly variable between sources and
aVe subject to change both with time and with operating conditions
at any specific source. The frequency and duration of soot blow-
ing periods is dependent on many factors including: boiler
design, firing method, furnace operating conditions, combustion
efficiency, type of fuel, ash content of fuel, operating load,
and the frequency/magnitude of load fluctuations. Soot blowing
may be conducted as a regularly scheduled intervals or may be
initiated as necessary when indicated by operating parameters
such as increased pressure drop across the furnace and heat
exchanger surfaces, or decreased heat transfer efficiency.
Some modern large scale generators blow soot continuously. For
steam generators with intermittent soot blowing, the frequency
of the cleaning periods ranges from once per 24 hours to nearly
continuously. Both manual and automatic soot blowing systems
are used at steam generators.
The soot blowing process employs a number of lances to remove
accumulated material from the heat exchange surfaces in the fur-
nace, boiler, superheater, and air preheater while the boiler is
operating. The lances travel across the heat exchange surfaces
and remove the deposits by means of high pressure jets of steam
or air. The effectiveness of the lances is dependent on (1)
spacing of the lances, (2) nozzle design and ahgle of attack,
(3) air or steam pressure, (4) lance-to-tube speed, (5) frequency
and duration of operation, and (6) the nature of the deposits
on the tube surfaces.
The particulate concentration of the uncontrolled effluent stream
is subject to large temporal variations during the soot blowing
period due to the nature of the tube cleaning process. For a
specific lance, most of the accumulated material is removed
from the tube surfaces on the instroke of the lance. The re-
maining deposits are removed as the lance is retracted. In
addition, the cleaning process is usually initiated at the heat
H
-------
H*
exchange surfaces nearest the burners and moves downstream,
finally cleaning the air preheater. Since deposits on the various
heat exchange surfaces are generally not uniform, this method
ot cleaning adds to the temporal variations in the uncontrolled
particulate concentration during the soot blowing period. The
variations in the particulate concentration during soot blowing
may be minimized or "smoothed" to some extent by the particulate
control device and effluent handling system.
For the purposes of conducting particulate emission performance
tests, steam generators utilizing intermittent soot blowing
practices should be treated as cyclic or batch processes where
each cycle consists of a period of normal operation and a period
of soot blowing. The normal operation period is characterized
by steady-state source operation and relatively constant emission
levels over the duration of the performance tests. In contrast,
the soot blowing period is characterized by increased particulate
emissions and large fluctuations in the emission values over a
relatively short time period.
Representative Emission Values
Isokinetic sampling for particulate matter automatically integrates
or averages the particulate concentration of the effluent stream
over the duration of the sampling run. Thus, at most sources, the
time period for averaging emission values is indirectly defined by
the duration of the sampling run. Three sample runs are averaged
to determine the performance test results. For steam generators
with intermittent soot blowing, the fluctuations in particulate
concentration are relatively large and the interval between soot
blowing periods may be considerably greater than the duration of
the sampling runs. Therefore, at these sources, alternate sampling
procedures and alternate averaging or weighting procedures must be
employed to determine representative emission values.
For the purposes of this discussion, "representative" emissions
are considered to be the emission values which would be measured
if, for a given tine period, the entire effluent stream could be
-------
collected, well mixed, and then sampled. Employing this defini-
tion, the representative emission rate for a steam generator with
intermittent soot blowing is equivalent to the emission rate from
a! steady-state source which would produce the same net pollutant
mass emissions over the time period being considered.
Consider the simplest case where independent sampling runs are
conducted to determine the pollutant mass rate at normal operating
conditions and during soot blowing. If multiple sampling runs
are performed at either operating condition, then the averages of
the samples at each operating condition should be used to determine
the representative emission rate. The pollutant mass emission
rate which is representative of the emissions from the source,
(pmr), may be calculated from the following equation:
pmr »(pmr^t^ + pmr2t2) x 100
where: pmr. - average pollutant mass rate of
samples at normal operating
conditions
pmr2 • average pollutant mass rate of
samples during soot blowing
t1 - percent of source operation time
at normal operating conditions
t2 ¦ percent of source operation time
blowing soot
The volumetric flow rate, (dry, standard conditions) and percent
excess air are not expected to vary significantly between periods
of normal operation and periods of soot blowing. Therefore a
representative mass concentration, (C),or representative specific
emission rate, (E, lbs/10 Btu), may also be determined by simply
time weighting the measurements at each condition;
-------
C = (C,t. + C-t,) x 100
11 u u
(2)
E - PCC1tL + C2t2) x 100 x ( 20.9 - %C>2 ^
(3)
where: C, » average particulate concentration
of samples at normal operating
conditions
C~ ¦ average particulate concentration
of samples during soot blowing
It should be emphasized that if the volumetric flow rate varies
significantly between normal operation and soot blowing periods,
then alternate equations should be employed to determine repre-
sentative particulate concentrations and representative specific
emission rates. In addition, if the percent excess air varies
significantly between the two source operating modes, then alter
nate equations must be employed to determine representative spe-
cific emission rates. These equations are derived in Appendix A
of this paper.
As an alternate to conducting independent sampling runs during
normal operations and soot blowing periods, a representative
emission rate may be determined if sampling runs are conducted
at normal operating conditions and additional sampling runs are
conducted which include both normal operation and soot blowing.
In this case, the representative pollutant mass rate may be
calculated as:
pmr » pmr1(t1-|- t2) + pn»rx C^p)t2 x 100
*C4)
where:
pmr, - average pmr of sample(s) at normal operating
conditions
pmrx¦» average pmr of sample(s) containing soot blowi^
*This equation was developed by C. L. Goerner of the Texas Air
Control Board. See Appendix B for details./-
-------
t. ¦ percent of source operating time at normal
1 operating conditions
t2 » percent o£ source operating time blowing soot
A 3 hours of soot blowing during sample(s)
B a hours not soot blowing during sample(s)
containing soot blowing
The above equation may be employed to determine a representative
particulate concentration, (U) or representative specific emission
rate, (1") provided that the volumetric flow rate remains constant,
and in the case of the specific emission rate, the excess air also
remains constant. It should be noted that Equation 4 may be
employed even when independent sampling runs are conducted at
normal operating conditions and during soot blowing. In this
situation, 3*0 and Pmrx a prn^- Thus Equation 4 reduces to
Equation 1.
Sampling Strategies
Due to the variability of both operating conditions and soot
blowing practices between sources, an appropriate sampling strat-
egy should be devised for each source based on the source -
specific conditions encountered. It is essential that the source
operating conditions and soot blowing practices are clearly under-
stood and well documented in order to conduct performance tests
which are representative of emissions from the source. Factors
such as normal maximum operating load, frequency of soot blowing
periods, duration of soot blowing periods, and methods or para-
meters employed to initiate soot blowing should be considered.
Data from installed transmissometers may provide the most useful
information for establishing the conditions at which the source
should operate during the performance tests. The source should
note all periods of soot blowing on the permanent data record of
the transmissometer measurements. A comparison of the plant pro-
duction rate records and transmissometer data will then provide
a simple means for determining both the frequency and duration of
typical soot blowing periods while the source is operating at the
maximum normal production rate or other conditions which the con-
-------
trol agency may specify as representative conditions for conducting
the performance tests. In addition, assuming that a linear corre*
lation between the optical density and mass concentration of the
effluent exists, it provides a rough estimate of the relative
particulate emissions levels during soot blowing. Such an esti-
mate is useful in evaluating the significance of temporal varia-
tions during the soot blowing period and in determining the level
of effort which should be expended in sampling the soot blowing.
For example, if the transraissometer data indicates that the part-
iculate concentration is much greater during soot blowing and if
soot blowing constitutes a significant fraction of the total
source operating time, then more emphasis should be placed on
sampling the soot blowing period than would be expended in sampling
soot blowing periods at a source where the apparent particulate
concentration is not drastically increased during cleaning, or
where the cleaning periods are infrequent or of short duration.
For sources where the interval between soot blowing periods is
relatively short, performance tests should be conducted such that
each sampling run spans an entire cycle of normal operation and
soot blowing. Each sample traverse should be intitated at either
a different sampling point or at a different time in the operating,
cycle so that the composite sampling during the soot blowing period
is representative of the effluent across the entire stack or duct
cross section. The agency should not allow the source to schedul®
sampling such that sampling at a point of minimum velocity or
minimum particulate concentration is always coincident with the
soot blowing portion of the plant cycle. The average of three
sampling runs should provide a representative emission value.
For sources where the interval between soot blowing periods is too
long to permit sampling runs to be conducted over the entire oper-
ating cycle, two options are available: (1) separate sampling run*
may be conducted during normal operation and during soot blowing
to determine the parameters required for calculation of represen-
tative emission values; or (2) sampling runs may be conducted at
normal operating conditions and additional runs may be conducted
which include both normal operation and soot blowing to allow
^¦"Use of In-stack Transmissometer in Manual Source Sampling for
Particulate Mass Concentration Measurements", K.Foster,°N.White*
Presented at East Central Section, APCA Annual Meeting, Dayton,
Ohio, September 17-19, 1975.
-------
calculation of a representative emission value according to
Equation 4. The number of sampling runs used to determine values
f^r the appropriate parameters directly affects the accuracy of
the calculated emission rates. At a minimum, two runs should be
conducted during normal operating conditions and one run should
be conducted during or containing soot blowing. For sources where
soot blowing constitutes a very significant portion of the total
emissions from the source, it may be necessary to conduct more
than one sampling run during or containing soot blowing. Essen-
tially, the number of runs conducted at each operating condition
should be directly dependent on the fraction of emissions arising
during each operating condition. Sampling runs conducted during
soot blowing should span the entire blowing period due to the
existence of temporal variations in the effluent particulate
concentration over the cleaning cycle.
If independent sampling run(s) are to be conducted during the soot
blowing period, the short duration of typical soot blowing periods
will usually prohibit completion of a full sampling traverse during
the cleaning cycle. When a short duration soot blowing period re-
quires a reduced number of sampling points, all of the sampling
points should lie on the same stack or duct diameter to allow con-
tinuous sampling during the blowing period without interruption of
sampling to change ports. Ideally, the sampling points which are
selected would be representative of both the average particulate
concentration and average volumetric flow rate in the stack or
duct. However, the sampler and agency observer have no prior
knowledge regarding the particulate concentration variation across
the stack with the exception of those cases with obvious flow
disturbances. Sampling sites where the velocity profile is fully
developed and where the particulate concentration is relatively
uniform reduce the significance of measurement errors arising from
traversing only a portion of the stack. Single point particulate
sampling should always be avoided but may be necessitated at sources
with very short duration soot blowing periods. A point of repre-
sentative velocity should be selected when single point sampling is
required. When this situation is encountered the errors in the
-------
calculated emission rate due to sampling at a single point will
be minimized due to the relatively small fraction of the total
fissions occurring during the short soot blowing period. If more
than one soot blowing period is to be sampled, the sample traverse5
should be initiated at different sampling points, Cor conducted
at different sampling points for single point sampling) to mini-
mize the effects of concurrent spatial and temporal variations.
The effluent velocity must be measured at the point(s) sampled
during soot blowing runs in order to maintain isokinetic sampling
conditions. These velocity measurments should be compared to
the values measured at the same points during normal operation
sampling runs to check the validity of assumptions regarding con-
stant volumetric flow rate during both operational conditions.
For sources subject to specific emission standards, (mass per
unit of heat input) measurements of SCC^ and/or $02 during soot
blowing periods should be used to determine if the excess air
varies significantly between soot blowing and normal operation.
The equations in Appendix A should be employed to determine
representative specific emission values for sources where sig-
nificant variations in the percent excess air are encountered.
-------
APPENDIX A
N
-------
n
It should be noted that the method for determining a representa-
tive emission value is in some cases dependent on the applicable
amission standard, (i.e., mass emission rate, concentration, or
specific emissions standard - lbs/10^ Btu). Each case is consid-
ered separately in the following sections. The following nomen-
clature is employed.
C, - effluent particulate concentration during normal
operating conditions, (dry standard conditions)
C? - effluent particulate concentration during soot
blowing, (dry standard conditions)
Q. - effluent volumetric flow rate during normal operating
conditions, (dry, standard conditions)
Q, - effluent volumetric flow rate during soot blowing
(dry, standard conditions)
pmr^ - pollutant mass rate during normal operating conditions
pm^ - pollutant mass rate during soot blowing
- amount of time source operates at normal operating
conditions
- amount of time source blows soot
-------
I
Case I - Representative Mass Emission Rate, pmr
total mass emissions
pmr = total time A-l
The general equation for N operating modes is;
N N
V pmr. t. Y c.Q.t
pmr = fij[ i i - & * i i
\ A - 2
I. t. I. t.
1=1 l 1=1 l
For 3 FFFSG with intermittent soot blowing, N = 2, then;
pmr ^ T]_ + pmr-, T, ^l^l"1*! + C,Q,T-,
pmr _ _ _ _ A- 3
12 12
If the volumetric flow rate does not change during soot
blowing, then;
(C T + C T,)Q
5H7 t + T "5 * constant A_4
I 2
N
-------
Case II - Representative Concentration, C
^ _ total mass emissions A-5
C » total volume of effluent
The general equation for N operating modes is,
N
£, f-Vi Z CiQiti
c = * —
£ n
E Qiti E
N
C.Q.t.
1^1 i
A- 6
i = l
i = l
For a FFFSG with intermittent soot blowing, N = 2, then;
A- 7
l =
pmrl T1 + pmr2 T2 ^ C1Q1T1 + ^Q-,1,
Q1 T1 + Q2 h Q1T1 +
Q?t,
If the volumetric flow rate does not change during soot
blowing, then;
Ci1i + 4-8
C = T a. -f" " Q 31 constant
1 2
-------
Case III - Representative E, (lbs/106 btu)
_ total mass emissions
E = total heat input A"9
N
£ Pmri li
i-1 A-10
E - N
L Hi ci
i-1
where: H = heat input rate
Since considerable difficulty is encountered in attempting tc
measure heat input rates and/or total heat input, the F-factcr
method is usually employed. Therefore, a different approach
should be used to determine E, based on the parameters which
are actually measured.
2C.9 ^ 4-11
E * c F 20.5 - SO. 1
Define Z such that equation 11 can be written in generalized
form,
E (lbs/106 Btu) = C^ ?(€t St0ich-N)
\ft* J \ 10° Btu J
ft° v A-12
ft3 stoich
Since F is a constant, equation 10 can be written as;
f total mass emissions \ a -13
CT I total stoichiometric effluent volume ,
Note that § 3 Q
L s
where Q = stoichiometric volume flow rata
s
A general equation for N operating modes can be written as;
N
i?i CiQiti - £ C.Z.Q t.
ifJ: or » A-14
A Qj. ^
i-1 -l 1 ^ 'si1! ^
-------
For a FFFSG with intermittent soot blowing, N = 2
E = F
ci«iTi
~ C,Q,T,
L - 1
vr
Q2T2
L z
l
If the volumetric flow rate Joes not change during soot
blowing, then,
E =
ciTi + C2t:
ti +
Q = constant
A-16
If the excess air does not change during soot blowing, then
FZ
ci^iti * C;^2T2
L ^1^1 + ^2T2
Z = constant
A -17
If both t::? volumetric flow rati
Lte and excess air do not
change during soot blowing, then;
s C-
C1T1 * CZTZ
T1 + T2
Q = constant
Z = constant
A-13
For almost all steam generators with intermittent soot blowing
practices, the volumetric flow rate (dry standard basis) and the
quantity of excess air are not expected to vary between periods
of normal operation and periods of soot blowing, Therefore, simpl
time weighting the emission values can be employed to determine
the representative pollutant mass rate (eq> 4), representative
concentration (eq. 8), and the representative specific emission
rate, E (eq. 13). Where the volumetric flow rate, and in the
case of the specific emission rate E, the quantity of excej; air
vary significantly during soot blowing,the general form of the
equations should be employed to determine representative emission
-------
i i4m
APPENDIX B
-------
TEXAS AIR CONTROL BOARD
JOHN L. BLAIR
Chairman
CHARTS R. JAYNES
Vic# Chamman
BILL STEWART, P. E.
Executive Director
8520 SHOAL CREEK BOULEVARD
AUSTIN, TEXAS 78758
512/451-5711
WILLIAM N. ALLAN
JOE C. BRIOGEFARMER, P. E.
FRED HARTMAN
~. JACK KILIAN, M. 0.
FRANK H. LEWIS
WILLIAM 0. PARISH
JEROME W.S0RENS0N, P. E.
June 12, 1978
Mr. Quirino Wong
Surveillance & Analysis Branch
Environmental Protection Agency
Region VI
1201 Elm Street
First International Building
Dallas, Texas 75270
Dear Quirino:
As you know, we have had some problems with the recent EPA
determination concerning soot blowing in stack sampling
calculations. As suggested by yourself and Kirk Foster,
we would like to present our ideas for consideration.
The accompanying equation uses the pollutant mass rate (PKR)
basis but should-readily adjust to a concentration basis. It
yields a time averaged pollutant mass rate averaged over the
daily operating time. Although spikes are included in the
average, the equation has no penalty for spikes of emissions
above average (such as while blowing soot).
Development of the equation is included for the record.
'""m ¦ SBR ? * PMB!.OSB * !f>
PMR = Pollutant Mass Rato (lb/hr)
PMRavg = Average PMR for daily operating time
PMR3BR a Average PMR of sample(s) containing soot blowing
PMRN0Sb = Average PMR of sample(s) with no soot blowing
A » Hours soot blowing during sample(s)
B 3 Hours not soot blowing during sample(s) containing
soot blowing
R = Average hours of operation per 2k hours
S * Average hours of soot blowing per 2U hours
At least one sample must contain soot blowing and at least one
sample must contain no soot blowing.
Sincerely,
Charlie L. Coerner, P.E.
Source Evaluation Section
-------
Averaging Soot Blowing in Stack Samples
\4p'
PMRavg(r) - PMRsb(S) ~ PMRnosb(R-S)
PMR,-brCA*B) - PMRsb(A) * PMRnosbCB)
Solving equation (2) for PMRggi
PMRsb = (PMRSBRtA ~ B) - PMRnosbCB)] /A
Substitute equation (3) into equation (1) yields;
pu*avg(r> = ^mrsbr^ + " PMRNOSB(-B')^ A + PMRNOSB(-R"S-)
Collecting terms yields;
pmravg(R) - PMRsbr(A , B)f „ PMRnosb(R-S-^)
or;
PMR
AVG
PMR
PMR
AVG
PMR,
SB
PMR.
NOSB
PMRSBR
A
B
R
S
PMR S DMD ,-R~S . BS.
pmrsbr Tt pmrnosb c r ar-1
Pollutant Mass Rate (lb/hr)
Average PMR for daily operating time
PMR while blowing soot
Average PMR of sample(s) with no soot blowing
Average PMR of sample (s) containing soot blowing
Hours soot blowing during sample (s)
Hours not soot blowing during sample(s) containing
soot blowing
Average hours of operation per 24 hours
Average hours of soot blowing per 24 hours
(1)
(2)
(3)
(4)
(5a)
(5b)
n
-------
7/lS
NOTICE NO. 9A
Sro»
A number of procedures for deteriiiing representative emission values
for steam generators with intermittent soot blowing practices have been
considered. Although a final NSPS determination has not been prepared,
we can suggest at this time a preferred method for handling soot blowing.
After reviewing various techniques presently being used and per-
forming our own independent analysis of the problem and factors that must
be considered in developing an equation for adjusting performance test values
to reflect soot blowing emissions, we feel that the following equation de-
veloped by the Texas Air Control Board (C. L. Goerner) offers a satisfactory
and technically sound approach for determining a time-weighted pollutant mass
rate for the daily operating cycle.
PMRAVG " PMRSBRfA ARB) + PMRNOSB
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENC •
Office of Air Quality Planning and Standards
Research Triangle Park, North Carolina 27711
subject: Substitution of 10 Percent Ho09 for 3 Percent H,0o date: .yjAY 1 1 1Q7Q
in Method 6 Analysis 22 22 IV,HT 11 13/0
from: Kenneth Alexander, Test Support Section
Emission Measurement Branch, ESED (MD 19)
TO: Roger T. Shigehara, Chief, Test Support Section
Emission Measurement Branch, ESED (MD 19)
Introduction
The revised Method 6 published in the August 18, 1977
Federal Register calls for the use of 3 percent HpOg to
collect samples of S02 gas for analysis.
By bubbling SOp gas through HpOp, SO^ is oxidized to
H2SO4 which is then available for titration with barium
perchlorate (BaCClO^). Complete oxidation may not occur,
however, when SO? concentrations are high (C$02 > 15,000 mg/DSCM);
the 3 percent H0O0 is too dilute to oxidize large concentrations
of S02.
The objective of this test was to determine whether sub-
stituting 10 percent H2O2 for the 3 percent H2O2 would inter-
fere with the analysis procedure in Method 6.
Procedure
Audit samples were prepared by pipetting 5 ml of audit
solution into a 100 ml volumetric flask, then adding 30 ml of
3 percent H^Og and diluting to 100 ml with deionized water.
A second set of samples were prepared in the same manner sub-
stituting 10 percent H2O2 for 3 percent H2O2.
Three aliquots of each sample were titrated following the
normal procedure described in Method 6. Table 1 shows SOg
concentrations calculated from the titrated volumes.
Discussion and Conclusions
A t-test was made on the three pairs of average concentration
values shown in Table 1. At value of 1.063 was calculated;
using a t-table this value can be translated to say that there is
at least 95 percent probability that there is no significant dif-
ference between the two sets of data (concentrations of SO?).
This leads to the conclusion that there is no significant dif-
ference when 10 percent H2O2 is substituted for 3 percent H2O2
in the Method 6 analysis.
CPA Form I320"6 (R«v. 6-72)
0
-------
•3-P
2
As a check for the accuracy of the titrations, a percent,
error was calculated between the actual SO2 concentrations
and the concentrations calculated from the titrated samples.
The average percent error was 1.4 percent for the 10 percent
H2O2 solutions and 2.5 percent for the 3 percent solutions.
A percent error of 6.1 percent was calculated for sample #4349.
This could be clue to possible error in preparation of the audit
sample for titration or an error in the initial preparation of
the audit solution before reaching this laboratory. In either
case, it does not detract from the conclusion stated before
that substitution of 10 percent H2O2 ^or> 3 percent H2O2 ^oes
not cause any interference in the titration procedure.
Table 1. Titration of Audit Samples Prepared With
3% and 10% Hydrogen Peroxide
Sample
Number
Actual
s
mg/dscm
SOg
3% H202
mg/dscm
% Error
3% H202
lso2
10% h2o2
mg/dscm
% Error
10% h2o2
t-value
2220
4347
4338
0.2
4338
0.2
4349
5148
5464
6.1
5320
3.3
7409
1411
1428
1.2
1422
0.8
Average
2.5
1.4
1.063
0
-------
uf{
o.-j. i'iED STATES lIIWIRON.Vl^Yf AL MOTEC , AGENCY
Office of Air Quality Planning and Standards
Research Triangle Park, North Carolina 27711
subject: Method 8 Test for Peroxide Impurities in Isopropanol date: JUN 8 7978
from: Robert F. Vollaro, Test Support Section nL/
Emission Measurement Branch, ESED (MD-19)
TO: Roger T. Shigehara, Chief, Test Support Section
Emission Measurement Branch, ESED (MD-19)
In a recent letter (May 5, 1978), Mr. Vincent Ferraro of
the New York State Department of Health brought to our attention
what he considers to be "...technical error of omission..." in
the revised version of Method 8 (published in the August 18, 1977
Federal Register). Mr. Ferraro informed us (correctly) that the
method does not specify the optical path length to be used in the
test for peroxide impurities in isopropanol; rather, the method
simply states that the isopropanol shall have an optical density
of less than 0.1 at a wavelength of 352 nm.
A recent conversation with Joe Knoll (EMSL) confirmed that
Mr. Ferraro is correct in perceiving the need for a specified path
length in the isopropanol test procedure, because optical density
is a function of path length. According to Mr. Knoll, the most
commonly-used path length for this type of spectrophotometry
analysis is 1 cm. In view of this, to ensure uniformity of
application among source-testers, the peroxide impurity test pro-
cedure (which appears in both Methods 6 and 8), will be revised
to specifically state that a 1 cm. path length shall be used for
the isopropanol analysis.
Therefore, steps will be taken to see that the regional EPA
offices, source test contractors, and other affected parties are
notified of this revision.
cc: Foston Curtis (MD-19)
Vincent Ferraro, New York
Gary McAlister (MD-19)
J. E. McCarley (MD-13)
George W. Walsh (MD-13)
EPA Form 1320-6 («.». 4-72)
V
-------
METHODS FOR COLLECTING AND ANALYZING
GAS CYLINDER SAMPLES
Peter R. West!in and John W. Brown*
Introduction
Appendix of Part 60 - Standards of Performance for Mew
Stationary Sources - includes specifications for continuous moni-
toring equipment. These specifications require the analysis of
sulfur dioxide (S0?) and nitrogen oxides (NO ) calibration gases
b X
using Reference Methods 6 and 7, respectively.
Three gas cylinder sample collection and analysis procedures
are recommended as follows: (1) direct pressure, (2) vented
bubbler, and (3) evacuated flask methods. Laboratory tests
comparing these methods against National Bureau of Standards
(NBS) calibrated gases showed the error of individual measurements
to be within + 7 percent and the average of three consecutive
results to be within +5 percent.
Direct Pressure Method Procedure
The direct pressure method applies only to SOg cylinder gases
and uses Reference Method 6 sampling equipment and absorbing
solutions (see Figure 1). The mercury U-tube manometer is used
to monitor the system pressure at the inlet of the first impinger.
The isopropanol fritted bubbler in Reference Method. 6 need not
be used, and the meter box must be modified by by-passing the sample
pump.
~Emission Measurement Branch, ESED, OAQPS, EPA, Research
Triangle Park, North Carolina 27711, July, 1978.
-------
2
NCt:ni.E
VAJ .ML
CO
A
fSOTAMcTEfi
GAS
CYL
U !
a HYING
TUSE
U-TUBE i
MANOiVlcTEK
3%
h2°2
<15 ml]
DHY GAS
METER
Fitjure 1. Direct pressure method.
The procedure is as follows:
1. Place 15 ml of 3 percent hydrogen peroxide (HgOg)
absorbing solution in each of the two impirigers and connect
the manometer, impingers, and meter box as shown in Figure 1.
2. Open fully the rotameter valve.. Connect a zero-air
gas cylinder or other source of pollutant-free positive pressure
air in place of the calibration gas cylinder. Connect a
flow control valve between the zero-air cylinder and the mano-
meter. Plug the exhaust of the gas meter, and slowly open the
cylinder pressure valve until the manometer registers 0.5 in.
Hg. Close the pressure valve ana monitor the system pressure
for 3 minutes. If the pressure changes by more than 0.1
in. Hg. in 3 minutes, find the leak source, repair it, and
repeat the leak test. Relieve the pressure in the system at
the end of the leak test by removing the plug in the exhaust
or" the dry gas meter. After the system pressure reaches zero,
disconnect the zero-air pressure source and connect the SC^
-------
gas cylinder.
3. Record the initial meter volume, temperature, and the
barometric pressure. Open the gas cylinder valve, and adjust
the sample flow rate to 1 liter/min. Do not exceed 0.5-ir..
Hg pressure at the manometer; this is a key to obtaining
reliable resu.lts.
4. Record the meter temperature at ID-minute intervals;
sample until at least 1.0 cubic foot has been collected. Calcu-
late the sample concentration from the titration analysis and
the gas volume determination according to Reference Method 6.
Vented Subbler Method Procedure
The vented bubbler method applies only to SO^ calibration
gas cylinders and uses Reference Method 6 equipment and absorb-
ing solutions (see Figure 2). The midget bubbler (a straight
tube, no frit or impinger tip) is used to prevent excessive
pressure during sample collection. The impingers ar.d the meter
box are Reference Method 6 equipment.
ROTAMETEH
NEEDLE
VALVE
I / VEi\IT.(
ctf I
DRY GAS
METER
3031 U-TU3E :
H202 manometer
VENTED A
BUBBLER ( i
PUMP
2%
H202
(•15 mi)
Figure 2, Vunted bubbler method.
-------
4
The procedure is as follows:
1. Assemble the impinger train and meter box as described
in Reference Method 6. (The isopropanol fritted bubbler in
Reference Method 6 may be left empty or removed).
2. Conduct a positive pressure leak check as described in
step 2 for the direct pressure method from the manometer through
the test train. A negative-pressure leak check as prescribed
in Reference Method 6 is optional.
3. Fill the vented bubbler with 15 ml of 30 percent l^O^,
and complete the connections between the gas cylinder, the
vented bubbler, the U-tube manometer, and the test train. Re-
cord the barometric pressure, the initial gas meter volume reading,
and the meter temperature. Open the gas cylinder valve until a
steady stream of bubbles appears in the vented bubbler. Begin
sampling by starting the sample pump and adjusting the flow to
1 liter/min while maintaining a small stream of bubbles in the
vented bubbler. This flow of bubbles should be kept as slow as
practical, and the manometer reading should be monitored to
maintain the system pressure below 0.5 in. Hg. In addition, care
must be exercised in keeping the pump vacuum from exceeding the
pressure in the vented bubbler.
4. Record the meter temperature at 10-minute intervals; sample
until at least 1.0 cubic foot has been collected. Calculate the
sample concentration from the titration analysis and the gas volume
determination according to Reference Method 6.
-------
5
Evacuated Flask Method Procedure
The evacuated flask method applies to the sampling of either
Su9 or NO, gas cylinders and uses Reference Method 7 test
L A
equipment. (See Figure 3.)
NEEDLE
VALVE
GAS
CYL
VACUUM
PUMP
MANOMETER
/ABSORBING*
\ SOLUTION I
\ FLASK '
Figure 3. Flask method.
The procedure is as follows:
1. Place into the flask 25 ml of the Method 7 absorbing su.
solution (HgSO^ + HgOg) forNOx or 15 ml of the Method 6 absorbing
solution (H,,02) for SO^, gas.
2. Prior to connecting the gas cylinder to the sample flask,
purge the line from the gas cylinder with calibration gas.
Record the barometric pressure. Evacuate the flask to a pressure
of less than 3 in. Hg absolute, and leak-check the flask according
to the procedure 1n Reference Method 7.
3. Record the initial flask vacuum, and open the flask
to the cylinder line. Very slowly open the gas cylinder
valve slightly, and monitor the flask pressure. The key to
obtaining a valid sample is to collect the flask sample at a
relatively slow rate (the sample period should be about 30
-------
6
seconds). When the pressure in the flask approaches 0 in. Hg
for SCL gas or -4 in. Hg for NO gas, close the gas cylinder
b A
valve and close the flask to the gas cylinder line. Turn the
flask valve,and close the flask to the gas cylinder line.
Turn the flask valve so that the flask is open to the manometer.
Record the final flask pressure and temperature. Disconnect
the gas cylinder line from the flask. For N0x gas, open the
flask valve to the atmosphere to relieve the flask vacuum to
atmospheric pressure. Close the flask valve to all connections,
and disconnect the flask from the sample train.
4. Complete the analysis of the N0x flask according to
Method 7. For the S0£ gas sample, shake the flask vigorously
for 3 minutes and analyze the entire solution as one aliquot
by the barium-thorin titration procedure described in Reference
Method 6. Calculate the sample concentration from the calibrated
flask volume, the measured flask pressures and temperatures,
and the analyses results.
Criteria for Accepting Results
For any of these procedures, use the results of three
consecutive runs to determine an average. To be acceptable, all
results within the group of three must be within + 10 percent
of the average. If one result out of the three is not within
+ 10 percent of the average, discard that result and replace it
with the result of another run until the acceptability criterion
is met. If two or more results fail to be within + 10
percent of the three-run average, discard all three results and
repeat the test until the above criterion is met.
-------
7
Once the acceptability criterion is met, compare the
average value with the manufacturer1s gas cylinder tag value.
If the average is within + 5 percent of the gas cylinder tag
value, use the tag value as the true gas concentration.
If the average is not within +. 5 percent of the cylinder tag
value, make three additional test runs. Calculate the average
of these results plus the original three results. To be acceptable,
each result must be within + 10 percent of the average. Additional
runs may be made to replace any of the test results. Use the
average of the six acceptable results as the gas cylinder
concentration value.
Recommendati ons
Because the analysis procedure for Reference Method 7
requires a delay of at least 1 day before results are determined,
and the evacuated flask method for SOg gas allows for only one
sample aliquot per flask, it is advisable to collect more than
three flask samples, initially. Nine flask samples should be
sufficient to provide results that meet the acceptability
criteria. The sample results should be used in sequence with
the first three samples collected providing the base average.
This same recommendation can be applied to the other sampling
methods if the tester so desires.
Discussion
Preliminary tests have shown that the pressure in the
sampling system is a critical factor in obtaining accurate
results with the direct pressure and the vented bubbler procedures.
During the method validation tests, the system pressure was
-------
8
maintained below 0.5 in. Hg to avoid positive pressure leaks.
The test results comparing the direct pressure method
results with the NBS values are shown in Table 1. These
results show a consistent 1 to 6 percent positive bias for
single-run results and less than 5 percent positive bias for
the average of any three consecutive runs at the same concentration.
The test results determined using.the vented bubbler pro-
cedure are shown in Table 2. These data show a single-run
result variability from -7 to +8 percent and within + 5 percent
for the average of any three consecutive run results.
The test results found using the evacuated flask method
with the S02 cylinder gas are shown on Table 3. These results
show good consistency and accuracy with the range of single-
run errors between -9 and +5 percent. The maximum three-run
average error was less than + 5 percent.
Reference
1. 40 CFR Part 60, Appendix B - Performance Specifications,
Federal Register, Vol. 40, No. 194, October 6, 1975.
-------
TABLE 1. RESULTS OF CYLINDER VERIFICATION TESTS USING
DIRECT PRESSURE METHOD
NBS
concentration,
Measured
concentration,
Difference,
Percent
error
228
238
+10
+4
228
241
+13
+6
228
235
+7
+3
228
241
+13
+6
891
927
+36
+4 .
CT>
CO
899
+8
+1
891
921
+30
+3
891
935
+44
+5
891
915
+24
+3
891
931
+40
+4
-------
TABLE 2. RESULTS OF CYLINDER VERIFICATION TESTS USING
VENTED BUBBLER METHOD
NBS
concentration,
Measured
concentration,
Difference
Percent
e rror
228
226
-2
-1
228
235
+7
+3
228
232
' +4
+2
228
232
+4 '
+2
228
236
+8
+4
228
247
+19
+8
228
225
-3
-1
228
212
-16
-7
228
230
+2
+1
891
908
+17
+2
891
911
+20
+2
891
935
+44
+5
-------
TABLE 3. RESULTS OF CYLINDER VERIFICATION TESTS USING
EVACUATED FLASK METHOD
NBS
concentration
Measured
concentration
Difference
Percent
error
228
227
-1
0
228
234
+6
+3
228
234
+6
+3
228
238
+10
+4
228
235
+7
+3
228
239
+11
+5
CD
809
-82
-9
891
909
+18
+2
891
894
+3
0
891
901
+10
+1
891
879
-12
-1
891
932
+41
+5
891
872
-19
-2
-------
?/•»'/
A METHOD FOR ANALYZING NO CYLINDER GASES
Specific Ion Electrodi Procedure
Foston Curtis*
Introduction
Appendix B of Part 60 - Standards of Performance for Mew
Stationary Sources - includes specifications for continuous
monitoring equipment. One specification requires the analysis
of nitrogen oxides (N0V) calibration gases using Reference
Method 7.
The analysis of N0X by specific ion electrode has been
found to be acceptable as an alternative to Method 7. The
method is accurate and precise at the 200-and 500- ppm levels.
Laboratory tests of NO calibration gases collected by the
evacuated flask method and analyzed with a nitrate electrode
showed the error of individual measurements to be within + 5
percent.
Sampling Procedure
The evacuated flask method outlined in Reference Method 7
is used to collect the samples. A pressure balance device
should be constructed to eliminate variations due to dif-
ferences in cylinder line pressures (see Figure 1). The sam-
ple is collected by the following procedure:
1. Place into the flask 25 ml of the Method 7 absorbing
* Emission Measurement Branch, Emission Standards and Engi
neering Division, OAQPS, OAWM, EPA, Research Triangle Park,
N. C. 27711, October, 1978.
-------
solution (f^SO^q + f^O^).
2. Record the barometric pressure. Evacuate the flask
to a pros sure of "loss than /("> mm (3 in.) !!<| ahsolut.o. Thou leak-
check the flask according to the procedure in Reference Method 7.
TO
CYLII^'tR GAS
1/4-iri. TEFLON LINE
n &
mmr ^
'PRESSURE
BALANCE • ,
DEVICE t-"'
fc
1/4-in. SWAGELGCK FITTING (TEFLON)
LIMITING ORIFICE
12/5-1n. SOCKET TO 1/4-in.-
DIAMETER GLASS TUBING
. .-Jr. {.'
FLASX^i
FLASK SHIELCU-.
UMPVALVE
PUMP
MANOMETER
EVACUATE
THERMOMETER •
©v™
PURGE •
FIGURE 1. Sampling Train
3. Record the initial flask volume, pressure, and tem-
perature. Adjust the cylinder gas line to a pressure suffi-
cient to cause bubbling in the pressure balance device
«U
-------
3
when sampling. Open the flask to the cylinder line. When thp
pressure in the flask approaches 100 mm (4 in.) Hg vacuum,
close the flask to the cylinder gas line. Turn the flask valv"
so that the flask is open to the manometer. Record the final
flask pressure and temperature. Disconnect the gas cylinder
line from the flask. Open the flask valve to the atmosphere
to relieve the vacuum and provide oxygen for the reaction.
Close the flask valve to all connections and disconnect the
flask from the sample train.
4. Shake the flask for 5 minutes. Then allow it to sit
for a minimum of 16 hours prior to analysis.
5. After the 16-hour absorption period, shake the flask
contents for 2 minutes.
Analysis by Specific Ion Electrode
A nitrate specific electrode with a reference electrode
and a digital pH/mV meter is used 1n determining nitrate in the
absorbing solution. The procedure is as follows:
1. Dry some potassium nitrate (KNO^) in an oven overnight
at 110°C. Prepare a standard nitrate solution containing
2 mg/ml by dissolving exactly 3.261 grams of the dried KNO^ in
1 liter of distilled water. Prepare fresh daily (at the time
that samples are analyzed) a working standard solution
(200 ng/ml) by diluting 10 ml of this solution to 100 ml.
For calibration gases containing up to 500 ppm NO , add 5.0,
10.0, 15.0, and 20.0 ml of the KNOg working solution to a
-------
4
series of four 100-ml volumetric flasks. To each. >dd 25 ml
of Method 7 absorbing solution, 2 ml of 2 M ammon . >i sulfate,
and 1 ml of 1 M boric acid before diluting to volume. Shake
well.
2. Transfer the contents of the sample flask to a
100-ml volumetric flask using a funnel. Rinse the sample
flask twice with 5-ml portions of distilled water, and add the
rinses to the volumetric flask. Pi pet into the flask 2 ml
of 2 M ammonium sulfate (provides a constant background ion
strength of 0.12 M) and 1 ml of 1 M boric acid (preserves the
solution). Dilute to the mark and mix well.
3. Run triplicate analyses of the standard solutions
and the samples, alternating the samples and the standards.
Use a magnetic stirrer during analysis to maintain good mixing.
Calculations
Prepare a least square plot of the standard concentrations
versus millivolt responses. From this curve (or equation),
determine the sample concentrations of N0X in the cylinder;
use the following equation:
Cs
C - 38.80 ^
sc
Where:
C « Concentration of N0X in the calibration gas
cylinder, ppm.
C ¦ Concentration of N0V 1n the sample, pg/ml.
5 X
-------
5
V = Sample volume corrected to standard conditions
sc
as in Reference Method 7, liters.
38.80 = Microliters NOg per microgram NO^ per milliliter
of sample (100 ml sample).
Criteria for Accepting Results
Use the results of three consecutive runs to determine an
average. To be acceptable, all results within the group must
be within + 10 percent of the average. If one result out of
the three is not within + 10 percent of the average, discard
that result and replace it with the result of another run until
the acceptability criterion is met. However, if two or more
results fail to be within + 10 percent of the three-run average,
discard all three results and repeat the test until the above
criterion is met.
Once the acceptability criterion is met, compare the
average value with the manufacturer's gas cylinder tag value.
If the sample average is within + 5 percent of the gas cylin-
der tag value, use the tag value as the true gas concentration.
However, if the average is not within + 5 percent of the
cylinder tag value, make three additional test runs. Calcu-
late the average of these results plus the original three
results. To be acceptable, each result must be within + 10
percent of the average. Additional runs may be made to
replace any of the test results. Use the average of the six
acceptable results as the gas cylinder concentration value.
-------
6
Discussion
The specific ion electrode method allows for ease of
analysis and rapid readout of the nitrate electrode as opposed
to the Method 7 phenoldisulfonic acid analysis which requires
5 to 6 hours before completion. Sampling technique is a
critical factor in obtaining accurate results. The leak check
should be thorough and the sampling rate slow to prevent a
temperature change 1n the sampling flask due to rapidly
changing pressure. Experience has also shown that more con-
sistently accurate results are obtained when working standards
are prepared on the same day as the analysis is performed.
Test results are shown 1n Table 1. All individual sample
values varied from their average group value by less than 5
percent, though some varied from the certified values by as
much as 16 percent. This consistent bias occurred when fresh
working standards were not prepared dally.
1. Federal Register, Vol. 40, No. 194, October 6, 1975.
p. 4650-46271.
2. Driscoll, J. N., A. W. Berger, and J. H. Becker.
Determination of Oxides of Nitrogen 1n Combustion Effluents
with a Nitrate Ion Selective Electrode. Walden Research
Corporation, Cambridge, Mass. Presented at the 64th Annual
Meeting of the Air Pollution Control Association, Atlantic
City, New Jersey. June 1971.
-------
7
Table 1. Summary of Data
Measured Certified
Sample concentration, concentration, % error
sets
1
ppm
ppm
Difference
% error
from mean
515
500
+ 15
3
1.8
514
+ 14
3
1.5
516
+ 16
3
2.0
483
- 17
3
4.5
503
+ 3
1
0.6
526
£00
+ 26
5
2.3
509
+ 9
2
1.0
514
+ 14
3
0
511
+ n
2
0.6
511
' + n
2
0.6
468
500
- 32
6
5.4
423
- 77
15
4.7
441
-:,59
12
0.7
490
500
- 10
2
6.7
534
+ 34
7
1.7
531
+ 31
6
1.1
536
+ 36
3
2.1
524
+ 24
5
0.2
532
+ 32
6
1.3
465
500
- 35
7
2.4
471
- 29
6
3.6
446
- 54
11
1.8
432
- 68
14
4.8
452
- 48
10
0.7
447
- 53
n
0.4
448
- 52
10
0.2
443
- 57
n
1.3
455
- 45
9
1.3
450 •
- 50
10
0.2
-------
8
Table 1. Summary of Data
(Continued)
Measured Certified
Sample
sets
concentration,
ppm
concentration,
ppm
Difference
% error
% error
from mean
7
473
500
I
ro
5
2.8
451
- 49
10
2.0
441
- 59
12
4.1
476
- 24
5
3.5
444
- 56
11
3.5
473
- 27
5
2.8
8
479
500
- 21
4
0.2
474
- 26
5
1.3
477
- 23
5
0.6
479
- 21
4
0.2
479
- 21
4
0.2
474
- 6
1
2.9
9
485
500
- 15
3
2.2
493
- 7
1
0.6
495
- 5
1
0.2
499
- 1
0
0.6
495
- .5
1
0.2
505
+ 6
1
2.0
10
479
500
- 21
4
0.2
484
- 16
3
0.8
478
- 22
4
0.4
478
- 22
4
0.4
482
- 18
4
0.4
11
272
294
- 22
7
4
260
- 34
12
1
267
- 27
9
2
248
- 46
16
5
12
272
294
- 22
7
2
257
- 37
13
4
277
- 17
6
4
-------
9
Table 1. Summary of Data
(Continued)
Measured Certified
Sample concentration, concentration, % error
¦sets ppm ppm Difference % error from mean
260 - 34 12 3
13 282 294 - 12 4 4
275 - 19 6 1
267 - 27 9 1
280 - 14 5 3
250 - 44 15 8
-------
Fiu 2 21979
STRATIFICATION OF S02 EMISSION TESTS AT THE FMC
COAL-FIRED GREEN RIVER SODA-ASH PLANT
by
Peter R. West!in, U.S. EPA, OAQPS
Introduction
During the week of October 16, 1978, an EPA test crew conducted stack
traverse measurements at the FMC Green River, Wyoming Soda Ash Plant. The
purpose was to collect measurements of the relative stratification of sulfur
dioxide emissions in the exhaust stacks of the two scrubber units. A Dyna-
science S0£ monitor and a Beckman O2 monitor were used for the measurements.
The scrubber units were similar in design having a by-pass duct routing some
un-scrubbed boiler exhaust to the stack upstream of the entry of the scrubbed
gas. Emission monitoring data from plant-owned monitors were recorded for
comparison purposes and to establish that loadings remained constant through-
out the tests.
In addition, short-test flask samples were collected from one scrubber
stack for analysis for SOg. Sampling and analysis were performed according
to the outline in the monograph "Determination of Sulfur Dioxide Emissions -
Evacuated Flask Method."
Process Description and Operation
The FMC plant has two identical process boiler and scrubber systems. A
portion of the boiler gas for each system is by-passed around the scrubber
and is directed to the stack. This by-pass gas amount is controlled to some
extent by positioning of dampers in the duct. The by-pass duct enters the
11.5' stack about 40' upstream of the scrubber exhaust duct which is, in
-------
2
turn, about 45' upstream of the sample ports. The boilers are coal-fired
units supplying power for the soda-ash production, and were operated at
constant loads during the stratification tests.
Summary and Discussion of Results
SO2 Stratification
Tables 1 and 2 show the results of the S02 traverses for units 6 and 7,
respectively. Thirteen points, evenly spaced, were used for each traverse
diameter. Included was the central point on each diameter, and S02 and 02
concentrations were measured simultaneously at each point. Figures 1 and 2
show schematics of the stack cross-sections and the measured S02 concentra-
tions for the same units. Isopleths of SO2 concentrations corrected to zero
percent 02 are drawn on these figures.
A stack mean value was calculated for both stacks from the traverse
data using SOg and 02 concentration estimates at sample points defined by
a 10-point traverse in Reference Method 1. The mean SO^ at 0 percent
concentration for Unit 6 was 481 ppm and for Unit 7 was 406 ppm. Stratifica-
tion was determined by comparison of the measured traverse results with the
calculated stack mean value and these results are shown on Table 1 and 2
in terms of percent change from the mean.
These results show severe stratification of SO2 across both stacks.
The percent change for Unit 6 ranges from +27 to -32 percent and for Unit
7 ranges from +23 to -31 percent. The generally accepted value for maximum
percent change for determining gas stratification is +10 percent. These
results indicate that stratification of S02 gas does exist in both stacks.
-------
Further analysis of these data include a determination of path con-
centrations as specified in the revisions to the continuous monitoring
specifications. An average path concentration was calculated for each
port or diameter of the traverses. The average path measurements for Unit
6 were 491 ppm from the southeast port and 483 ppm from the northeast port.
These values are well within +5 percent of the stack average of 481 ppm.
The path measurements for Unit 7 were 393 ppm form the northeast port and
412 ppm from the southwest port. These values, also, are well within +5
percent of the stack average, 406 ppm.
Additionally, 3-point average concentrations were determined using
measurements of SO2 and O2 concentrations at 16.7, 50, and 83.3 percent
of each stack diameter. The average 3-point concentration for the south-
east port of Unit 6 was 491 ppm and for the northeast port was 471 ppm.
Both of these values are within +5 percent of the stack average. The
average 3-point concentrations for Unit 7 were 385 ppm for the northwest
port and 410 ppm for the southwest port. The lower concentration is about
5 percent different than the stack average while the other is about 1 per-
cent different.
These results indicate that stratification of S02 due to incomplete
mixing of by-pass and scrubbed gases can be overcome following the pro-
cedures of the continuous monitoring specifications revisions and such moni-
tor probe locations can obtain accurate representation of the stack emissions.
Analysis of these data show that either path measurements or 3-point measure-
ments will provide average stack concentrations within ;+5 percent of the
actual stack average. This was true for both stacks and represents good
support for the continuous monitoring specification revisions on the location
on monitors and the reference test methods.
1
-------
S02 Short Test Results
Samples were collected from the Unit 6 stack using the short test
procedure. The results shown on Table 3 are biased low by an average 35
percent from the stack monitor measurement average covering the same
period. This bias is due to poor sample handling technique in the transfer
of sample from the flasks to the sample jars. The distilled water rinse
step was inadvertently neglected and, no doubt, caused some portion of the
SC>2 collected to remain in the flasks and miss analysis. Therefore, these
results are inconclusive.
References
1. Determination of Sulfur Dioxide Emissions - Evacuated Flask Method;
monograph available from Chief, Test Support Section (MD 19); Environmental
Protection Agency; Research Triangle Park, N.C. 27711.
2. Performance Specification 2 - Specifications and Test Procedures for
S02 and N0X Continuous Monitoring Systems in Stationary Sources; Draft,
November, 1978.
3. Performance Specification 3 - Specifications and Test Procedures for
C02 and 02 Continuous Monitors in Stationary Sources; Draft, November, 1978.
-------
Table 1: Summary of S02 and 02 Stratification Measurements
in the Exhaust of the FMC Unit #6
(mean S02 concentration at 0% 02 = 481 ppm)
Port
Distance
from wall
(in.)
Uncorrected
so2
(ppm;
*
°o
(%)2
SO2
at 0% 0„
(ppm)
% Cha
from 1
9
282
8.6
479
0
19
268
8.4
448
- 7
29
272
8.2
448
- 7
39
283
8.0
459
- 5
49
296
6.8
439
- 9
59
328
6.5
476
- 1
69
344
6.3
492
+ 2
79
347
6.6
507
+ 5
89
353
6.6
516
+ 7
99
351
6.6
513
+ 7
109
365
6.6
533
+11
119
365
6.6
533
+11
129
369
6.6
539
+12
9
383
6.4
552
+15
19
403
6.4
581
+21
29
419
6.4
604
+26
39
425
6.4
613
+27
49
417
6.4
601
+25
59
373
6.5
541
+12
69
338
6.7
497
+ 3
79
318
6.7
468
- 3
89
287
6.7
422
-12
99
256
6.7
377
-21
109
244
6.8
362
-25
119
226
6.8
335
-30
129
218
7.0
328
-32
Southeast
Northeast
*Note: The Op for samples from the southeast port required significant
adjustment to be consistent with other measurements. This was due
calibration errors on the 02 monitors.
-------
Table 2: Summary of S02 and 02 Stratification Measurements
in the Exhaust of the FMC Unit #7
(mean SO^ concentration at 0% 02 = 406 ppm)
Distance Uncorrected * S02 % Change
from wall S02 02 at 0% 0? from mean
Port (in.) (DPnrt (%1 (ppmr
Northwest 9 171
19 196
29 200
39 204
49 216
59 228
69 242
79 264
89 286
99 305
109 315
119 319
129 317
Southwest 9 293
19 284
29 291
39 282
49 278
59 268
69 268
79 266
89 276
99 274
109 274
119 272
129 268
8.2 281 -31
7.6 308 -24
7.4 310 -24
7.6 321 -21
7.6 339 -17
6.6 358 -12
7.5 377 - 7
7.5 412 + 1
7.5 446 +10
7.5 476 +17
7.5 491 +21
7.5 498 +23
7.5 494 +22
6.8 434 + 7
6.7 418 + 3
6.6 425 + 5
6.8 418 + 3
6.8 412 + 1
6.8 397 - 2
6.8 397 - 2
6.8 394 - 3
6.8 409 + 1
7.0 412 + 1
7.1 415 + 2
7.2 415 + 2
7.2 409 + 1
-------
Is
\ o
hJ G
V H<\ '
*
Figure 1: Schematic of Unit 6 Stack Cross-Section with
SO2 at 0% O2 Isopleths.
1
-------
5 Va'
.r'JIV"
J!«\ I
rsds
Figurje 2: I Schematic of Unit 7 Stack
Ciross-Section with S0„ at
0% 02 ilsopleths.
-7
-------
iyf
Table 3: Summary of Short Test S02 Results from the FMC Unit 6 Stack
Run
S0?
(ppm)
1
167
2
16Q
3
205
4
219
5
166
6
219
7
163
8
144
9
140
10
142
11
139
12
146
dry
Mean 168 Plant Monitor Average = 260 ppm
J*
-------
Citation reprinted from March 7, 1978 issue of NTIS Environmental Pollution
and Control Abstract Summary
Evaluation of EPA Method 5 Probe Deposition and Filter
Media Efficiency. Progress Report, September 1975—
June 1977.
J. C. Elder, M. I. Tillery, and H. J. Ettinger.
Los Alamos Scientific Lab., N.Mex. Aug 77, 16p
LA-6899-PR Price code: PC A02/MF A01
While developing an improved extractive stack sampler,
Environmental Protection Agency Method 5 was evaluated
to quantitate probe deposition and collection efficiency of
several glass fiber filters accepted by the method.
Monodisperse fluorescing dye aerosols from 0.6- to 4.4-
mu m geometric diameter were generated from a vibrating
orifice aerosol generator. Collection efficiencies were mea-
sured for MSA 1106 BH, Reeve-Angel 934AH. and Whatman
GF/A and GF/C glass fiber filters at operating velocities of
5.2 and 10.3 cm/s. Efficiencies of these four filters were
comparable, ranging from 99.6 to 99.8 percent against the
0.6- mu m aerosol and above 99.9 percent for aerosols
larger than 1.0 mu m. Probe deposition of a large (13.4- mu
m mass median diameter) glass bead aerosol was 94 per-
cent. Probe deposition of a 2.0- mu m fly-ash aerosol was
10.5 percent, with approximately half deposited in the noz-
zle. Only 1.5 percent of a 1.2- mu m dye aerosol deposited
in the probe. These measurements emphasize the im-
portance of consistent probe washing procedures, lower
gas velocity in the probe nozzle, fewer bends and diameter
changes, and smoother transition between probe com-
ponents in the design of an improved sampler. (ERA cita-
tion 03:004688)
-------
Taken from August 1977 Issue of STACK SAMPLING NEWS
SPURIOUS ACID MIST VALUES
by
J. E. Knoll and M. R. Midgett
Quality Assurance Branch
Environmental Monitoring and Support Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
We wish to note that, in a recent evaluation study of EPA Reference Method 8, conversion of sulfur dioxide to sulfate
was observed in the isopropyl alcohol solution that is used to separate sulfuric acid mist from SOj. This resulted from
the presence of trace amounts of peroxide in the isopropyl alcohol. The observed conversion, though too small to affect
the sulfur dioxide measurement, produced sufficient HjSO* to cause a significant positive error in the acid mist value.
Testing of samples of reagent grade isopropyl alcohol from a number of well-known supply houses indicated that such
contamination is widespread.
A useful test for the presence of peroxides in isopropyl alcohol is as follows:
Shake 10 ml of isopropyl alcohol with 10 ml of freshly prepared 10% potassium iodide solution. Prepare a blank
by similarly treating 10 ml of distilled water. The appearance of a yellow color indicates the presence of peroxides.
After one minute, read absorbance at 352 nm. If absorbance exceeds 0.1, reject alcohol for use.
Contaminated isopropyl alcohol may conveniently be purified by passage through a column of activated alumina.
u
-------
•?/¦* H{*
CONTINUOUS EMISSION MONITORING (CEM)
Programing and Experiences; EPA, Region VIII, Denver
by John R. Floyd . 0«V • S'S S
I**# cst:
Attatched are some comments on: 1} Pre-specification Test Meeting, '
2) Field Responsibilities of the Agency Observer of a Specification Test,
3) Post-specification Test Activities, and *0 Specification Test Report Review
and Office Report. Region VIII is primarily involved with power plants, there-
fore the comments focus more on GEM for this source category. Below is an out-
line of some of the experiences Region VIII has worked through. One key item
in any viable GEM program is the active support of a strong and progressive En-
forcement Section, both technical and legal.
Region VIII Experiences
I, Program Development
A, EPA Headquarters
B. Regional Growth
G. State Involvement and Implementation
II. The Program
A. Resources Availability
B. Contrast Support (0332)
G. Planning Field Work
D. Travel Required—documenting key items
E. Quality Assurance
F. Field Audits
G. Report Auditing
H. Excess Emission Reporting, Storage, and Use
III. Technical Difficulties
A. The Regulations—*+0 CFR 60, Appendix B
B. The State*-Of-The-Art
C. Location and Relocation— Mft. Young, ND
\)
-------
D. Stratification—FMC, Wyoming^300/£ (303)
E. Accuracy in Units of the Standard (lb/lO^BTU)
F. Quality Assurance—varies with vender
G. Recertifications
H. Resources Demand and Travel Constraints
I. Enforcement and Data Use
IV, New Developments
A. Subpart
B. PSD Psrmits
G. NSP3 Revisions'. Specs 1, Z, 3
D. SIP Revisions
E. GEM Work Group
-------
The Pre-Spec. Test Meeting
By John R. Floyd, USEPA, Region VIII
11/77
Because the continuous emission monitoring (CEM) regulations are lengthy,
somewhat complicated, and often not understood by a source, a pre-spec. test
meeting at the monitoring site with the agency(s), plant engineer, company environ-
mental expert, vendor, and the testing contractor, is a big step in assuring the
most timely completion of the requirements and acceptance of the continuous
monitoring system (CMS) being tested. Prior to this meeting, the agency should
forward to the company, a package of CEM information which would include a summary
of the regulations, a caution on the location of the CMS in the gas stream, an
example report format with data forms, and a suggested work schedule for the week
of the operational test period (OTP).
The plant people can then make sure that the monitor location is acceptable
and begin planning its testing activities to minimize the loss of resources by
all parties Involved. The pre-spec. test meeting at the plant should then be
scheduled about 8 weeks prior to the intended OTP, at a time convenient to the
five parties mentioned earlier.
The meeting might proceed something like the agenda in Table I, below. The
agency person would be the most likely to chair the meeting, in that he should
know more about what needs to be addressed and planned for than anyone else.
Pre-Spec. Test Meeting Agenda
9:00 Introduction of Attendees
9:10 Statement of Purpose Agency
9:30 Description of System Plant or Vendor
10:00 Physical Inspection and Tour of System
Installation and Operation Tour Plant
D-l.l
I1
-------
Pre-Spec. Test Meeting Agenda (continued)
11:00 Review historical data, as available to determine
likelihood of stratification
11:30 Lunch
12:30 Review applicable regulations and reference Agency and Tester
methods to be used (consolidate testing)
1:30 Establish schedule of events, including
input from all parties, for the week of All
the operational test period (OTP)
2:15 Review the report format, including factory Agency
certification and raw data
2:30 Determine date for OTP, report due date, Agency
final compliance date (in case of failures),
and first Quarterly Excess Emission Report
date
3:00 Discussion and Adjourn
Early in the meeting, the agency person should explain the purpose of the
meeting and what needs to be agreed upon during the meeting. After the physical
layout of the CMS is explained, the group should tour the facility, especially
the entire CMS. During the tour, note the location of the monitors and the
orientation to bends in the ductwork or position of stack breeches from the
scrubber(s). Back at the meeting room the subject of stratification of particulate
or SO2 should be addressed. This is more of a problem in scrubber applications,
especially those that have by-pass capability and only scrub enough gas to meet
the SO2 standard. Data are available showing a radical SO2 gradient more than
eight diameters from a disturbance. Particulate can also be stratified after
eight diameters in certain duct and breech designs. If the plant followed your
guidelines in the package sent out earlier, the transmissometer should be installed
"in the plane defined by the bend" (Spec. 1, 4.1.3), regardless of the eight
diameter assumption. The gas monitor(s) should be installed so as to give emission
D-1.2
-------
s#8
values "representative of the total emissions from the affected facility."
(Spec. 2, 4.2) Attached here is an actual case where a source was forced to
reorient and relocate a transmissometer/gas system already located 12.7 diameters
from a disturbance. IS? ^ f ^ | ( ^ . D U
If, after the tour, you find the monitoring system to be located in a repre-
sentative location, the applicable reference methods should then be discussed.
Keep in mind that these are the same procedures used for the performance tests
for compliance with the emission standards. A significant savings of both company
and agency resources is possible by consolidating the required SO2 and N0X per-
formance tests for compliance with the 9 SO2 and 27 N0X monitor performance
specification tests. The agency should point this out and encourage it to be
done when possible.
In any case, the same procedures should be used for both--e.g., if traversing
during the S02 performance test was done and justified, then traversing for SO2
during the specification test is necessary also. The intent is to judge the
monitor by the same reference techniques used to demonstrate compliance.
During the 168-hour OTP, several different tests need to be done. The
instruments need to be tested for accuracy. The zero and calibration drift checks,
and the calibration error tests are to be conducted, as well as various other
smaller checks on the CMS. This typically involves the agency, the plant, the
vendor, and the contractor. Without a detailed plan for the events of the week,
it is extremely difficult to get everything done. An efficiently planned OTP may
look something like Table II, for a complete CMS.
Table II - The OTP
Monday 0800 - start OTP with a 24-hour calibration check and adjustment.
0930 Finish 1st hour of accuracy test
1030 " 2nd
1130 " 3rd
D-1.3
-------
Table II - The OTP (continued)
t«fV
1230
Finish
4th
1330
11
5th
1430
II
6th
1530
It
7th
1630
II
8th
1730
11
9th
Tuesday 0800
calibrations,
from previous
1000
1200
1400
1600
1800
2000
2200
2400
Wed. 0200
0400
0600
0800
0800
0800
1000
1200
1400
1400
1400
Thurs. 0800
0800
1300
Fri. 0800
0800
Sat. 0800
Sun. 0800
Mon. 0800
- record 1st 24-hour drift values, and set system up for 2-hour
automatically if possible. Contractor begins analyzing SO2 samples
day.
Record 1st 2-hour drift values
" 2nd
" 3rd
" 4th
" 5th
" 6th
" 7th
" 8th
" 9th
" 10th
" 11th
Record 2nd 24-hour drift values
" 12th 2-hour drift values
Contractor analyzes NO.. samples from previous day
Record 13th 2-hour drift values
" 14th
" 15th
Begin 1st particulate test if necessary
Run response time and calibration error tests
Record 3rd 24-hour drift values
Begin 2nd particulate test
" 3rd
Record 4th 24-hour drift values
Rerun any accuracy tests as needed
Record 5th 24-hour drift values
" 6th
" 7th
D-1-4
1I
-------
The suggested minimum format for the Spec. Test Report sent to the company
should be reviewed during the meeting. It should be made very clear that certain
entries are a must for an acceptable report. Table III might be used as a table
of contents in an acceptable Spec. Test Report.
Table III - Table of Contents
I. Background and Purpose (include attendees and test date)
II. Executive Summary
A. Plant production and operation
B. Monitoring system description
C. 1. Instrument performance (results of Spec. Test)
2. Reference method results (compare to instrument)
D. Conclusion of acceptability of the system (compared to
allowable Specs.)
III. Plant Operation and Production during OTP
A. During hours of accuracy testing
B. During other instrument specification testing
C. During duration of the 168 hours
IV. Results of Specification Tests on the System
A. Accuracy (relative to reference methods)
B. Drift (2-hour and 24-hour calibration)
C. Response time and calibration error tests
D. Reference methods description and results (include tests
on cal. gases, if used)
E. Factory and field certification of remaining specifications
F. Detailed description and schematic of monitoring system; include
type, model, serial number, drawing of installation location,
zero and span values to be used, installation date, method of
daily calibration checks, etc.
V. The Reference Method Tests
A. Results of SO2, N0X, diluent
B. Method and equipment used
C. Calibration of equipment
D. Quality assurance checks results
VI. Conclusions
A. Level of acceptability of the monitoring system
B. Any problems with data validity I4uri/«g
C. Action scheduled by company, if any part is failed
VII. Appendix (copies of:)
A. Original raw instrument data for:
1. Accuracy tests
2. Drift and cal. error tests
B. Original raw lab and field data for reference methods
C. Original logs of plant operation and production (daily)
Should any questions about either the methods to be used, the schedule, or
the minimum report requirements surface, they should definitely be solved well
D-1.5
-------
before the actual day of the field test. In section D-5 of this manual, you will
see parts of actual reports which may be used as examples.
One of the most important items on the meeting agenda is defining a date
for the seven-day OTP to begin. This should be a date, within the 30 days of
the performance and not more than 210 days after the plant first began production,
at which all parties agree to have their part of the OTP ready. Should any one
of the five parties not be ready on the first day of the OTP, all other parties
are wasting their time. At the same time, it should be pointed out that 60 days
after the start of the OTP, the final report is due. This same date should be
established as the date of final compliance of the source. In any case, the
date of final compliance cannot be extended beyond 270 (180 + 30 + 60) days after
the plant first was started up. It should be pointed out to the plant that should
it operate without an approved CMS beyond the established date of final compliance,
it would be in violation of the NSPS (or SIP) regulations. The date the first
Quarterly Excess Emission Report - EER (see Figure 4, page E-2.29) is due to the
agency (postmarked) the 30th day following the end of the calendar quarter in
which the seven-day OTP was completed.
The purpose of the pre-specification test meeting is threefold: one, to
familiarize the agency with the individual source and its CMS program, as well as
to force the agency to prepare itself for the upcoming spec, test and the applicable
regulations; two, to review, with the source and its tester, the applicable
regulations and required testing methods, including all necessary modifications;
and three, to insure that all problems and questions have been dealt with prior
to the start of the OTP, such that the chances of having to repeat the OTP and
required specification testing would be greatly minimized.
Indeed, a well planned pre-spec. test meeting of all parties involved with such
tests can guarantee timely completion of the testing requirements as well as
expeditious acceptance of the CMS being evaluated.
D-1.6 |/
-------
EMISSION (. STORING REQUIREMENTS
•ON-SITE CERTIFICATION PROCEDURES
P"
1.5 Emission Standard
Full Scale
N0XI SO^i Oj
NOx, SOa
fail |
fai
pass
pass
Maintenance
168 hour
Operational
Period
Calibration
Error
Calibration
Performance
Response
Time
Calculations,
Compare With
Criteria
Instrument
Certification
Sampling
Analyze
Gases
Within 2 Weeks
Reference Method
SO;
Zero,
Calibration
Drift
START-UP
Instruments
Reference Method
Calculations,
Compare With
Criteria
Relative
Accuracy
Documentation
Reference: Fed.Reg. 9/11/74
(MRfr Instruments
-------
CERTIFICATION OF EMISSION MONITORING SYSTEM
SAMPLING FOR COMPLIANCE
CONTRACTOR TRAINING
INSTRUMENT CALIBRATION
OBSERVATION
START-UP SERVICE
NORMAL CHECKOUT
EPA CERTIFICATION PROCEDURE RECHECK t tr
DOCUMENTATION
TRAINING
BEGIN EPA ON-SITE SEQUENCE
3*
-------
,\vl>
(SEZ)
1; iMiii '
Field Activities of an Agency Observer During a
Specification Test of a Continuous Monitoring
System (CMS)
by John R. Floyd \ USEPA, Region VIII
There are certain responsibilities an agency field person would
naturally assume during a Specification Test of a CMS. These include
observing the reference method testing for technique, noting the pro-
duction and operation mode of the plant, and accepting or rejecting
modifications or problems with monitors being tested or the tests being
conducted. This type of observing is carried over from having been an
observer at a traditional performance test for compliance with emission
standards. However, an observer at CMS Specification Test should assume
a much broader role in his responsibilities. A Specification Test is at
least five times more expensive to the source than a normal performance
test; it cannot easily be repeated. Much more documentation of the data
and the testing is necessary in the field to render the CMS and its data
continually more useful, both to the agency and the source.
These added responsibilities can be broken down into five basic
categories: First, the physical equipment (type and serial numbers, etc.)
of the entire CMS should be recorded. The changing of any single component
of a CMS (as defined in specs. 1,2, and 3)., can have a tremendous impact
on the quality of the system and its resulting data. It is reasonable to
make the acceptance, or certification of a CMS conditional on the continued
use, and proper maintenance of the same individual components as were
originally evaluated during the specification Test. In certain cases, if
D-2.1
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
m I11< >N VIII
I860 L iNt.OI N hlKtM
DENVER. COLORADO 80203*
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2
a component, such as the output recorder, is being changed out, it may
be possible to evaluate a few days of data (calibrations and emission
values) produced with the old component (a recorder) just prior to the
change, as compared to similar data from the system using the new
component (possibly a computer), taken just after all the "post-maintenance
bugs" have been worked out of the system. If little or no change in data
or drift character is discovered from such a comparison, recertification
might be waived.
A second item to pay close attention to during a Specification Test
of a CMS is the procedure used to operate w* system, record data, and conduct
the required daily calibration check. Look at the way in which the data is
recorded. Can a 3-hour, or 1-minute (opacity) average be adequately deter-
mined (e.g. if the chart speed is one inch per day, neither 1 minute or even
3-hour averages can be read); One might think twice about accepting this
system. If the data is on mag tape, where is it stored and how is it de-
coded? Is a daily calibration check automatic? What does it look like on the
record? If not automatic, how is such a calibration check done; how long does
it take? If an actual calibration adjustment is necessary, who actually is
responsible for determining the need, doing it, and seeing to it that it is
done promptly? What are the values for the various zero and calibration
values used? Are these reasonable^considering the design of the system and
expected emission values of the plant? Finally, what system is employed for
reducing the data showing excess emissions in units of the standard for
purposes of the Quarterly Excess Emission Report (EER)? Who prepares the
D-2.2
-------
UdV
3
EER and how are the excusable "upsets" documented, by whom, and where are the
records kept? These items may seem unnecessary. However, if you ever intend
to make any use of subsequent data from the system, you will need to know
all this and probably more.
The third major area of concern with a Specification Test and it's
validity is the technique and method used to accomplish the field test
for relative accuracy. Of course, they are the same methods (see page D-1.3)
used to demonstrate compliance with the emission standards. In virtually
all cases, the same procedures, as modified and approved (if such is the
case), should be used both in the performance test and the Specification
Test. The intent is to judge the acceptability of the monitor by the exact
same reference techniques used to demonstrate compliance. If this is not
done, how then is the CMS to be relied on as an indicator of the source's
compliance status? If any modified methods need to be used for the two
tests, these should be discussed and resolved during a pretest meeting, and
definitely not during a field test. Should the tester be using any techniques
not previously approved, or in sloppy manner, it is the responsibility of the
observer to inform the company and the tester, on the spot, that the procedures
(or part of) used cannot be accepted.
Fourth, certain Quality Assurance (QA) procedures should be implemented in
the field by the agency observer of a Spec. Test. QA can prevent the need to
come back and redo portions of the test, as well as lend a significant amount of
credibility to the tests, such that the entire CMS is more useful. Such QA
procedures might include giving the tester blind N0X and S02 samples for analysis
with the field samples. These can be obtained by contacting Region VIII, or the
Quality Assurance Branch in North Carolina. Any mistake in the analysis procedure
D-2.3
-------
-------
The extreme case would be that the plant was down (zero production - no
flow in the stack). An instrument, depending on the design, might appear to have
no drift and be exactly accurate. It is not difficult for an instrument to read
zero on a zero stack when it is calibrated at zero. Without the heat, vibration,
gases, and dust, the instrument would certainly perform well. However, this is
not the environment in which the instrument will be asked to perform in most
plant installations. So with that as an extreme, the agency would do well to
define the minimum limits of production, for purposes of the various parts of the
Spec. Test.
Of course, these limits would depend on the way in which the source was
normally operated. But, in the case of a base-loaded power plant or boiler,
it is normally operated above 80% of its absolute maximum capacity (valves wide
open and 10% over pressure). In that case, such limits as listed in Table I might
be in order.
If the agency does a good job in the field of documenting what is needed,
the office evaluation becomes much simpler and less time consuming. In addition,
if the responsibilities in the field are not properly conducted, the credibility
and utility of the entire CMS will certainly be diminished as a continual indicator
of the compliance status and operation/maintenance procedures of the source.
Table I - Production Limits for the Spec. Test
Test Mode
% of Maximum Capacity (Average)
Accuracy
Drift (2-hour)
Cal. Error and Response
Drift (24-hour)
Entire 168 hours
Minimum to continue testing
80-90
70+
60+
60+
60+
Minimum operating capacity of plant
D-2.5
-------
" / 7 7
The Observers Post-Spec. Test Activities
By John R. Floyd
In addition to the follow up evaluations and quality assurance procedures
discussed in section "E", the agency person evaluating a continuous monitoring
system (CMS) should develop certain office procedures, after the Spec. Test,
in order to complete the file on the CMS Spec. Test and evaluation. Table I
is a sampling of such activities.
Table I: Post-Spec. Test Activities
1. Trip report on what transpired in the field.
2. Office audit of Spec. Test report.
3. Final report on compliance status of source and acceptability of CMS.
4. Letter of agency findings to source.
5. Review Quarterly Excess Emission Reports (EER), see Figure 4, E-2.29.
6. Office and field evaluations of continued source compliance and
condition of CMS.
7. Redo (as needed), compliance test.
8. Redo (as needed), Spec. Tests on monitors.
See section D-4 on report auditing, D-5 for example reports, and "E" for
the use of the EER as a follow-up tool.
D-3.1
-------
"In
Auditing the Specification Test Report and
Reporting Your Final Determination
. By John R. Floyd; USEPA, Region VIII
The review of a Spec. Test report is a fairly sizable task. Having done a
good job while observing the field test will help a great deal. Basically, the
items to be sure and check in a Spec. Test report are listed in Table I.
Table I - Items to Look for in Spec. Test Report
1. All math on field and lab data.
2. Standard sample volumes.
3. Normality calculation.
4. Calculations to ppm.
5. Moisture calculations and correction, as applicable.
6. Orsat math and reasonableness (use nomographs)
7. Calculations to lb./10° BTU.
8. Compare ppm and lb./106 BTU from instrument with reference.
9. The one-hour average values from the instrument record.
10. The drift values from the record.
11. The calculation of drift according to register.
12. The calculation of accuracy by registered method.
13. The response and cal. error tests.
14. The factory (and other misc.) certification checks.
15. Original copied field and lab data for your initials.
16. Crosscheck of key numbers earlier recorded.
17. Problems with methods or results.
18. Other items as included on Table III, p. D-1.4.
By using a preprogrammed calculator or computer, one can complete such an
audit in much less time (by an order of magnitude). On the following pages please
note the program developed by Region VIII to use a TI Prograimiable 59 to assist
in such an audit. The example here 1s for an audit for a particulate test; one
will be developed by Region VIII for S02, NO^, and drift calculations.
Once the actual calculations are checked, a final report of the status of
the CMS being evaluated should be written, usually to the enforcement section of
the agency office. Table II lists the key Items to include in this final office
report.
D-4.1
V
-------
Table II - Final Office Report of CMS Status
1. Results of specification testing - summary.
2. Problems with the Spec. Test.
3. Need to redo portions.
4. Summary of testing history.
5. Scheduled follow-up activities.
6. Date final EER expected.
•7, H eevirtiHettjA ho* s
See Section D-5 for an example of a final office report. The final office
is the last official function in the acceptance of a CMS, except for notifying
the source of its status. The follow-up activities in Section E will insure
that good quality continuous monitoring data are being sent in, as well as flag
the need for redoing portions of the Spec. Test.
D-4.2
-------
zu SEP 19/7
A METHOD FOR THE DETERMINATION OF PARTICULATE AND TOTAL
GASEOUS HYDROCARBON EMISSIONS FROM THE
ASPHALT ROOFING INDUSTRY
1. Principle and Applicability
1.1 Principle. Particulate matter is withdrawn isokinetically
from the source and collected on a glass fiber filter maintained at
a temperature no greater than 50°C (122°F). The particulate mass,
which Includes any material that condenses at or above the filtration
temperature, is determined gravimetrically after removal of uncombined
water. In addition to particulate matter measurement, a simultaneous
determination of total gaseous hydrocarbon emissions is made by passing
a small portion of the filtered gas sample stream through a flame
Ionization detector (FID) hydrocarbon analyzer.
1.2 Applicability. This method 1s applicable for the determina-
tion of particulate and total gaseous hydrocarbon emissions from
asphalt roofing industry process saturators and blowing stills.
2. Apparatus
2.1 Sampling Train. A schematic of the sampling train used in
this method is shown in Figure 1. Complete construction details are
given in APTD-0581 (Citation 2 in Section 7); commercial models of
this train are also available. For changes from APTD-0581 and for
allowable modifications of the train shown in Figure 1, see the
following subsections.
The operating and maintenance procedures for the sampling train
are described in APTD-0576 (Citation 3 in Section 7). Since correct
-------
TEMPERATURE
SENSOR
FLOW THERMOMETER
ZERO & SPAN
CALIBRATION
GAS
temperature
SEBSQR
PROBE
^Tr
FLOW
CONTROL
THERMOMETER AIR-TIGHT VALVE
FLAME
IONIZATION
OETECTOR
THERMOMETER
PITOT TUBE
CHECK
VALVE
STACK
FILTER
VACUUM
GAUGE
THERMOMETERS
VACUUM'O' MAIN
LINE | VALVE
BY-PASS
VALVE
bUPlUGERS
REVERSE
PITOT TUBE
ORY GAS
METER
PRECOLLECTOR
CYCLONE
WITH
GLASSV.'OOL
ICE BATH
AIRTIGHT
PUMP
ORIFICE
~o
PITOT MANOMETER
Figure 1. Particulate and gaseous hydrocarbon sampling train.
-------
usage 1s important in obtaining valid results, all users should
read APTD-0576 and adopt the operating and maintenance procedures
outlined in it, unless otherwise specified herein. Instrument
manufacturer's Instructions should be followed when operating the
flame ionization detector HC measurement system, unless otherwise
specified herein. The sampling train consists of the following
components:
2.1.1 Probe Nozzle. Stainless steel (316) or glass with sharp,
tapered leading edge. The angle of taper shall be <30° and the taper
shall be on the outside to preserve a constant internal diameter. The
probe nozzle shall be of the button-hook or elbow design, unless
otherwise specified by the Administrator. If made of stainless steel,
the nozzle shall be constructed from seamless tubing; other materials
of construction may be used, subject to the approval of the Administrator
A range of nozzle sizes suitable for Isokinetic sampling should
be available, e.g., 0.32 to 1.27 cm (1/fl to 1/2 in.)--or larger if
higher volume sampling trains are used—inside diameter (ID) nozzles
in increments of 0.16 cm (1/16 in.). Each nozzle shall be calibrated
according to the procedures outlined 1n Section 5.
2.1.2 Probe Liner. Borosillcate or quartz glass tubing with a
heating system capable of maintaining a gas temperature at the exit end
during sampling of no greater than 50°C (122°F). Since the actual
temperature at the outlet of the probe is not usually monitored during
sampling, probes constructed according to APTD-0581 and utilizing the
calibration curves of APTD-0576 (or calibrated according to the pro-
cedure outlined in APTD-0576) will be considered acceptable.
-------
Either borosilicate or quartz glass probe liners may be used
for stack temperatures up to about 480°C (900°F); quartz liners
shall be used for temperatures between 480 and 900°C (900 and 1650°F).
Both types of liners may be used at higher temperatures than speci-
fied for short periods of time, subject to the approval of the
Administrator. The softening temperature for borosilicate is 820°C
(1508°F) and for quartz it Is 1500°C (2732°F).
When practical, every effort should be made to use borosilicate
or quartz glass probe liners. Alternatively, metal liners (e.g., 316
stainless steel, IncoToy 8251, or other corrosion resistant metals)
made of seamless tubing may be used, subject to the approval of the
Administrator. Note: At certain stack temperatures, water-cooled
probes may be required to keep the probe exit temperature below 50°C
(122°F.
2.1.3 Pi tot Tube. Type S, as described in Section 2.1 of Method 2,
or other device approved by the Administrator. The pi tot tube shall
be attached to the probe (as shown in Figure 1) to allow constant
monitoring of the stack gas velocity. The impact (high pressure)
opening plane of the pi tot tube shall be even with or above the nozzle
entry plane (see Method 2, Figure 2-6b) during sampling. The Type S
pi tot tube assembly shall have a known coefficient, determined as
outlined 1n Section 4 of Method 2.
2.1.4 Differential Pressure Gauge. Inclined manometer or equiva-
lent device (two), as described 1n Section 2.2 of Method 2. One
Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
-------
manometer shall be used for velocity head (Ap) readings, and
the other, for orifice differential pressure readings.
2.1.5 Particulate and Moisture Cyclone Precollector. To be
used when stack gas moisture concentration is high (above 10 percent)
or when the stack gas oil concentration is high enough to cause oil
to seep through the glass filter mat. The collector shall be
constructed of borosilicate glass. The top section of the cyclone
contains a known weight of glass wool to trap any condensed oil
and/or water. A 125 ml, or larger borosilicate glass Erlenmyer
collecting flask shall be connected to the bottom of the cyclone to
hold any condensate.
2.1.6 Filter Holder. Borosilicate glass, with a glass frit
filter support and a silicone rubber gasket. Other materials of
construction (e.g., stainless steel, Teflon, Viton) may be used,
subject to the approval of the Administrator. The holder design
shall provide a positive seal against leakage from the outside or
around the filter. The filter holder shall be attached immediately
at the outlet of the probe (or cyclone, if used).
2.1.7 Filter Heating System. Any heating system capable of
maintaining a sample gas temperature at the exit end of the filter
holder during sampling of no greater than 50°C (122°F). A temperature
gauge capable of measuring temperature to within 3°C (5.4°F) shall be
installed at the exit end of the filter holder so that the sample gas
temperature can be regulated and monitored during sampling (see
Figure 1). Heating systems other than the one shown in APTD-0581
may be used.
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2.1.8 Total Gaseous Hydrocarbon Measurement System. To remove
and analyze a portion of the filtered sample gas for total gaseous
hydrocarbon emissions (see Figure 1).
2.1.8.1 Heated Sample Line. FEP fluorocarbon tubing, heated
to maintain a gas temperature entering the FID analyzer slightly
above the filter exit temperature. The tubing length should be kept
to a minimum to reduce transport delay time.
2.1.8.2 Flame Ionization Detector Analyzer. Commercially
available system with a gas pump and flow regulation device for
conveying a known amount of sample gas to the detector cell. The
sample stream temperature is 50°C (122°F) or less; therefore, either
ambient or heated cell FID instruments may be used. Operating
Instructions and calibration procedures are given in later sections.
2.1.8.3 Data Recorder. To provide a permanent record of the
output signal, 1n terms of concentration units.
2.1.9 Condenser. The following system shall be used to determine
the stack gas moisture content: Four Impingers connected in series with
1i»&k-free ground glass fittings or any similar leak-free no-icontaminating
fittings. The first, third, and fourth impingers shall be of the
Greenburg-Smlth design, modified by replacing the tip with a 1.3 cm
(1/2 in.) ID glass tube extending to about 1.3 cm (1/2 In.) from the
bottom of the flask. The second impinger shall be of the Greenburg-
Smlth design with the standard tip. The first and second Impingers
shall be empty, and the fourth shall contain a known weight of silica
gel or equivalent desiccant.
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2.1.10 Metering System. Vacuum gauge, leak-free pump,
thermometers capable of measuring temperature to within 3°C (5.4°F),
dry gas meter capable of measuring volume to within 2 percent, and
related equipment, as shown in Figure 1. Other metering systems
capable of maintaining sampling rates within 10 percent of isokinetic
and of determining sample volumes to within 2 percent may be used,
subject to the approval of the Administrator. When the metering system
1s used in conjunction with a pitot tube, the system shall enable
checks of isokinetic rates.
Sampling trains utilizing metering systems designed for higher
flow rates than that described in APTD-0581 or APTD-0576 may be used
provided that the specifications of this method are met.
2.1.11 Barometer. Mercury, aneroid, or other barometer 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
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
sampling point shall 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.
2.1.12 Gas Density Determination Equipment. Temperature sensor
and pressure gauge, as described in Sections 2.3 and 2.4 of Method 2,
and gas analyzer, if necessary, as described 1n Method 3. The
temperature sensor shall, preferably, be permanently attached to the
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pltot tube or sampling probe 1n a fixed configuration, such that
the tip of the sensor extends beyond the leading edge of the probe
sheath and does not touch any metal. Alternatively, the sensor
may be attached just prior to use 1n the field. Note, however,
that 1f the temperature sensor 1s attached In the field, the sensor
must be placed 1n an interference-free arrangement with respect to
the Type S pltot tube openings (see Method 2, Figure 2-7). As second
alternative, provided that a difference of not more than 1 percent 1n
the average velocity measurement Is Introduced, the temperature gauge
need not be attached to the probe or pltot tube. (This alternative
1s subject to the approval of the Administrator.)
2.2 Sample Recovery. The following Items are needed:
2.2.1 Probe-Liner and Probe-Nozzle Brushes. Nylon bristle brushes
with stainless steel wire handles. The probe brush shall have extensions
(at least as long as the probe) of stainless steel, Nylon, Teflon, or
similarly inert material. The brushes shall be properly sized and
shaped to brush out the probe liner and nozzle.
2.2.2 Wash Bottles—Two. Glass wash bottles are recommended.
2.2.3 Glass Sample Storage Containers. Chemically resistant,
boros111cate glass bottles, for 1,1,1 trichloroethane (TCE) washes,
500 ml or 1000 ml. Screw cap liners shall either be rubber-backed
Teflon or shall be constructed so as to be leak-free and resistant
to chemical attack by TCE. (Narrow mouth glass bottles have been
found to be less prone to leakage.)
-------
2.2.4 Petri Dishes. For filter samples and for transporting
tared glass wool plugs to the field. Glass, unless otherwise
specified by the Administrator.
2.2.5 Graduated Cylinder and/or Balance. To measure condensed
water to within 1 ml or 1 g. Graduated cylinders shall have sub-
divisions no greater than 2 ml. Most laboratory balances are capable
of weighing to the nearest 0.5 g or less. Any of these balances is
suitable for use here and 1n Section 2.3.4.
2.2.6 Plastic Storage Containers. A1r-t1ght containers to store
sil1ca gel.
2.2.7 Funnel and Rubber Policeman. To aid in transfer of
silica gel to container; not necessary 1f silica gel is weighed in
the flel.
2.2.8 Funnel. Glass, to aid 1n sample recovery.
2.3 Analysis. For analysis, the following equipment 1s needed:
2.3.1 Glass Weighing Dishes.
2.3.2 Desiccator.
2.3.3 Analytical Balance. To measure to within 0.1 mg.
2.3.4 Balance. To measure to within 0.5 g.
2.3.5 Beakers. Glass, 250 and 500 ml.
2.3.6 Hygrometer. To measure the relative humidity of the
laboratory environment.
2.3.7 Temperature Gauge. To measure the temperature of the
laboratory environment.
2.3.8 Separatory Funnel. 100 ml.
-------
3. Reagents
3.1 Sampling. The reagents used 1n sampling are as follows:
3.1.1 Filters. Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent
penetration) on 0.3-m1cron dloctyl phthalate smoke particles.
The filter efficiency test shall be conducted in accordance with
ASTM standard method D 2986-71. Test data from the supplier's
quality control program are sufficient for this purpose.
3.1.2 Precollector Glass Wool. No. 7220, Pyrex brand, or
equivalent.
3.1.3 Silica Gel. Indicating type, 6 to 16 mesh. If previously
used, dry at 175°C (350°F) for 2 hours. New silica gel may be used
as received. Alternatively, other types of deslccants (equivalent
or better) may be used, subject to the approval of the Administrator.
3.1.4 Crushed Ice.
3.1.5 Stopcock Grease. TCE-lnsoluble, heat-stable grease (1f
available). This 1s not necessary 1f screw-on connectors with Teflon
sleeves, or similar, are used.
3.1.6 Zero Gas. A grade of compressed zero air containing less
than 1 ppm hydrocarbon (as methane).
3.1.7 Calibration Gases. Compressed gas mixtures containing
known concentrations of methane or propane 1n air. Nominal concentra-
tions of 50 percent and 90 percent of the Instrument full scale range
are required. The higher (90 percent of scale) concentration gas
mixture 1s used to set and check the Instrument span and 1s referred
to as the span gas.
-------
3.2 Sample Recovery. 1,1,1 trlchloroethane—reagent grade,
<0.001 percent residue, and stored in glass bottles—1s required.
TCE from metal containers generally has a high residue blank and
should not be used. Sometimes, suppliers transfer TCE to glass
bottles from metal containers; thus, TCE blanks shall be run prior to
field use and only TCE with low blank values (£0.001 percent) shall
be used. In no case shall a blank value of greater than 0.001 percent
of the weight of TCE used be subtracted from the sample weight.
3.3 Analysis. Two reagents are required for the analysis:
3.3.1 TCE. Same as 3.2.
3.3.2 Desiccant. Anhydrous calcium sulfate, indicating type.
Alternatively, other types of deslccants may be used, subject to the
approval of the Administrator.
4. Procedure
4.1 Sampling Train Operation. The complexity of this method 1s
such that, 1n order to obtain reliable results, testers should be
trained and experienced with the test procedures.
4.1.1 Pretest Preparation. All the components shall be maintained
and calibrated according to the procedure described in APTD-0576,
unless otherwise specified herein.
Prepare several probe liners and sampling nozzles for use.
Thoroughly clean each component with soap and water, followed by a
minimum of three TCE rinses. Use probe and nozzle brushes during at
least one of the TCE rinses (refer to Section 4.2 for rinsing
techniques). Cap or seal the open ends of the probe liners and
nozzles to prevent contamination during shipping.
-------
Weigh several 200 to 300 g portions of silica gel In air-tight
containers o the nearest 0.5 g. Record the total weight of the
silica gel plus container, on each container. As an alternative,
the silica gel need not be prewelghed, but may be weighed directly
In Its Implnger just prior to train assembly.
Check filters visually against light for irregularities and
flaws or pinhole leaks. Label filters of the proper diameter on the
back side near the edge using numbering machine ink. As an alterna-
tive, label the shipping containers (glass petrl dishes) and keep
the filters 1n these containers at all times except during sampling
and weighing.
Desiccate the filters at 20 + 5.6°C (68 + 10°F) and ambient
pressure for at least 24 hours and weigh at intervals of at least
6 hours to a constant weight, i.e., <0.5 mg change from previous
weighing; record results to the nearest 0.1 mg. During each weighing
the filter must not be exposed to the laboratory atmosphere for a
period greater than 2 minutes and a relative humidity above 50 percent.
Alternatively (unless otherwise specified by the Administrator), the
filters may be oven dried at 105°C (220°F) for 2 to 3 hours, desiccated
for 2 hours, and weighed. Procedures other than those described, which
account for relative humidity effects, may be used, subject to the
approval of the Administrator.
Prepare cyclone precollector systems for use, as follows: Desiccate
or oven-dry several plugs of glass wool and weigh these to a constant
weight (use techniques similar to those described above for glass fiber
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filters). Place each tared glass wool plug 1n a labeled petrl
dish. Next, thoroughly clean equal numbers of glass cyclones and
125 ml Erlenmeyer flasks, using soap and water, followed by several
TCE rinses. Pair each cylcone with a flask and identify (mark or
label) each piece of glassware. Determine the tare weight of each
glass cyclone, to the nearest 0.1 mg. Seal the open ends of each
flask and cyclone to prevent contamination during transport.
4.1.2 Preliminary Determinations. Select the sampling site and
the minimum number of sampling points according to Method 1 or as
specified by the Administrator. Determine the stack pressure,
temperature, and the range of velocity heads using Method 2; 1t 1s
recommended that a leak-check of the pltot lines (see Method 2,
Section 3.1) be performed. Determine the moisture content using
Approximation Method 4 or Its alternatives for the purpose of making
Isokinetic sampling rate settings. Note: A portion of flow will go
to the FID analyzer. If this flow exceeds 1.0 liters/min, a nomograph
correction will be needed to properly set Isokinetic sampling rates
(see Section 6.3.1). Determine the stack gas dry molecular weight,
as described 1n Method 2, Section 3.6; 1f Integrated Method 3 sampling
1s used for molecular weight determination, the integrated bag sample
shall be taken simultaneously with, and for the same total length of
time as, the sample run.
Select a nozzle size based on the range of velocity heads, such
that 1t is not necessary to change the nozzle size 1n order to maintain
-------
Isokinetic sampling rates. During the run, do not change the
nozzle size. Ensure that the proper differential pressure gauge
1s chosen for the range of velocity heads encountered (see Section
2.2 of Method 2).
Select a suitable liner and probe length such that all traverse
points can be sampled. For large stacks, consider sampling from
opposite sides of the stack to reduce the length of probes.
Select a total sampling time greater than or equal to the minimum
total sampling time specified 1n the test procedures for the Industry
such that (1) the sampling time per point 1s not less than 2 minutes
(or some greater time interval as specified by the Administrator), and
(2) the sample volume taken (corrected to standard conditions) will
exceed the required minimum total gas sample volume. The latter 1s
based on an approximate average sampling rate.
It 1s recommended that the number of minutes sampled at each
point be an Integer or an Integer plus one-half minute, 1n order to
avoid timekeeping errors.
In some circumstances, e.g., batch cycles, 1t 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.
. 4.1.3 Preparation of Collection Train. During preparation and
assembly of the sampling train, keep all openings where contamination
can occur covered until just prior to assembly or until sampling is
about to begin.
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Place 100 ml of water 1n each of the first two implngers,
leave the third 1mp1nger empty, and transfer approximately 200 to
300 g of prewelghed silica gel from Its container to the fourth
1mp1nger. More silica gel may be used, but care should be taken to
ensure that It 1s not entrained and carried out from the 1mp1nger
during sampling. Place the container In a clean place for later use
1n the sample recovery. Alternatively, the weight of the silica gel
plus 1mp1nger may be determined to the nearest 0.5 g and recorded.
Using a tweezer or clean disposable surgical gloves, place a
labeled (Identified) and weighed filter In the filter holder. Be
sure that the filter is properly centered and the gasket properly
placed so as to prevent the sample gas stream from circumventing the
filter. Check the filter for tears after assembly is completed.
If a cyclone precollector 1s to be used, prepare 1t for use by
placing a tared glass wool plug in one of the tared cyclones and then
connecting the cyclone to a 125 ml Erlenmeyer flask (see Section 4.1.1).
When glass probe liners are used, install the selected nozzle
using a V1ton A 0-r1ng when stack temperatures are less than 260°C
(500°F) and an asbestos string gasket when temperatures are higher.
See APTD-0576 for details. Other connecting systems using either
316 stainless steel or Teflon ferrules may be used. When metal liners
are used, install the nozzle as above or by a leak-free direct
mechanical connection. Mark the probe with heat resistant tape or
by some other method to denote the proper distance into the stack or
duct for each sampling point.
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Set up the train as 1n Figure 1, using no silicone grease on
ground glass joints, unless the grease 1s Insoluble 1n TCE.
Place crushed 1ce around the 1mp1ngers.
4.1.4 Leak-Check Procedures.
4.1.4.1 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 shall be used.
After the sampling train has been assembled, turn on and set the
filter and probe heating systems at the desired operating temperatures.
Allow time for the temperatures to stabilize. If a V1ton A 0-r1ng or
other leak-free connection 1s used 1n assembling the probe nozzle to
the probe Hner, leak-check the train at the sampling site by plugging
the nozzle and pulling a 380 mm Hg (15 1n. Hg) vacuum.
Note: A lower vacuum may be used, provided that 1t Is not exceeded
during the test.
If an asbestos string 1s used, 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 holder (cyclone, 1f applicable) and
pulling a 380 mm Hg (15 1n. Hg) vacuum (see Note Immediately above).
Then connect the probe to the train and leak-check at about 25 mm Hg
(1 1n. Hg) vacuum; alternatively, the probe may be leak-checked with
the rest of the sampling train, 1n one step, at 380 mm Hg (15 In. Hg)
vacuum.
Leakage rates In excess of 4 percent of the average sampling rate
or 0.00057 m /mln (0.02 cfm), whichever Is less, are unacceptable.
-------
The gaseous hydrocarbon system may be shut off for the leak check.
However, all fittings on the analyzer system should be checked to
Insure they are properly tightened.
The following leak-check instructions for the sampling train
described in APTD-0576 and APTD-0581 may be helpful. Start the pump
with bypass valve fully open and coarse adjust valve completely closed.
Partially open the coarse adjust valve and slowly close the bypass
valve until the desired vacuum 1s reached. Do not reverse direction
of bypass valve; this will cause water 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.
When the leak-check 1s completed, first slowly remove the plug
from the inlet to the probe, filter holder, or cyclone (if applicable)
and Immediately turn off the vacuum pump. This prevents the water in
the Implngers from being forced backward and silica gel from being
entrained backward Into the third Impinger.
4.1.4.2 Leak-Checks During Sample Run. If, during the sampling
run, a component (e.g., filter assembly or impinger) change becomes
necessary, a leak-check shall be conducted immediately before the
change is made. The leak-check shall be done according to the
procedure outlined in Section 4,1.4.1 above, except that it shall be
done at a vacuum equal to or greater than the maximum value recorded
up to that point 1n the test. If the leakage rate is found to be no
greater than 0.00057 m /mln (0.02 cfm) or 4 percent 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; 1f, however, a higher leakage rate 1s obtained, the tester
shall either record the leakage rate and plan to correct the sample
volume as shown 1n Section 6.2.2 of this method, or shall void the
sampling run.
Immediately after component changes, leak-checks are optional; if
such leak-checks are done, the procedure outlined in Section 4.1.4.1
above shall be used.
4.1.4.3 Post-test Leak-check. A leak-check is mandatory at the
conclusion of each sampling run. The leak-check shall be done 1n
accordance with the procedures outlined In Section 4.1.4.1, except
that 1t shall be conducted at a vacuum equal to or greater than the
maximum value reached during the sampling run. If the leakage rate
1s found to be no greater than 0.00057 m /min (0.02 cfm) or 4 percent
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 1s obtained, the
tester shall either record the leakage rate and correct the sample
volume as shown in Section 6.2.2 of this method, or shall void the
sampling run.
4.1.5 Particulate Train Operation. During the sampling run,
maintain an isokinetic sampling rate (within 10 percent of true
Isokinetic unless otherwise specified by the Administrator) and a gas
temperature exiting the filter of no greater than 50°C (122°F).
-------
For each run, record the data required on a data sheet such as the
one shown in Figure 2. Be sure to record the initial dry gas meter
reading. Record the dry gas meter readings at the beginning and end of
each samDling time increment, when changes in flow rates are made,
before and after each leak check, and when sampling is halted. Take
other readings required by Figure 2 at least once at each sample point
during each time increment and additional readings when significant
changes (20 percent variation in velocity head readings) necessitate
additional adjustments in flow rate. Level and zero the manometer.
Because the manometer level and zero may drift due to vibrations and
temperature changes, make periodic checks during the traverse.
Clean the portholes prior to the test run to minimize the chance of
sampling deposited material. Allow time for the hydrocarbon analyzer
operation to stabilize and for the heated hydrocarbon sample line to
reach the required temperature. To begin sampling, remove the nozzle
cap, verify that the filter and probe heating systems are up to tempera-
ture, and that the pitot tube and probe are properly positioned. Position
the nozzle at the first traverse point with the tip pointing directly
into the gas stream. Immediately start the pump and adjust the flow to
isokinetic conditions. Nomographs are available, which aid in the rapid
adjustment of the isokinetic sampling rate without excessive computa-
tions. These nomographs are designed for use when the Type S pitot tube
coefficient is 0.85 +0.02, and the stack gas equivalent density
(dry molecular weight) Is equal to 29 + 4, A0TD-0576 details the
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procedure for using the nomographs. If Cp and are outside the above
stated ranges, do not use the nomographs unless appropriate steps (see
Citation 7 in Section 7) are taken to compensate for the deviations.
After starting and adjusting the flow of the sampler pump, start
the flow of sample gas through the hydrocarbon analyzer and allow a
constant, regulated amount of gas to go to the hydrocarbon analyzer.
The flow rate of the hydrocarbon system should be preset to a value no
greater than 1.0 liter per minute. If the HC system flowrate exceeds
1.0 liter/min, a nomograph correction will be necessary to establish
accurate isokinetic sampling rate settings (see Section 6.3.1).
When the stack is under significant negative pressure (height of
impinger stem), take care to close the coarse adjust valve before
inserting the probe into the stack to prevent water from baking into the
filter holder. If necessary, the pump may be turned on with the coarse
adjust valve closed.
When the probe is in position, block off the openings around the
probe and porthole to prevent unrepresebtative dilution of the gas
stream.
Traverse the stack cross-section, as required by Method 1 or as
specified by the Administrator, being careful not to bump the probe
nozzle Into the stack walls when sampling near the walls or when r
removing or Inserting the probe through the portholes; this minimizes
the chance of extracting deposited material.
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During the test run, make periodic adjustments to keep the
temperature of the sample gas exiting the filter below 50°C (122°F); add
more 1ce and, 1f necessary, salt to maintain a temperature of less than
20°C (68°F) at the impinger/slUca gel outlet. Also, periodically check
the level and zero of the manometer. Record the hydrocarbon concen-
tration for each traverse point on both the chart record and on the data
form.
If, in the midst of a sample run, the pressure drop across the
filter becomes too high, making isokinetic sampling difficult to
maintain, replace the filter. It 1s recommended that another complete
filter assembly be used rather than attempting to change the filter
itself. When a precollector is used, if a yellow-brown color forms on
the filter or 1f condensed moisture begins to fill the precollector,
both the precollector and the filter shall be replaced. Before a new
precollector and/or filter assembly is Installed, conduct a leak-check
(see Section 4.1.4.2). The total particulate weight shall include the
summation of all precollector and filter assembly catches.
A single train shall be used for the entire sample run, except in
cases where simultaneous sampling 1s required in two or more separate
ducts or at two or more different locations within the same duct, or, in
cases where equipment failure necessitates a change of trains. In all
other situations, the use of two or more trains will be subject to the
approval of the Administrator.
Note that when two or more trains are used, separate analyses of
the particulate catches from each train shall be performed, unless
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Identical nozzle sizes were used on all trains, 1n which case, the
catches from the Individual trains may be combined and one analysis
performed. Consult with the Administrator for details concerning the
calculation of results when two or more trains are used.
At the end of the sample run, shut off the flow of gas to the
hydrocarbon sample system, turn off the coarse adjust valve, remove the
probe and nozzle from 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, 1n order to
validate the velocity head data.
4.1.6 Calculation of Percent Isokinetic. Calculate percent
isokinetic (see Section 6.2.10) to determine whether the run was valid
or another test run should be made. If there was difficulty in
maintaining isokinetic rates due to source conditions, consult with the
Administrator for possible variance on the Isokinetic rates.
4.2 Hydrocarbon Analyzer Operation.
4.2.1 Install the hydrocarbon analyzer system as close as possible
to the probe and filter apparatus.
Heat the fluorocarbon sample line to a temperature above the filter
temperature in order to prevent condensation of hydrocarbons. Note:
Due to the design of most FID analyzers, 1t will be necessary to
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protect the instrument from the ambient environment (rain, dust, extreme
heat or cold, etc.). Check for stable electrical power; voltage
fluctuations can cause instrument drift in some analyzers. Calibrate the
analyzer using a span concentration, zero air and one other upscale
concentration of methane in air to check the linearity of the system;
refer to Section 5.2 for details.
After particulate sampling has begun at the first traverse point,
the gaseous hydrocarbon sample pump shall be started and the flow
regulated so that the analyzer functions properly. The average
hydrocarbon analyzer reading shall be recorded at each traverse point.
A strip chart or other data recorder can also be used to monitor the
analyzer unit.
At the conclusion of the test, shut off the hydrocarbon system
before stopping the particulate sampling train pump. The hydrocarbon
analyzer shall be recalibrated after the test so that zero and span
drift can be determined.
4.2.2 Zero Drift. "Zero drift" is the change in analyzer output
during a sample run, when the input to the measurement system is a zero
grade of air (zero gas). The maximum allowable zero drift for the
analyzers used in this method is +2 percent of the specified instrument
span. The zero drift calculation is made for each test run; this is
done by taking the difference of the zero gas concentration values
measured at the start and finish of the test. The zero drift is
recorded (as a percentage of the instrument span) on a form similar to
Figure 3.
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4.2.3 Span Drift. "Span drift" is the change in the analyzer
output during a sample run, when the input to the measurement system is
span gas. The maximum allowable span drift for the analyzers used 1n
this method is +2 percent of the specified Instrument span. The span
drift calculation is made for each test run; this is done by taking the
difference between the span gas concentration values measured at the
beginning and end of the test. Span drift is recorded (as a percentage
of instrument span) on a form similar to Figure 3. Span drift must be
corrected for any zero drift that occurred during the test period (see
Figure 3).
4.2.4 Analyzer Response Time. When a change in pollutant
concentration occurs at the inlet of the hydrocarbon analyzer, the
change is not immediately registered by the analyzer; "response time" is
defined as the amount of time that 1t takes for the analyzer to register
a concentration value within 5 percent of the new inlet concentration.
The maximum response time for the analyzers used In this method is three
minutes.
To determine response time, first introduce zero gas into the
system until all readings are stable; then, Introduce span gas Into the
system. The amount of time that It takes for the analyzer to register
95 percent of the final span gas concentration Is the upscale response
time. Next, reintroduce zero gas Into the system; the length of time
that it takes for the analyzer output to come within 5 percent of the
final reading is the downscale response time. The upscale and down-
scale response times shall each be measured three times. The readings
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Site Location
Operator
Dote:
Test Mo.:
Analyzer: Type
S/N
Initial
Calibration
Final
Calibration
Difference
Initial-Final
%
ppm or %
ppm or %
ppm or %
of Span
Zero Gas
i
1
1
Hich Calibration
Gas (Span Gas)
i
«
i
i
i
i
• % of Span
Absolute Value of Difference
x 100
Instrument Span
~Corrected for zero drift, i.e., if zero drift over test period is +2 ppm
then 2 com shall be subtracted from the difference between the initial
and final readings.
Figure 3. Zero and Span Drift Data.
V
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shall be averaged, and the average upscale or downscale response
time, whichever 1s preater, shall be reported as the "response
time" for the analyzer. Pesponse time data are recorded on a form
similar to Figure 4. P response time test shall be conducted prior
to the Initial field use of the analyzer, and shall be repeated 1f
changes are made 1n the system.
4.3 Sample Recovery. Proper cleanup procedure begins as soon
as the probe 1s removed from the stack at the end of the sampling
period. Allow the probe to cool.
When the probe can he safely handled, wipe off all external oil
and particulate matter near the tip of the probe nozzle and place a
cap over 1t. Do not cap off the probe tip tightly v/hile the sampling
train is cooling down as this would create a vacuum 1n the filter
holder, thus drawing water from the 1mp1wjers Into the filter holder.
Before moving the sample train to the cleanup site, remove the
probe from the sample train, and cap the open outlet of the probe. Be
careful not to lose any condensate that might be present. Remove the
umbilical cord from the last Implnger and cap the Implnger. If a
flexible line 1s used between the first Implnger and the filter holder,
disconnect the Hne at the filter holder and let any condensed water
or liquid drain Into the implngers, Cap off the filter holder outlet
and Implnger Inlet. Either oround-alass stoppers on non reactive caps
nay he used to close these openings.
Transfer the probe and filter-Implnger assembly to the cleanup
area. This area should he clean and protected from the wind so that
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pyrr
Date of Test
Analyzer Type
S/N
SD?.n Gas Concentration
. PPtf
Analvzer Soan Settinq
ppm
1
seconds
Unseale. 2
seconds
3
seconds
Average upscale.response
seconds
1
SReonas
Downscale 2
seconds
3
seconds
Average downscale response
seconds
System response time - slower average time
» seconds.
Figure 4. Response time.
V
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the chances of contaminating or losing the sample will he minimized.
Save a portion of the TCE used for cleanup as a blank. Take
200 ml of this TCE directly from the wash bottle being using and
place it in a class sample container labeled "TCE blank."
Inspect the train prior to and during disassembly and note any
abnormal conditions. Treat the samples as follows:
Container Mo. 1. Carefully remove the filter from the filter
holder and place it in its identified petri dish container. Use a
pair of tweezers and/or clean disposable surgical gloves to handle
the filter. If it is necessary to fold the filter, do so such that
the film of oil is Inside the fold. Carefully transfer to the petri
dish any particulate matter and/or filter fibers which adhere to
the filter holder casket, by using a dry Nylon bristle brush and/or
a sharp-edged blade. Seal the container.
Container No. 2. Remove the Erlenmeyer flask from the cyclone.
I'slnp glass or other nonreactlve caps, seal the ends of the cyclone
and store for shipment to the laboratory. Do not remove the glass
wool plug from the cyclone.
Container Mo. 3. Taking care to see that material on the
outside of the probe or other exterior surfaces does not get Into the
sample, Quantitatively recover particulate matter or any condensate
from the probe nozzle, probe fitting, probe Uner, cyclone collector
flask, and front half of the filter holder by washing these components
with TCE and placing the wash 1n a glass container. Carefully measure
the total amount of TCE used 1n the rinses. Perform the TCE rinses
as follows:
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Carefully remove the probe nozzle and clean the Inside surface
by rinsing with TCE from a wash bottle and brushing with a Nylon
bristle brush. Prush until the TCE rinse shows no visible particles
or discoloration, after which, make a final rinse of the inside
surface with TCE.
Brush and rinse the inside parts of the Swagelok fitting with
TCE 1n a similar way until no visible particles remain.
Rinse the probe Uner with TCE by tilting and rotating the probe
while squirting TCE into its upper end so that all inside surfaces will
be wetted, let the TCE drain from the lower end into the sample
container. A plass funnel nay be used to aid in transferring liquid
washes to the container. Follow the TCE rinsp with a probe brush. Hold
the probe in an inclined position, squirt TCE into the upper end as the
probe brush is beino pushed with a twisting action through the probe;
hold the sample container underneath the lower end of the probe, and
catch any TCE and particulate matter which 1s brushed from t.he probe.
Run the brush through the probe three times or more until no visible
particulate matter is carried out or until no discoloration is
observed in the TCE. With stainless steel or other metal probes, run
the brush through 1n the above prescribed manner at least six times,
since r>etal probes have small crevices 1n v>h1 ch particulate matter can
be entrapped. Rinse the brush with TCE and quantitatively collect
these washings in the sample container. After the brushing, make a
final TCE rinse of the probe as described abovp.
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It 1s recommended that two people be used to clean the probe
to minimize sample losses. Petween sampling runs, keep brushes
clean and protected from contamination.
Clean the Inside of the cyclone collection flask and the front
half of the filter holder by rubbing the surfaces with a nylon
bristle brush and rlnsinp with TCE. Rinse each surface three times
or more, 1f necessary, to remove visible particulate. Make a final
rinse of the brush and filter holder. After all TCE washlnps and
particulate matter have been collected in the sample container,
tighten the lid on the sample container so that TCE will not leak
out when it is shipped to the laboratory. Mark the height of the
fluid level to determine whether or not leakage occurred durlnp
transport. Label the container to clearly Identify Its contents.
Container Ho. 4. Note the color of the indicating silica pel
to determine if 1t has been completely spent and make a notation of
Its condition. Transfer the silica pel from the fourth Impinger to
Its original container and seal. A funnel may make 1t easier to pour
the silica pel without spilling. A rubber policeman may be used as
an aid In removing the silica pel from the Impinger. It Is not
necessary to remove the small amount of dust particles that may adhere
to the Impinger wall and are difficult to remove. Since the gain 1n
weight 1s to be used for moisture calculations, do not use any water
or other Houids to transfer the silica pel. If a balance Is
available In the field, follow the procedure for Container No. 4 In
Section 4.4.
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Plant ;
Date __
Run Mn-
Filter No.__
Amount liquid lost during transport
TCE blank volume, ml _i !
TCE wash volume, ml
TCE blank concentration, mg/inQ (equation 4),
TCE wash blank, my (equation 5)
CONTAINER
NUMBER
WEIGHT OF PARTICULATE COLLECTED.,
mg
FINAL WEIGHT
TARE WEIGHT
WEIGHT GAIN
1
2
3
Total
Less TCE blank
Weight of particulate matter
«
VOLUME OF LIQUID'
WATER COLLECTED
IMPINGER
VOLUME,
ml.
SILICA GEL
WEIGHT.
0
FINAL
1
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
0* ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER ClQ/mt).
INCREASE, g , VQLmE WATER, ml
1 fl/ml
Figure 5. Analytical data.
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evaporated. Weigh the cyclone plus contents (glass wool plug and
oil). Determine the weight of the oil by subtracting out the
combined tare weight of the cyclone plus class wool. Transfer
the glass wool and cyclone catch Into a tared weighing dish; use
TCE to aid 1n the transfer process. Desiccate the cyclone for
24 hours and rewelgh the cyclone. If the final weight of the clean
cyclone 1s within 10 r*g of Its Initial tare weight, the calculated
oil weight will be considered valid. If the weight difference is
greater, extract the oil from the glass wool (use treasured amount of
TCE) and add this oil solution to Container 3. Note: To prevent
error, the glass wool fibers should be kept from contacting the oil
solution.
Container No. 3. Note the level of liquid in the container and
confirm on analysis sheet whether or not leakage occurred during
transport. (Do this before adding either the rinse from either
Container No. 1 or the TCE-oll mixture from the glass wool extraction
to Container No. 3.) If noticeable leakage has occurred, either void
the sample, or take steps, subject to the approval of the Administrator,
to correct the final results. Measure the liquid 1n t.hls container
either volumetrlcally to +1 ml or gravlmetrically to +0.5 0. Check
to see 1f there is any appreciable quantity of condensed water present
in the TCE rinse (look for a boundary layer or phase separation). If
the volume of condensed water appears larger than 5 ml it will be
necessary to separate the oil-TCE fraction from the water fraction.
This should be done with a separatory funnel. Measure the volume of
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the water phase, to the nearest pi; adjust the stack oas moisture
content, 1f necessary (see Sections 6.2.3 and P.2.4). Next, extract
the water phase with several 25 ml portions of TCF until, by visual
observation, the TCE does not remove any additional organic material.
The remaining water fraction shall be evaporated to dryness at 93°C
(200°F), desiccated for 24 hours and weighed to the nearest 0.1 mg.
Treat the total TCE fraction (including TCE from filter container
rinse, H^O pbase extractions and qlass wool extraction, if applicable)
as follows: Transfer the TCE and oil to a tared beaker, and evaporate
at ambient temperature and pressure. The term "constant weight," as
it is normally understood, 1s not appropriate for liquid oil samples.
The evaporation of TCE from the solution may take several days. The
sample should not be desiccated until the solution has reached an
apparent constant volume or until the odor of TCE is not detected.
Therefore, when 1t appears that the TCE has evaporated, desiccate the
sample and weioh it at 24-hour intervals to obtain a "constant weight"
(as defined for Container Mo. 1 above). The "total weight" for
Container No. 3 is the sum of the evaporated particulate weight of
the TCE-oil and water phase fractions. Report the results to the
nearest 0.1 mg.
Container No. 4. This step may be conducted 1n the field. Weigh
the spent silica pel (or silica ael plus 1mp1nger) to the nearest 0.5 g
using a balance.
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"TCE Blank" Container. Measure TCE in this container either
volumetrically or oravimetrlcally. Transfer the TCE to a tared
250 ml heaker 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 mg.
5. Calibration
Maintain a laboratory log of all calibrations.
5.1 Sampling Train Calibration. The components of the sampling
train shall be calibrated according to the following sections of
Reference Method 5: Section 5.1 (probe nozzle); Section 5.2 (pltot
tube); Section 5.3 (metering system); Section 5.4 (probe heater);
Section 5.5 (temperature oauges); Section 5.7 (barometer). Note that
the leak check of the metering system, described in Section 5.6 of
Method 5, also applies to this method.
5.2 Calibration of Gaseous Hydrocarbon System. Prior to the
test run, the hydrocarbon measurement system shall be calibrated
according to the procedures described 1n this section. The manu-
facturer's operation and calibration instructions are also to be
followed as required.
5.2.1 The measurement system shall be put into operation and
allowed to warm up until stable conditions are achieved. Then, 1n
succession, zero qas, span nas, and a mid-scale gas mixture
corresponding to approximately 50 percent of span shall be introduced
Into the analyzer. The analyzer response to each gas shall be
-------
measured, and the values shall be used to establish a calibration
curve or to verify the manufacturer's calibration curve. The data
obtained 1n these procedures shall be recorded on a form similar to
Figure 6. If the manufacturer's calibration curve, or the expected
response curve (I.e., an accuracy of better than 2 percent of full
scale at the mid-scale point) cannot be attained, the calibration
shall be considered Invalid and corrective measures shall be taken.
The calibration procedure shall be repeated using only zero gas and
span gas at the conclusion of the test, for the purpose of calculating
zero and span drift.
5.2.2 Hydrocarbon (HC) calibration gas mixture concentrations
shall be certified by the gas manufacturer to be within +2 percent
of the Indicated concentration.
6. Calculations
Carry out calculations, retaining at least one extra decimal
figure beyond that of the acquired data. Round off figures after
final calculation.
6.1 Nomenclature
2 2
A„ ¦ Cross sectional area of nozzle, m (ft ).
n
2 2
A « Cross sectional area of stack, m (ft ).
d
B = Water vapor 1n the gas stream, proportion by volume.
W 5
Bwt = Water vapor in the sample gas stream, proportion by volume.
c$ * Concentration of particulate matter 1n stack gas, dry
basis, corrected to standard conditions, g/dscm (g/dscf).
C^ a TCE blank residue concentration, mg/g.
-------
Date
Analyzer Type
S/N
High Range Gas Cone.
% Full Scale
Mid Ranee Gas Cone.
% Full Scale
Low Range Gas Cone.
% Full Scale
Zero Gas
% Full Scale
Figure 6. Calibration data.
-------
I - Percent of isokinetic sampling.
L e Maximum acceptable leakage rate for either a pretest
A
leak check or for a leak check following a component
change; equal to 0.00057 m /m1n (0.02 cfm) or 4 percent
of the average sampling rate, whichever 1s less.
Lj B Individual leakage rate observed during the leak check
conducted prior to the "1^" component change (1 = 1,2,
3 . . . n), m /m1n (cfm).
tp = Leakage rate observed during the post-test leak check,
m3/m1n (cfm).
Mn = Total amount of particulate matter collected, mg.
M ¦ Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-mole),
W
¦ Mass of residue of TCE after evaporation, mg.
Pbar * Barometric pressure at the sampling site, mm Hg (1n. Hg).
pmr = Pollutant mass rate, g/hr (Ib/hr).
ppmy « Parts per million by volume for hydrocarbons corrected to
methane equivalents.
Ps * Absolute stack gas pressure, mm Hg (1n. Hg).
Pstcj = Standard absolute pressure, 760 mm Hg (29.92 1n. Hg).
R = Ideal gas constant, 0.06236 mm Hg m3/°g-mole (21.85 1n.
Hg-ft3/°R-lb-mole).
T a Absolute average dry gas meter temperature (see Figure 2),
m
°K (°R).
8 Absolute temperature of hydrocarbon sample at flow meter,
°K (°R).
-------
Ts ¦ Absolute average stack gas temperature (see Figure 2),
°K (°R).
Tst(1 ¦ Standard absolute temperature, 293°K (528°R).
Vlc ° Total volume of liquid collected in impingers and silica
gel (see Figure 5), ml.
Vm ¦ Volume of gas sample as measured by dry gas meter, dcm (dcf).
V|n(std)=! Volume of gas sample measured by the dry gas meter,
corrected to standard conditions, dscm (dscf).
VpC ¦ Volume of water collected 1n precollector, ml.
V^ ¦ Volume of TCE blank, ml.
Vtw * Volume of TCE used 1n wash, ml.
^w(std)" Volume water vapor 1n the gas sample corrected to
standard conditions, scm (scf).
Vwt(std)s Vo^ume water vapor 1n sample gas corrected to
standard conditions, scm (scf).
v$ « Average stack gas velocity, calculated by Equation 2-9
of Method 2 using data obtained from this method, m/sec
(ft/sec).
¦ Weight of residue 1n TCE wash, mg.
Y ¦ Dry gas meter calibration factor.
AH ¦ Average pressure differential across the orifice meter
(see Figure 2), mm H20 (in. H20).
pj. = Density of TCE, mg/ml (see Label on bottle).
Pw » Density of water, 0.9982 g/ml (0.002201 lb/ml).
e « Total sampling time, min.
¦ Sampling time Interval, from the beginning of a run until
the first component change, min.
-------
B Sampling time interval, between two successive component
changes, beginning with the Interval between the first
and second changes, min.
6p = Sampling time interval, from the final (nth) component
change until the end of the sampling run, min.
13.6 = Specific gravity of mercury.
60 » sec/mln.
100 = Conversion to percent.
6.2 Particulate Calculations.
6.2.1 Average dry gas meter temperature and average orifice
pressure drop. See data sheet (Figure 2).
6.2.2 Dry Gas Volume. Correct the sample volume measured by
the dry gas meter to standard conditions (20°C, 760 tun Hg or 68CF,
29.92 In. Hg} by using Equation 1.
^ + Ph»rs + (AH/13.6)
m(staj m T —a1 • ¦ ¦¦ 1 m T,
•" std ro
Equation 1
where:
= 0.3858 °K/mm Hg for metric units.
= 17.64 °R/in. Hg for English units.
Note: Equation 1 can be used as written unless the leakage ratfc
observed during any of the mandatory leak checks (i.e., the post-test
leak check or leak checks conducted prior to component changes)
exceeds Lfl. If Lp or exceeds La, Equation 1 must be modified as
follows:
-------
a. Case I. No component changes made during sampling run.
In this case, replace Vm in Equation 1 with the expression:
C»n, " el " «L1 ' La> el "
and substitute only for those leakage rates (L. or L ) which exceed L .
1 P O
6.2.3 Volume of Water Vapor.
p RT
Vw(std) = V,c (p^f) " Vic E,u.t)on 2-1
.RT
Wm) ¦ (Vlc + V (P^f» ¦ K2(Vlc'V'
Equation 2-2
where:
3
K2 ¦ 0.001333 m /ml for metric units.
= 0.04707 ft^/ml for English units.
Note: V t 1s used 1n place of Vw when there is measurable
condensed water 1n the particulate precollector catch.
6.2.4 Moisture content.
y
Bws " TZ—tW: x Equation 3-1
ws m(std) + w(std)
Bwt - n Equation 3-2
wt Vm(std) + wt(std)
-------
Note: B * 1s used 1n place of when there is measurable
Wt W5
condensed water in the particulate precollector catch.
In saturated or water droplet-laden gas streams, two calculations
of the moisture content of the stack gas shall be made, one from the
implnger and precollector analysis (Equations 2 and 3), and a second
from the assumption of saturated conditions. The lower of the two
values of moisture content shall be considered correct. The procedure
for determining the moisture content based upon assumption of saturated
conditions is given in the Note of Section 1.2 of Reference Method 4.
For the purposes of this method, the average stack gas temperature
from Figure 2 may be used to make this determination, provided that
the accuracy of the 1n-stack temperature sensor 1s +1°C (2°F).
6.2.5 TCE blank concentration.
"t
C. = n-=- Equation 4
1 Vt
6.2.6 TCE wash blank.
Wt ¦ (Ct)(Vtw)(pt) Equation 5
6.2.7 Total particulate weight. Determine the total particulate
catch from the sum of the weights obtained from Containers 1, 2, and 3
less the TCE blank (see Figure 5).
6.2.8 Particulate concentration.
cs - (0.001 g/mg)
-------
6.2.9 Conversion Factors:
From
scf
g/ft3
g/ft3
To
m
gr/fr
lb/ft3
3
Multiply by
0.02832
15.43
2.205 x 10
35.31
-3
g/ft g/m
6.2.10 Isokinetic Variation.
6.2.10.1 Calculations from raw data.
. ,0° TS CVlc + s vs An °
where:
s 4.320 for metric units.
¦ 0.09450 for English units.
* Note: Use Bwt> 1f applicable.
Equation 7
Equation 8
6.2.10.3 Acceptable results. If 90 percent < I <_ 110 percent,
the results are acceptable. If the results are low in comparison to
-------
the standards and I 1s beyond the acceptable range, the Administrator
may opt to accept the results. Use Citation 4 1n Section 7 to make
judgments. Otherwise, reject the results and repeat the test.
6.3 Gaseous Hydrocarbon Calculations.
6.3.1 Nomograph Correction. If the HC side-stream flow rate
exceeds 1.0 liter/m1n, a nomograph correction must be made to com-
pensate for the side-stream; otherwise, Isokinetic sampling rates will
not be maintained. A suggested approach is as follows: Perform an
orifice calibration run (prior to the sample run) at a flow rate equal
to the side-stream flow rate; use the dry gas meter and a stop watch
to set the flow rate. Determine the orifice pressure drop (aH) at
this flow rate. Then, during the sample run, subtract out this pressure
drop from the value of AH at each traverse point. Other nomograph
correction procedures may be used, subject to the approval of the
Administrator.
6.3.2 Average the ppm by volume readings of gaseous hydrocarbons
for each traverse point and calculate the average concentration. The
stack area and the velocity (calculated using Equation 2-9 of Method 2)
can be used to calculate the mass emission rate of hydrocarbons as
methane by using Equation 9.
pmr = 0.67 x 106 (ppin ) (v.) (A ) Equation 9
V 5 5
7. Bibliography
1. Addendum to Specifications for Incinerator Testing at Federal
Facilities. PHS, NCAPC. Dec. 6, 1967.
-------
2. Martin, Robert M. Construction Details of Isokinetic
Source-Sampling Equipment. Environmental Protection Agency.
Research Triangle Park, N.C. APTD-0581. April, 1971.
3. Rom, Jerome J. Maintenance, Calibration, and Operation of
Isokinetic Source-Sampling Equipment. Environmental Protection Agency.
Research Triangle Park, N.C. APTD-0576. March, 1972.
4. Smith, W. S., R. T. Shlgehara, and W. F. Todd. A Method of
Interpreting Stack Sampling Data. Paper Presented at the 63rd Annual
Meeting of the A1r Pollution Control Association, St. Louis, Mo.
June 14-19, 1970.
5. Smith, W. S., et. al. Stack Gas Sampling Improved and
Simplified With New Equipment. APCA Paper No. 67-119. 1967.
6. Specifications for Incinerator Testing at Federal Facilities.
PHS, NCAPC. 1967.
7. Shlgehara, R. T. Adjustments 1n the EPA Nomograph for
Different P1tot Tube Coefficients and Dry Molecular Weights. Stack
Sampling News 2_:4-ll. October, 1974.
8. Vollaro, R. F. A Survey of Commercially Available Instrumenta-
tion 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).
9. Annual Book of ASTM Standards. Part 26. Gaseous Fuels; Coal
and Coke; Atmospheric Analysis. American Society for Testing and
Materials. Philadelphia, Pa. 1974. pp. 617-622.
-------
PLANT
LOCATION
OPERATOR—
BATE_—
ma BO
SAMPLE MX NO..
METER BOX NO..
METE* AH0
FFACTOR
mot TO BE COEFFICIENT. Cp .
SCHEMATIC OF STACK CROSS SECTION
FILTER HO*
AMBIENT TEMPERATURE —
BAROMETRIC PRESSURE .
ASSUttEO MOISTURE, *
PROBE LENGTH, a (f|>
NOZZLE IDENTIFICATION NO. _____
AVERAGE CALIBRATED NOZZLE DIAMETER, cm CO
PROSE NEATER SETTING
LEAK RATE. IcM
PROBE LINER MATERIAL
STATIC PRESSURE, mm Hg (in. Hg)
TRAVERSE POINT
NUMBER
sampling
TWE
\eitmK
~ACUDM
jmHi
G«.Htf
HACK
TEXPERATURE
VELOCITY
HEAO
UP*).
mrTiiUHiO
PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE .
METER
mmnjp
(«. H?0)
CAS SAMPLE
VOLUME
•* (f|3)
CAS SAMPLE TEMPERA-
TURE AT ORY GAS METER
FILTER CAS
EXIT
TEMPERATURE,
*C(*Fl
TEMPERATURE
OF CAS
LEAVING
CONDENSER OR
LAST UlPltMSER.
•c Pf)
TOTAL
GASEOUS
HYDROCARBON
INLET
#C(#F)
OUTLET
°CfF>
-
TOTAL
AVC.
AVG.
AVERAGE
AVG.
Figure 2. Paniculate and gaseous hydrocarbon field data.
-------
7.0 SOURCE SURVEILLANCE; EMISSION SAMPLING
For lead emission source sampling and analysis, EPA reconmends a
modified EPA Method 5^ sampling train for sample collection, with lead
analysis by atomic absorption spectrometry (AAS).
In this adaptation of the Method 5 sampling train, 100 ml of 0.IN
HNOj is placed 1n each of the first two iinplngers to facilitate collection
of gaseous lead. Since no separation of gaseous and particulate lead
is attempted, a filter, which is of high purity glass fiber, is located
between the third and fourth Impingers as a backup collector. After
sampling 1s completed, the filter portion 1s extracted for lead in a nitric
acid reflux procedure.
A rigorous pretneatment with HNO^ of all sample-exposed surfaces and
containers, blank analyses of filters and 0.1N HNOg, and the most recent
revisions of the Method 5 sample recovery procedure are all employed to
Insure that high quality samples are obtained.
As a precaution against the problem of sample matrix effects, the
analytical technique known as the Method of Standard Additions is used
for the filter portion of the sample. For the more general lead emission
measurement method required by the SIP regulations, EPA 1s now planning
to extent this technique (which is commonly employed by those who use AAS)
to the total sample. Additionally, the 1mp1nger portion will also be
refluxed to Insure solubilization of all lead compounds. Work has been
Initiated to confirm those approaches on a variety of sources.
A detailed description of the emission sampling and analysis tech-
niques appears In Appendix a/of this cju^c/iag.
40 CFR Part 50, "Standards of Performance for New Stationary Sources,"
Appendix A, "Reference Methods," Method 5, "Determination of Particulate
HrnissiooG from Stationary Sources."
.36'
7
x
-------
u u/ia
APPENDIX A
TENTATIVE PRXEDURE FOR DETERMINING
INORGANIC LEAD EMISSIONS FROM STATIONARY SOURCES
-------
APPENDIX A
TENTATIVE PROCEDURE FOR DETERMINING
INORGANIC LEAD EMISSIONS FROM STATIONARY SOURCES
1. Principle, Applicability, and Range
1.1 Principle. Particulate and gaseous lead emissions are
withdrawn isokinetically from the source. The collected samples are
digested in acid solution and analyzed by atomic absorption spectro-
photometry.
1.2 Applicability. This method 1s applicable for the determina-
tion of inorganic lead emissions from stationary sources.
1.3 Range. The upper limit can be considerably extended by
dilution. For a minimum analysis accuracy of + 10 percent, a minimum
lead mass of 50 yg should be collected 1n each sample fraction,
2. Apparatus
2.1 Sampling Train. A schematic of the sampling train used in
this method 1s shown 1n Figure A-l. Complete construction details are
2
given 1n APT0-0581 ; commercial models of this train are also avail-
able. For changes from APTD-0581 and for allowable modifications
of the train shown 1n Figure A-l, see the following subsections. The
use of a flexible line between the probe and first impinger 1s not
allowed.
The operating and maintenance procedures for the sampling train
are described 1n APTD-0576^. Since correction7'jsage 1s important
1n obtaining valid results, all users should read APTD-0576 and
adopt the operating and maintenance procedures outlined 1n 1t, unless
otherwise specified herein. The sampling tratn consists of the
following components:
A-l
X
-------
THERMOMETER
TEMPERATURE SENSOR
THERMOMETER
CHECK
VALVE
PROBE
3»
l
t\»
1.9 TO 2.5 cm
(0.75 TO 1 in.)
FILTER HOLDER
STACK
WALL
~
REVERSE-TYPE
PITOTTUBE
7
PITOT MANOMETER
TEMPERATURE
d SENSOR
HEATED AREA
V77*
IMPINGERS
PROBE
THERMOMETERS
VACUUM
GAUGE
BY PASS VALVE
ORIFICE
PITOTTUBE
MAIN VALVE
DRY
CAS METER
AIR-TIGHT
PUMP
VACUUM
LINE
1.9 cm (0.75 in.)
Figure-' A _i .Lead sampling train.
*IF DIFFICULTY IS EXPECTED IN INSERTING THE TEMPERATURE SENSOR-PITOT TUBE-PROBE ASSEMBLY INTO
THE STACK DUE TO SPACING REQUIREMENTS, THE TEMPERATURE SENSOR MAY BE LOCATED BETWEEN THE
PROBE AND PITOT TUBE SO THAT THE TIP OF THE TEMPERATURE SENSOR IS NO CLOSER THAN 5cm (2 in.)
FROM THE TIP OF THE PITOT TUBE.
*
-------
s$*
2.1.1 Probe Nozzle. Stainless steel (316) or glass with
sharp, tapered leading edge. The angle of taper shall be <_ 30° and
the taper shall be on the outside to preserve a constant Internal
diameter. The probe nozzle shall be of the button-hook or elbow
design, unless otherwise specified by the Administrator. If made of
stainless steel, the nozzle shall be constructed from seamless tubing;
other materials of construction may be used, subject to the approval
of the Administrator.
A range of nozzle sizes suitable for isokinetic sampling should
be available, e.g., 0.32 to 1.27 cm (1/8 to 1/2 in.)—or larger 1f
'higher volume sampling trains are used—inside diameter (ID) nozzles
In increments of 0.16 cm (1/16 in.). Each nozzle shall be identified
and calibrated (see Section 5.2).
2.1.2 Probe Liner. Borosllicate or quartz glass tubing with a
heating system capable of maintaining a gas temperature at the exit end
during sampling of 120 + 14°C (248 + 25°F); note that lower exit
temperatures are acceptable, provided that they exceed the stack gas
dew point. Since the actual temperature at the outlet of the probe is
not usually monitored during sampling, probes constructed according to
APTD-0581 and utilizing the calibration curves of APTD-0576 (or cali-
brated according to the procedure outlined in APTD-0576) will be
considered acceptable.
Either borosllicate or quartz glass probe liners may be used for
stack temperatures up to about 480°C (900°F); quartz liners shall be
A-3
-------
used for temperatures between 480 and 900°C (900 and 1650°F).
Both types of liners may be used at higher temperatures than
specified for short periods of time, subject to the approval of
the Administrator. The softening temperature for borosilicate
is 820°C (1508°F), and for quartz it is 1500°C (2732°F).
Whenever practical, every effort should be made to use
borosilicate or quartz glass probe liners. Alternatively, metal
liners (e.g., 316 stainless steel, Incoloy 825,* or other corrosion
resistant metals) made of seamless tubing may be used, subject to
the approval of the Administrator.
2.1.3 Pitot Tube. Type S, as described 1n Section 2.1 of
Method 2.? or other device approved by the Administrator. The
pitot tube shall be attached to the probe (as shown 1n Figure A-l)
to allow constant monitoring of the stack gas velocity. The impact
(high pressure) opening plane of the pitot tube shall be even with
or above the nozzle entry plane (see Method 2, Figure 2-6b) during
sampling. The Type S pitot tube assembly shall have a known coef-
ficient, determined as outlined in Section 4 of Method 2.
2.1.4 Differential Pressure Gauge. Inclined manometer or
equivalent device (two), as described 1n Section 2.2 of Method 2.
One manometer shall be used for velocity head (Ap) readings, and the
other, for orifice differential pressure readings.
~Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
A-4
-------
2.1.5 Filter Holder. Borosilicate glass, with a glass frit
filter support and a silicone rubber gasket. Other materials of
construction (e.g., stainless steel, Teflon, Viton) may be used,
subject to the approval of the Administrator. The holder design
shall provide a positive seal against leakage from the outside or
around the filter. The filter holder shall be inserted between the
third and fourth impingers.
2.1.6 Impingers. Four Impingers connected in series with
leak-free ground glass fittings or any similar leak-free noncon-
taminating fittings. The first, third, and fourth impingers shall
.be of Greenburg-Smith design, modified by replacing the tip with
a 1.3 cm (1/2 1n.) Il5 glass tube extending to about 1.3 cm (1/2 1 n.)
from the bottom of the flask. The second 1mp1nger shall be of the
Greenburg-Smith design with the standard tip. The first and second
impingers shall contain known quantities of 0.1 normal nitric acid
(Section 4.1.3), the third shall be empty, and the fourth shall
contain a known weight of silica gel, or equivalent deslccant. A
thermometer, capable of measuring temperature to within 1°C (2°F)
shall be placed at the outlet of the fourth 1mp1nger for monitoring
purposes.
2.1.7 Metering System. Vacuum gauge, leak-free pump, ther-
mometers capable of measuring temperature to within 3°C (5.4°F), dry
gas meter capable of measuring volume to within 2 percent, and
related equipment, as shown 1n Figure Arl. Other metering systems
capable of maintaining sampling rates within 10 percent of isokinetic
and of determining sample volumes to within 2 percent may be used,
A-5
-------
subject to the approval of the Administrator. When the metering
system is used in conjunction with a pitot tube, the system shall
enable checks of isokinetic rates.
Sampling trains utilizing metering systems designed for higher
flow rates than that described in APTD-0581 or APTD-0576 may be
used provided that the specifications of this method are met.
2.1.8 Barometer. Mercury, aneroid, or other barometer 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
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 sampling point shall 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.
2.1.9 Gas Density Determination Equipment. Tempeature sensor
and pressure gauge, as described 1n Sections 2.3 and 2.4 of Method 2,
14
and gas analyzer, 1f necessary, as described in Method 3. The
temperature sensor shall, preferably, be permanently attached to
the pitot tube or sampling probe in a fixed configuration, such that
the tip of the sensor extends beyond the leading edga of the probe
sheath and does not touch any metal. Alternatively, the sensor may
be attached just prior to use in the field. Note, however, that 1f
the temperature sensor 1s attached 1n the field, the sensor must be
placed 1n an Interference-free arrangement with respect to the Type S
A-6
-------
pi to t tube openings (see Method 2, Figure 2-7). As a second
alternative, provided that a difference of not more than 1 percent
in the average velocity measurement is introduced, the temperature
gauge need not be attached to the probe or pi tot tube. (This
alternative is subject to the approval of the Administrator.)
2.2 Sample Recovery. The following items are needed:
2.2.1 Probe-Liner and Probe-Nozzle Brushes. Nylon bristle
brushes with stainless steel wire handles. The probe brush shall
have extensions (at least as long as the probe) of stainless steel,
Nylon, Teflon, or similarly Inert material. The brushes shall be
t properly sized and shaped to brush out the probe liner and nozzle.
2.2.2 Glass Wash Bottles--Two.
2.2.3 Glass Sample Storage Containers. Chemically resistant,
borosilicate glass bottles, for 0.1 N HNOj Impinger and probe
solutions and washes, 1000 ml. Screw cap liners shall either be
rubber-backed Teflon or shall be constructed so as to be leak-free
and resistant to chemical attack by 0.1 N HNOg. (Narrow mouth glass
bottles have been found to be less prone to leakage.)
2.2.4 Petri Dishes. For filter samples, glass or polyethylene,
unless otherwise specified by the Administrator.
2.2.5 Graduated Cylinder and/or Balance. To measure condensed
water to within 2 ml or 1 g. The graduated cylinder shall have a
minimum capacity of 500 ml, and subdivisions no greater than 5 ml.
Most laboratory balances are capable of weighing to the nearest 1.0 g
or less. Any of these balances 1s suitable for use here and in
Section 2.3.4.
-------
/W*
2.2.6 Plastic Storage Containers. Air-tight containers
to store silica gel.
2.2.7 Funnel and Rubber Policeman. To aid in transfer of
silica gel to container; not necessary if silica gel is weighed in
the field.
2.2.8 Funnel. Glass, 'to aid in sample recovery,
2.3 Analysis.
2.3.1 Atomic Absorption Spectrophotometer. With lead hollow
cathode lamp and burner for air/acetylene flame.
2.3.2 Steam Bath.
2.3.3 Hot Plate.
2.3.4 Reflux Condensers. 300 mm, 24/40 5 to fit Erlenmeyer
flasks.
2.3.5 Erlenmeyer Flasks. 125 ml 24/40 5.
2.3.6 Membrane Filters. Mi 11ipore SCWPO 4700 or equivalent.
2.3.7 Filtering Apparatus. Millipore filtering unit, consisting
of one of the assemblies shown 1n Figure A-3.
2.3.8 Volumetric Flasks. 100 ml.
3. Reagents
3.1 Sampling.
3.1.1 Filters. High purity glass fiber filters, without organic
binder, exhibiting at least 99.95 percent efficiency {<0.05 percent
penetration) on 0.3 micron dioctyl phthalate smoke particles. The
filter efficiency test shall be conducted 1n accordance with ASTM
Standard Method D 2986-71. Test data from the supplier's quality
X
-------
*4#
control program are sufficient for this purpose. Filters shall be
Gelman Spectro Grade, or equivalent, with lot Assay for Pb. Reeve
Angel 934 AH and MSA 1106 BH filters have been found to be equivalent.
3.1.2 Silica Gel. Indicating type, 6 to 16 mesh. If previously
used, dry at 175°C (350°F) for two hours. New silica gel may be used
as received. A1ternatively, other types of desiccants (equivalent or
better) may be used, subject to the approval of the Administrator.
3.1.3 Nitric Acid, 0.1 Normal (N). Prepared from reagent grade
HNO^ and deionized, distilled water (Reagent 3.4.1, below). It may
be desirable to run blanks prior to field use to eliminate a high blank
.on test samples. Prepare by diluting 6.5 ml of concentrated nitric
"acid (69 percent) to 1 liter with deionized, distilled water.
3.1.4 Crushed Ice.
3.1.5 Stopcock Grease. HNOj insoluble, heat stable silicone
grease. This is not necessary 1f screw-on connectors with Teflon
sleeves, or similar, are used. Alternatively, other types of stopcock
grease may be used, subject to the approval of the Administrator.
3.2 Pretest Preparation.
3.2.1 Nitric Acid, 6 N. Prepared from reagent grade HN03 and
deionized, distilled water. Prepare by diluting 390 ml of concentrated
nitric acid (69 percent) to 1 liter with deionized, distillied water.
3.3 Sample Recovery.
3.3.1 Nitric Acid, 0.1 N. Same as 3.1.3 above.
3.4 Analysis.
3.4.1 Water. Deionized, distilled to conform to ASTM Specification
D 1193-74, Type 3.1'
X
-------
124*
3.4.2 Nitric Acid. Redistilled ACS reagent grade, concentrated.
3.4.3 Nitric Acid, 4.6 N. Dilute 300 ml of redistilled
concentrated nitric acid to 1 liter with deionized, distilled water.
3.4.4 Stock Lead Standard Solution (100 yg Pb/ml). Dissolve
0.1598 g of reagent grade Pb (N03)2 in about 700 ml of deionized
distilled water, add 10 ml redistilled concentrated HNOj, and dilute
to 1000 ml.
3.4.5 Lead Standards.
3.4.5.1 Solution Sample Standards. Pipet 1.0, 5.0, 10.0 and
20.0 ml aliquots of the 100 wg/ml stock lead standard solution
.(Reagent 3.4.4) into 100 ml volumetric flasks. Add 30 ml redistilled
'concentrated HNO-j to each flask and dilute to volume with deionized,
distilled water. These working standards contain 1.0, 5.0, 10.0 and
20.0 ug Pb/ml, respectively. Additional standards at other concen-
trations should be prepared as needed. Use 4.6 N HN03 (Reagent 3.4.3)
as the reagent blank.
3.4.5.2 Filter Sample Standards. Pipet 1.0, 5.0, 10.0 and 20.0 ml
aliquots of the 100 yg/ml stock lead standard solution into 125 ml
Erlenmeyer flasks. Place a glass fiber filter (Section 3.1.1), cut
into strips, in each flask. Use filters from the same lots as those
used for sampling. Add 30 nil of redistilled concentrated nitric acid
to each flask and sufficient distilled, deionized water to make a
total volume of 60 ml. Reflux each solution for two hours and cool
to room temperature. Rinse the condenser column with a small amount
of deionized, distilled water and remove the flask. Filter each
A-10
X
-------
\W
standard through a milUpore membrane filter into a 100 tnl volumetric
flask. Rinse the membrane filter and the remaining glass fiber mass
with several small portions of deionized, distilled water, and
combine with the filtrate. Dilute each standard to 100 ml.
3.4.6 Air. Of a quality suitable for atomic absorption analysis.
3.4.7 Acetylene. Of a quality suitable for atomic absorption .
analysis.
4. Procedure
4.1 Sampling. The complexity of this method is such that, in
order to obtain reliable results, testers should be trained and
•experienced with the test procedures.
4.1.1 Pretest Preparation. All the components shall be maintained
and calibrated according to the procedure described in APTD-0576,
unless otherwise specified herein. In addition, prior to testing,
all sample-exposed surfaces shall be rinsed, first with 6 N HN03 and
then with deionized, distilled water.
Weigh several 200 to 300 g portions of silica gel 1n air-tight
containers to the nearest 0.5 g. Record the total weight of the
silica gel plus container, on each container. As an alternative, the
silica gel need not be prewelghed, but may be weighed directly in its
impinger just prior to train assembly.
Check filters visually against light for Irregularities and flaws
or pinhole leaks. Label the shipping containers (glass or plastic
patri dishes) and keep the filters in these containers at all times
except during sampling and analysis.
-------
iW
4.1.2 Preliminary Determinations. Select the sampling site and
the minimum number of sampling points according to Method 1 or as
specified by the Administrator. Determine the stack pressure,
temperature, and the range of velocity heads using Method 2*, it is
recommended that a leak-check of the pi tot lines (see Method 2,
Section 3.1) be performed. Determine the moisture content using
Approximation Method 14^ or its alternatives for the purpose of making
isokinetic sampling rate settings. Determine the stack gas dry
molecular weight, as described 1n Method 2, Section 3.6; if integrated
Method 3 sampling is used for molecular weight determination, the
'integrated bag sample shall be taken simultaneously with, and for
the same total length of time as, the sample run.
Select a nozzle size based on the range of velocity heads, such
that it is not necessary to change the nozzle size in order to
maintain isokinetic sampling rates. During the run, do not change
the nozzle size. Ensure that the proper differential pressure gauge
is chosen for the range of velocity heads encountered (see Section 2.2
of Method 2).
Select a suitable probe liner and probe length such that all
traverse points can be sampled. For large stacks, consider sampling
from opposite sides of the stack to reduce the length of probes.
Select a total sampling time greater than or equal to the minimum
total sampling time specified in the test procedures for the specific
industry such that (1) the sampling time per point 1s not less than
2 minutes (or some greater time Interval as specified by the
A-12
-------
Administrator), and (2) the sample volume taken (corrected to standard
conditions) will exceed the required minimum total gas sample volume.
The latter is 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 minute, 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.
4.1.3 Preparation of Collection Train. During preparation and
'assembly of the sampling train, keep all openings where contamination
can occur covered until just prior to assembly or until sampling 1s
about to begin.
Place 100 ml of 0.1 HN03 1n each of the first two Impingers,
leave the third impinger empty, and transfer approximately 200 to
300 g of preweighed silica gel from Its container to the fourth impinger.
More silica gel may be used, but care should be taken to ensure that
1t is not entrained and carried out from the impinger during sampling.
Place the container in a clean place for later use 1n the sample
recovery. Alternatively, the weight of the silica gel plus impinger
may be determined to the nearest 0.5 g and recorded.
Using a tweezer or clean disposable surgical fjloves, place a
filter 1n the filter holder. Be sure that tlu> filter is properly
centered and the gasket properly placed so <» • invent the sample
A-13
X
-------
m*
gas stream from circumventing the filter. Check the filter for tears
after assembly is completed.
When glass liners are used, install the selected nozzle using
a Viton A 0-ring when stack temperatures are less than 260°C (500°F)
and an asbestos string gasket when temperatures are higher. See
APTD-0576 for details. Other connecting systems using either 316
stainless steel or Teflon ferrules may be used. When metal liners
are used, install the nozzle as above or by a leak-free direct
mechanical connection. Mark the probe with heat resistant tape or
by some other method to denote the proper distance into the stack or
duct for each sampling point.
Set up the train as in Figure A-l, using (if necessary) a very
light coat of silicone grease on all ground glass joints, greasing
only the outer portion (see APTD-0576) to avoid possibility of con-
tamination by the silicone grease.
Place crushed ice around the impingers.
4.1.4 Leak-Check Procedures.
4.1.4.1 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 shall be used.
After the sampling train has been assembled, turn on and set the
probe heating system at the desired operating temperature. Allow time
for ths temperature to stabilize. If a Viton A 0-ring or other leak-
free connection 1s used 1n 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 Hg (15 in. Hg) vacuum.
A-14
-------
17&
Note: A lower vacuum may be used, provided that 1t is not
exceeded during the test.
If an asbestos string is used, do not connect the probe to the
train during the leak-check. Instead, leak-check the train by first
plugging the inlet to the impingers and pulling a 380 mm Hg (15 in.
Hg) vacuum (see note immediately above). Then connect the probe to
the train and leak-check at about 25 mm Hg (1 in. Hg) vacuum;
alternatively, the probe may be leak-checked with the rest of the
sampling train, 1n one step, at 380 mm Hg (15 in. Hg) vacuum. Leakage
rates in excess of 4 percent of the average sampling rate or 0.00057
3
m /min (0.02 cfm), whichever is less, are unacceptable.
The following leak-check instructions for the sampling train
described in APTD-0576 and APTD-0581 may be helpful. Start the pump
with bypass valve fully open and coarse adjust valve completely closed.
Partially open the coarse adjust valve and slowly close the bypass
valve until the desired vacuum is reached. Do_ not reverse direction
of bypass valve; this will cause 0.1 N HN03 to back up into the probe.
If the desired vacuum is exceeded, either leak-check at this higher
vacuum or end the leak check as shown below and start over.
When the leak-check is completed, first slowly remove the plug
from the inlet to the probe and immediately turn off the vacuum pump.
This prevents the 0.1 N HNO^ in the impingers from being forced backward
and silica gel from being entrained backward.
4.1.4.2 Leak-Checks During Sample Run. If, during the sampling
run, a component (e.g., filter assembly or impinger) change becomes
A-15
-------
(H*
necessary, a leak-check shall be conducted immediately before the
change is made. The leak-check shall be done according to the
procedure outlined in Section 4.1.4.1 above, except that it shall
be done at a vacuum equal to or greater than the maximum value
recorded up to that point in the test. If the leakage rate is found
to be no greater than 0.00057 m /min (0.02 cfm) or 4 percent 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
shall either record the leakage rate and plan to correct the sample
volume as shown in Section 6.3 of Reference Method s]6or shall void the
sampling run.
Immediately after component changes, leak-checks are optional;
if such leak-checks are done, the procedure outlined in Section 4.1.4.1
above shall be used.
4.1.4.3 Post-test Leak-Check. A leak-check is mandatory at the
conclusion of each sampling run. The leak-check shall be done in
accordance with the procedures outlined in Section 4.1.4.1, except
that it shall be conducted at a vacuum equal to or greater than the
maximum value reached during the sampling run. If the leakage rate
is found to be-no greater than 0.00057 m^/min (0.02 cfm) or 4 percent
of the average sampling rate (whichever 1s less), the results are
acceptable, and no correction need be applied to the total volume of
dry gas metered. However, if a higher 'leakage rate 1s obtained, the
tester shall either record the leakage rate and correct the sample
A-16
-------
[<\{*
volume as shown in Section 6.3 of Method 5, or shall void the
sampling run.
4.1.5 Sampling Train Operation. During the sampling run,
*
maintain an isokinetic sampling rate (within 10 percent of true
isokinetic unless otherwise specified by the Administrator).
For each run, record the data required on a data sheet such
as the one shown in Figure A-2. Be sure to record the initial dry
gas meter reading. Record the dry gas meter readings at the beginning
and end of each sampling time increment, when changes in flow rates
are made, before and after each leak check, and when sampling 1s halted.
.Take other readings required by Figure A-2 at least once at each
'sample point during each time increment and additional readings when
significant changes (20 percent variation in velocity head readings)
necessitate additional adjustments 1n flow rate. Level and zero the
manometer. Because the manometer level and zero may drift due to
vibrations and temperature changes, make periodic checks during the
traverse.
Clean the portholes prior to the test run to minimize the chance
of sampling deposited material. To begin sampling, remove the nozzle
cap, verify that the probe heating system is up to temperature, and
that the pitot tube and probe are properly positioned. Position the
nozzle at the first traverse point with the tip pointing directly into
the gas stream. Immediately start the pump and adjust the flow to
Isokinetic conditions. Nomographs are available, which aid in the
rapid adjustment of the Isokinetic sampling rate without excessive
A-17
K
-------
HAMT
VOCATION
OPCtAlOK
DATl
run no.
SAMfU IOX NO.
MITU IOX NO.
MlllR ftMW ______
C /ACTO*
WOI TIM COEFFICIENT. C*
FiLTC* i>e»n »r »' /\ri,
AMI If NT TEMPERATURE
(AtOMETRlC PRESSURE
ASSUMED MOISTURE. %
MOM UNCTH. m Cft.l
NOZ7U rOCWfflCATrON hlQ.
AVERAGE CAUtlATCO NOZZlC DIAMETER, «¦»(¦»•).
PROW HI All* SETTING
I ICAK IATC. IcU)
SCMWATIC or STACK CKKS StCT.ON rtolf ^
STATIC msswf,"
TRAVERSE ^OfW
NUMBER
SAMSUNG
TWrtE
(*)<*«
VACuv*
M.
(i n3*;
STACK
TEMPE'-ATURE
r$)
•c rn
VELOCITY
WAD
-------
7\<*
computations. These nomographs are desiyned for use when the
Type S pitot tube coefficient is 0.85 + 0.02, and the stack gas
equivalent density (dry molecular weight) is equal to 29 +4.
APTD-0576 details the procedure for using the nomographs. If Cp and
Mj are outside the above stated ranges, do not use the nomographs
unless appropriate steps (see Citation 7 In Section 7) are taken to
compensate for the deviations.
When the stack is under a significant negative pressure (i a
water column the height of the implnger stem), take care to close the
coarse adjust valve before Inserting the probe into the stack to pre-
vent 0.1 N HN03 from backing Into the probe. If necessary, the pump
may be turned on with the coarse adjust valve closed.
When the probe is 1n position, block off the openings around the
probe and porthole to prevent dilution of the gas stream.
12
Traverse the stack cross-section, as required by Method 1 or as
specified by the Administrator, without bumping the probe nozzle Into
the stack walls when sampling near the walls or when removing or
inserting the probe through the portholes.
During the test run, add 1ce and, 1f necessary, salt to the ice
bath, to maintain a temperature of less than 20°C (68°F) at the
impinger/silica gel outlet. Also, periodically check the level and
zero of the manometer.
A single train shall be used for the entire sample run, except
1n cases where simultaneous sampling 1s required in two or more
separate ducts or at two or more different locations within the same
A-19 X
-------
3*4#
duct, or, in cases where equipment failure necessitates a change of
trains. In all other situations, the use of two or more trains will
be subject to the approval of the Administrator.
Note that when two or more trains are used, separate analyses of
the sample fractions from each train shall be performed, unless other-
wise specified by the Administrator. Consult with the Administrator
for details concerning the calculation of results when two or more
trains are used.
At the end of the sample run, turn off the coarse adjust valve,
remove the probe and nozzle from 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 pitot lines as
described in Method 2, Section 3.1; the lines must pass this leak-check,
in order to validate the velocity head data.
4.1.6 Calculation of Percent Isokinetic. Calculate percent
isokinetic (see Section 6.11 of Method 5), to determine whether the
run was valid or another test run should be made. If there was
difficulty in maintaining isokinetic rates due to source conditions,
consult with the Administrator for possible variance on the Isokinetic
rates.
4.2 Sample Recovery. Proper cleanup procedure begins as soon
as the probe is removed from the stack at the end of the sampling
period. Allow the probe to cool.
When the probe can be safely handled, wipe off all external
particulate matter near the tip of the probe nozzle and place a cap
i
A-20
-------
over it. Do not cap off the probe tip tightly while the sampling
train is cooling down as this would create a vacuum in the filter
holder, thus drawing liquid from the impingers into the probe.
Before moving the sample train to the cleanup site, remove the
probe from the sample train, wipe off the silicone grease, and cap
the open outlet of the probe. Be careful not to lose any condensate
that might be present. Wipe off the silicone grease form the glassware
inlet where the probe was fastened and cap the Inlet. Remove the
umbilical cord from the last impinger and cap the impinger. Either
ground-glass stoppers, plastic caps, or serum caps may be used to close
•these openings.
Transfer the probe and filter-impinger assembly to the cleanup
area. This area should be clean and protected from the wind so that
the chances of contaminating or losing the sample will be minimized.
Save a portion of the 0.1N HNQ3 used for sampling and cleanup
as a blank. Place 200 ml of this 0.1N HNO^ taken directly from the
bottle being used into a glass sample container labeled "0.1N HNO^
blank."
Inspect the train prior to and during disassembly and note any
abnormal conditions. Treat the samples as follows:
Container No. 1. Carefully remove the filter from the filter
holder and place in its identified petrl dish container. If it is
necessary to fold the filter, do so such that the sample-exposed side
1s inside the fold. Carefully transfer to the petrl dish any visible
sample matter and/or filter fibers which adhere to the filter holder
A-21
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gasket by using a dry Nylon bristle brush and/or a sharp-edged
blade. Seal the container.
Container No. 2. Taking care to see that dust on the outside
of the probe or other exterior surfaces does not get into the sample,
quantitatively recover sample matter or any condensate from the
probe nozzle, probe fitting, probe liner, and front half of the
filter holder by washing these components with 0.1N HN03 and placing
the wash into a glass container. Measure and record (to the nearest ml)
the total amount of 0.1N HNO^ used for each rinse. Perform the 0.1N
HNO^ rinses as follows:
Carefully remove the probe nozzle and clean the inside surface
by rinsing with 0.1N HN03 from a wash bottle while brushing with a
stainless steel, Nylon-bristle brush. Brush until the 0.1N HN03 rinse
shows no visible particles, and then make a final rinse of the inside
surface with 0.1N HNO,.
Brush and rinse with 0.1N HNO^ the inside parts of the Swagelok
fitting in a similar way until no visible particles remain.
Rinse the probe liner with 0.1N HN03 by tilting the probe and
squirting 0.1N HN03 into its upper end, while rotating the probe so
that all inside surfaces will be rinsed with 0.IN HNO^. Let the
0.1N HNO^ drain from the lower end Into the sample container. A glass
funnel may be used to aid In transferring liquid washes to the container.
Follow the 0.1N HN03 rinse with a probe brush. Hold the probe in an
Inclined position, squirt 0.1N HN03 Into the upper end of the probe
as the probe brush is being pushed with a twisting action through the
-------
Xtpf
proe; hold a sample container underneath the lower end of the
probe, and catch any 0.1N HNO^ and sample matter which is brushed
from the probe. Run the brush through the probe three times or
more until no visible sample matter is carried out with the 0.1N HNO^
and none remains on the probe liner on visual inspection. With
stainless steel or other metal probes, run the brush through in the
above prescribed manner at least six times since metal probes have
small crevices in which sample matter can be entrapped. Rinse the
brush with 0.1N HNOg and quantitatively collect these washings in the
sample container. After the brushing make a final 0.1N HN03 rinse
of the probe as described above.
It is recommended that two people be used to clean the probe to
minimize loss of sample. Between sampling runs, keep brushes clean
and protected from contamination.
After ensuring that all joints are wiped clean of silicone grease,
clean the inside of the front half of the filter holder by rubbing
the surfaces with a Nylon bristle brush and rinsing with 0.1N HNOg.
Rinse each surface three times or more 1f needed to remove visible
sample matter. Make a final rinse of the brush and filter holder.
After all 0.1N HNOg washings and sample matter are collected 1n the
sample container, tighten the lid on the sample container so that
0.IN HNO^ will not leak out when it is shipped to the laboratory. Mark
the height of the fluid level to determine whether leakage occurred
during transport. Label the container to clearly identify Its contents.
A-23
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Container No. 3. Check the color of the indicating silica gel
to determine if it has been completely spent and make a notation of
its condition. Transfer the silica gel from the fourth impinger to
the original container and seal. A funnel may make it easier to pour
the silica gel without spilling. A rubber policeman may be used as an
aid in removing the silica gel from the impinger. It is not necessary
to remove the small amount of dust particles that may adhere to the
walls and are difficult to remove. Since the gain in weight is to be
used for moisture calculations, do not use any water or other liquids
to transfer the silica gel. If a balance is available in the field,
follow the procedure for Container No. 3 under "Analysis."
Container No. 4. Due to the large quantity of liquid involved,
the impinger solutions are placed together in a separate container.
However, they may be combined with the contents of Container No. 2 at
the time of analysis in order to reduce the number of analyses required.
Clean each of the first three impingers and connecting glassware in
the following manner:
1. Wipe the impinger ball joints free of silicone grease and
cap the joints.
2. Rotate and agitate each impinger, so that the impinger contents
might serve as a rinse solution.
3. Transfer the contents of the impingers to a 500 ml graduated
cylinder. The outlet ball joint cap should be removed and the contents
drained through this opening. The impinger parts (inner and outer
tubes) must not be separated while transferring their contents to the
cy'l inder.
A-24
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Measure the liquid volume to within + 2 ml. Alternatively,
determine the weight of the liquid to within +2.0 g by using a
balance. The volume or weight of liquid present, along with a
notation of any color or film observed in the impinger catch, is
recorded in the log. This information is needed, along with the
silica gel data, to calculate the stack gas moisture content (see
Method 5, Figure 5-3).
4. Transfer the contents of the first three implngers to
Container No. 4.
5. Pour approximately 30 ml of 0.1N HNO^ into each of the first
'three Impingers and agitate the Impingers. Drain the 0.1N HN03
through the outlet arm of each impinger into the No. 4 sample container.
Repeat this operation a second time; Inspect the impingers for any
abnormal conditions.
6. Wipe the ball joints of the glassware connecting the impingers
free of silicone grease and rinse each piece of glassware twice with
0.1N HNOg; this rinse is collected 1n Container No. 4. (Do not rinse
21 brush the glass-fritted filter support.)
Mark the height of the fluid level to determine whether leakage
occurred during transport. Label the container to clearly identify its
contents.
Note: In steps 5 and 6 above, the total amount of 0.1N HN03 used
for rinsing must be measured and recorded.
A-25
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#4*
4.3 Analysis. 1
4.3.1 Container No. 3. This step may be conducted in the
field. Weigh the spent silica gel (or silica gel plus impinger)
to the nearest gram.
4.3.2 Lead Sample Preparation and Analysis.
4.3.2.1 Container No. 1 (Filter). Cut the filter into strips
and transfer the strips and all loose particulate matter to a 125 ml
Erlenmeyer flask. Rinse the petri dish with 30 ml of distilled water
to insure complete transfer of the sample; add the rinse to the flask.
Add 30 ml redistilled concentrated nitric acid. Reflux for two hours
•and cool to room temperature. Rinse the condenser column with a small
amount of deionized, distilled water and remove the flask. Filter the
sample through a millipore membrane filter into a 100 ml volumetric
flask. Rinse the membrane filter and the remaining glass fiber mass
with several small portions of deionized, distilled water, and combine
with the filtrate. Dilute to 100 ml with distilled, deionized water.
4.3.2.2 Container No. 4 (Impinger Samples). Evaporate the liquid
sample just to dryness on a steam bath and transfer to an Erlenmeyer
flask using 30 ml of distilled, deionized water followed by 30 ml of
redistilled concentrated nitric acid. Reflux for two hours. Rinse
the condenser column, cool to room temperature, and dilute to 100 ml
with deionized, distilled water.
4.3.2.3 Container No. ?. (Probe Wash). Treat in the same manner
as directed in Section 4.3.2.2. As an option, this solution can be
combined with the impinger solution prior to analysis.
A-26
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Note: Prior to analysis, the liquid level in Containers No. 2
and/or No. 4 should be checked; confirmation as to whether or not
leakage occurred during transport should be made on the analysis
sheet. If a noticeable amount of leakage has occurred, either void
the sample or take steps, subject to the approval of the Administrator,
to correct the final results.
4.3.2.4 Filter Blank. Determine a filter blank using two filters
from each lot of filters used in the sampling train. Cut each filter
into strips and treat each filter Individually as directed in
Section 4.3.2.1.
4.3.2.5 0.1M HNOj Blank. Treat the entire 200 ml of 0.1N HN03
as directed in Section 4.3.2.2.
4.3.2.6 Spectrophotometer Preparation. Turn on the power, set
the wavelength, s11t width, and lamp current as Instructed by the
manufacturer's manual for the particular atomic absorption spectro-
photometer. Adjust the burner and flame characteristics as necessary.
4.3.2.7 Lead Determination. After the absorbance values have
been obtained for the standard solutions (Section 5), determine the
absorbances of the filter blank and each sample against the reagent
blank, if the sample concentration falls above the limits of the curve
make an appropriate dilution with 4.6 N HNOj, such that the final con-
centration falls within the range of the curve. Determine the lead
concentration in the filter blank (i.e., the average of the two blank
values from each lot). Next, using the appropriate standard curve,
determine the lead concentration 1n each sample fraction.
4.3.2.8 Lead Determination at Low Concentration. Flame atomic
absorption spectrophotometry is a very good analytical method for lead
A-27
-------
concentrations as low as 1 mg/1. If it is necessary to determine
quantities of lead at the microgram per liter level, the graphite
rod or tube furnace, available as accessory components to all
atomic absorption spectrophotometers, 1s recommended. Manufacturer's
instructions should be followed in the use of such equipment.
4.3.2.9 Mandatory Check for Matrix Effects on the Lead Results.
The analysis for lead by atomic absorption is sensitive to the chemical
composition and to the physical properties (viscosity, pH) of the
sample (matrix effects). Since the lead procedure described here will
be applied to many different sources, it can be anticipated that many
.different sample matrices will be encountered. Thus, it is mandatory
"that at least one sample from each source be checked using the Method
of Additions to ascertain that the chemical composition and physical
properties of the sample did not cause erroneous analytical results.
Three acceptable "Method of Additions" procedures are described in
the General Procedure Section of the Perkin Elmer Corporation Manual!^
If the results of the Method of Additions procedure on the source
sample do not agree to within 5 percent of the value obtained by the
conventional atomic absorption analysis, then all samples from the
source must be reanalyzed using the Method of Additions procedure.
5. Calibration
Maintain a laboratory log of all calibrations.
5.1 Standard Solutions. Determine the absorbance of the solution
sample standards and filter sample standards (see Section 3.4.5) against
A-28
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a reagent blank of 4.6N HNO^ (Reagent 3.4.3). These absorbances 9
should be checked frequently during the analysis to insure that
baseline drift has not occurred. Prepare two standard curves of
absorbance versus concentration, one for the solution sample
standards and one for the filter sample standards. (Note: For
instruments equipped with direct concentration readout devices,
preparation of a standard curve will not be necessary.) In all cases,
the manufacturer's instruction manual should be consulted for proper
calibration and operational procedures.
5.2 Sampling Train Calibration. Calibrate the sampling train
components according to the Indicated sections of Method^: probe nozzle
.(Section 5.1); pitot tube assembly (Section 5.2); metering system
(Section 5.3); probe heater (Section 5.4); temperature gauges
(Section 5.5); barometer (Section 5.7). Note that the leak check of
the metering system (Section 5.6 of Method 5) applies to this method.
6. Calculations
6.1 Nomenclature
A = 100 ml/aliquot a sample volume
C = Concentration of lead as read from the standard curve,
a
vg/ml.
C-j » Lead concentration in stack gas, dry basis, converted
to standard conditions, g/dscm (g/dscf).
- Dilution factor = 1 if the sample has not been diluted.
« Total mass of lead collected in a specific part of the
sampling train, ug.
¦ Total mass of lead collected in the sampling train, yg.
A-29
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V / ..jn = Volume of gas sample measured by the dry gas meter,
m(std;
corrected to standard conditions, dscm (dscf);
calculated using Equation 5-1! of Method 5.
6.2 Calculate the average stack gas velocity, according to
Equation 2f9 of Method 2; use data obtained from this method (see
Figure A-2).
6.3 Referring to tfie Indicated sections of Method 5, perform
the following calculations: Average gas meter temperature and orifice
pressure drop (Section 6.2); dry gas volume (Section 6.3); volume of
water vapor (Section 6.4); moisture content (Section 6.5); isokinetic
variation (Section 6.11). Note that for the purposes of this method,
any references made to Figure 5.2 should be Interpreted as references
to Figure A-2.
6.4 Amount of Lead Collected.
6.4.1 Calculate the amount of lead collected in each part of the
sampling train, as follows:
6.4.2 Calculate the total amount of lead collected 1n the
sampling train as follows:
Mt ¦ Mn (filter) + Mn (probe)+ Mn (Impingers) - Mn (filter blank)
6.5 Calculate the lead concentration 1n the stack gas (dry basis*
adjusted to standard conditions) as follows:
Equation A-l
Equation A-2
C, - . (1 X 10"6 g/yg) (Mt/Vm( st£l)) Equation A-3
A-30
-------
»
-------
6.6 Conversion Factors.
From
To
Multiply by
0.02832
scf
g/ft3
g/ft3
g/ft3
gr/ft3
lb/ft3
g/m3
15.13
2.205 x 10"3
35.31
7• Bibliography
1. Addendum to Specifications for Incinerator Testing at Federal
Facilities. PHS, NCAPC. Dec. 6, 1967.
2. Martin, Robert M. Construction Details of Isokinetic Source-
Sampling Equipment. Environmental Protection Agency. Research Triangle
Park, N. C. APTD-0581. April, 1971.
3. Rom, Jerome J. Maintenance, Calibration, and Operation of
Isokinetic Source Sampling Equipment. Environmental Protection
Agency. Research Triangle Park, N. C. APTD-0576. March, 1972.
4. Smith, W.S., R,T. Sfilgehara, and W. F. Todd. A Method of
Interpreting Stack Sampling Data. Paper Presented at the 63d Annual
Meeting of the A1r Pollution Control Association, St. Louis, Mo.
June 14-19, 1970.
5. Smith, U.S., et al, Stack Gas Sampling Improved and Simplified
With New Equipment. APCA Paper No. 67-119. 1967.
6. Specifications for Incinerator Testing at Federal Facilities.
PHS, NCAPC. 1967.
7. Shigehara, R.T. Adjustments 1n the EPA Nomograph for
Different Pi tot Tube Coefficients and Dry Molecular Weights. Stack
Sampling News 2:4-11. October, 1974,
A-32
-------
8. 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).
9. Annual Book of ASTM Standards. Part 26. Gaseous Fuels;
Coal and Coke; Atmospheric Analysis. American Society for Testing
and Materials. Philadelphia, Pa. 1974. pp. 617-622.
10. Analytical Methods for Atomic Absorption Spectrophotometry.
Perkln Elmer Corporation. Norwalk, Connecticut. September, 1976.
11. Annual Book of ASTM Standards. Part 31; Water, Atmospheric
Analysis. American Society for Testing and Materials. Philadelphia,
PA. 1974. pp. 40-42.
12. Code of Federal Regulations. Title 40, Part 60, Appendix
A "Reference Methods." (Published 1n the Federal Register of August
18, 1977, p. 41754). Method 1—Sample and Velocity Traverses for
Stationary Sources.
13. Method 2—Determination of Stack
Gas Velocity and Volumetric Flow Rate (Type S P1tot Tube).
14. Method 3—Gas Analysis for Carbon
Dioxide, Oxygen, Excess A1r, and Dry Molecular Weight.
15 .
Content 1n Stack Gases.
16.
Method 5—Determination of Particu-
Metbod 4—Determination of Moisture
late Emissions from Stationary Sources.
A-33
-------
reference method for DETERMINATION Or
PARTICULATE AMD GASEOUS ARSENIC EMISSION
FROM NON-FERROUS SHELTERS
"1. Principi e and AdpI i csbi 1 it.y
1.1 principle. Particulate and gaseous arsenic emissions are
isokinetically sampled from the source and collected on a glass
mat vi 1 ter and in wat&r. The collected arsenic is then analyzed
using atomic absorption spectrophotometry.
1.2 Applicability. This method is applicable for the
determination of inorganic arsenic emissions from non-ferrous
smelters and as specified in applicable subparts of the standards.
2. Apparatus
2.1 Sampling Train. A schematic of the sampling train used
in this method is shown in Figure 108-1-1. Complete construction
tleti.ils are given in APTD-0531 (Citation 2 in Section 7); commer-
cial models of this train are also available. For changes from
APTG-GS3"; and for allowable modifications of the train shown
in Figure ICS-l-l, see tha following subsections.
The operating and maintenance procedures for the sampling
train are described in APTD-0576 (Citation 3 in Section 7). Since
correct usage is important in obtaining valid results, all users
should read APTD-C575 and adopt the operating and maintenance
procedures outlined in it, unless otherwise specified herein.
The sampling train consists of tha following components:
2.1.1 Probe Nozzle. Stainless steel (315) or glass with
sharp, tapered leading edge. The angle of taper shall be £30°
-------
2
and the taper shall be on the outside to preserve a constant
internal diameter. The probe nozzle shall be of the button-hook
or elbow design, unless otherwise specified by the Administrator.
If made of stainless steal, the nozzle shall be constructed from
seamless tubing; other materials of construction may be used,
subject to the approval of the Administrator.
A range of nozzle sizes suitable for isokinetic sampling
should be available, e.g., 0.32 to 1.27 cm (1/8 to 1/2 in.) —
inside diameter (ID) nozzles in Increments of 0.15 cm (1/16 in.).
Each nozzle shall be calibrated according to the procedures
outlined in Section 5.
2.1.2 Probe Liner. Borosilicate or quartz glass tubing with
a heating system capable of maintaining a gas temperature range
at the exit end during sampling of 110-135°C (230-275°F).
Since the actual temperature at the outlet of the probe is not
usually monitored during sampling, probes constructed according
to APTD-0581 and utilizing the calibration curves of APTD-0576
(or calibrated according to the procedure outlined in APTD-0576)
will be considered acceptable.
Either borosilicate or quartz glass probe liners may be
used for stack temperatures up to about 48Q°C (90Q°F); quartz
liners shall be used for temperatures between 480 and 900°C
(900 and 1550°F). Both types of liners may be used at higher
temperatures than specified for short periods of time, subject
to the approval of the Administrator. The softening temperature
-------
for borosilicuta is 820°C (150S°F), and for quartz It is 1500°C
(2732°F).
Whenever practical, every effort should ba made to use
borosilicato or quartzvglass probe lir.ors. Alternatively, metal
liners (e.g., 316 stainless steel, Incoloy 823,^ or other corrosion
resistant metals) made of seamless tubing may be used, subject to
the approval of the Administrator.
2.1.3 Pi tot Tube. Type S, as described in Section 2.1 of
Method 2,* or other device approved by the Administrator. The
pitot tuba shall be attached to the proba (as shown in Figure 108-1-
to allow constant monitoring of the stack gas velocity. The impact
(high pressure) opening plane of the pitot tuba shall be even with
or above the nozzle entry plane (see ffcthod 2, Figure 2-6b) during
sampling. The Type S pitot tube assembly shall have a known
coefficient, determined as outlined in Section 4 of Method 2.
2.1.4 Differential Pressure Gauge. Inclined manometer or
equivalent device (two), as described in Section 2.2 of Method 2.
One manometer shall be used for velocity head (Ap) readings, and
the other, for orifice differential pressure readings.
2.1.5 Filter Holder. Borosflicate glass, with a glass frit
filter or stainless steal screen support and a silicone rubber
gasket. Other materials of construction (e.g.. Teflon, Viton) may
^Mention of trade namas or specific products does not consti-
tute endorsement by the Environmental Protection Agency.
* A.
Note: This and all subsequent references to other methods
refer to the Methods in 40 CFR 50, Appendix A.
-------
4
be used, subject to the approval of the Administrator. The holder
design shall provide a positive seal against leakage from the
outside or around the filter. The holder shall be attached
immediately at the outlet of the probe (or cyclone, if used).
2.1.6 Filter Heating System. Any heating system capable of
maintaining a temperature range around the filter holder during
sampling of 110-135°C (230-275°F). A temperature gauge capable of
measuring temperature to within 3°C (5.4°F) shall be installed so
that the temperature around the filter holder can be regulated and
monitored during sampling. Heating systems other than the one
shovm in APTD-Q581 may be used.
2.1.7 Impingers. Six impingers connected in series with
leak-free ground glass fittings or any similar leak-free non-con-
taminating, fittings. The first, third, fourth, fifth, and sixth
impingers shall be of the Greenburg-Smith design, modified by
replacing the tip with a 1.3 cm (1/2 in.) ID glass tube extending
to about 1.3 cm (1/2 in.) from the bottom of the flask. The
second impinger shall be of the Greanburg-Smith design with the
standard tip. Modifications (e.g., using flexible connections
between the Impingers or using materials other than glass
(flexible vacuum lines to connect the filter holder to the con-
denser) may be used, subject to the approval of the Administrator.
The first and second impingers shall contain known quantities
of daionizad, distilled water (Section 4.1.3), the third, fourth,
and fifth shall contain 10 percent hydrogen peroxide, and the sixth
-------
5
shall contain a known weight of silica gel, or equivalent desiv
A thermometer, capable of measuring temperature to within 1°C
(2°F) shall be placed at the outlet of the sixth impinger for
monitoring purposes.
2.1.8 Metering System. Vacuum gauge, leak-free pump, ther-
mometers capable of measuring temperature to within 3°C (5.4°F),
dry gas meter capable of measuring volume to within 2 percent,
and related equipment, as shewn In Figure 103-1. Other metering
systems capable of maintaining sampling rates within 10 percent
of isokinetic and of determining sample volumes to within 2 per-
cent may be used, subject to the approval of the Administrator.
When the metering system is used in conjunction with a pitot tube,
the system shall enable checks of isokinetic rates.
2.1.9 Barometer.. .Mercury, aneroid, or other baomater capable
of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
In mdny 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 differences between the weather
station and sampling point shall 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.
2.1.10 Gas Densi ty Determi r,at1 on Equi pr.ar.t. Temperature
sensor and pressure gauge, as described 1n Sections 2.3 and 2.4
of Method 2, and gas analyzers, if necessary, as described 1n Method 3.
-------
If carbon dioxide concentration is determined by Orsat analysis
it.will have to be corrected for SOg interference by subtracti r0
the S02 concentration 'from the C02 reading. The S02 concentra-
tion may be determined from this method as described under
Secc'ion 4.^.
The temperature sensor shall, preferably, be permanently
attached to the pitot tuba or sampling probe in a fixed configura-
tion, such that the tip of the sensor extends beyond the leading
edge of the probe sheath and does not touch any metal. Alterna-
tively, the sensor may be attached just prior to use in the
field. Note, however, that if the temperature sensor is attached
in ths field, the sensor must be placed in an interference-free
arrangement with respect to the Type S pitot tube openings
(ses Method 2, Figure 2-7). As a second alternative if a dif-
ference of not more than 1 percent in the average velocity measure
msnt 1s introduced, the temperature gauge need not be attached
to the proba or pitot tube. (This alternative is subject to
the approval of the Administrator),
2.2 Sample Recovery. The following items are needed:
2.2.1 Probe-Linar and Probe-Nozzle Brushes. Nylon bristle
brushes with stainless steel wire handles. The proba brush shall
have extensions (at least as long as the probe) of stainless steel
Nylon, Teflon, or similarly inert material. The brushes shall be
properly sized and shaped to brush out the probe liner and nozzle.
2.2.2 Wash Bottles—Tv/o. Polyethylene wash bottles are
recommended.
-------
7
2.2.3 Plastic Storage Containers. Chemically resistant,
polyethylene or polypropylene for glassware washc-s, 500 ml or
1000 ml. Also, air-tight containers to store silica gal.
2.2.4 Petri Dishes. For filter samples, glass or
polyethylene, unless otherwise specified by the Administrator.
2.2.5 Graduated Cylinder and/or Balance. To measure con-
densed water to within 1 ml or 1 g. Graduated cylinders shall
have sub-divisions no greater than 2 ml. Most laboratory balances
are capable of weighing to the nearest 0.5 g or less. Any of
these balances is suitable for use here and ir. Section 2.3.4.
2.2.6 Funnel and Rubber Policeman. To aid in transfer of
silica gel to container; not necessary if silica gel is weighed
in the field.
2.2.7 Funnel. Glass or polyethylene, to aid in sample
recovery.
2.3 Analysis. For analysis, the following equipment is
needed:
2.3.1 Spectrophotometer. To measure absorbance at 193.7 m.
It shall be equipped with art electrode!ass discharge lamp and a
background corrector. For measuring samples having less than
10 ug/ml of As, the spectrophotometer shall be equipped with a
vapor generator accessory.
2.3.2 Recorder. To match the output of the spectrophotometer.
2.3.3 Volumetric Flasks. 50 ml.
2.3.4 Balance. To measure within 0.5 g.
-------
8
3. Recants
3.1 Sampling. The reagents used in sailing are as follows:
3.1.1 Filters." '.Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (£0.05 percent
penetration) on 0.3-micron dioctyl phthalate smoke particles. The
filter efficiency test shall be conducted in accordance with ASTM
standard method D 2S86-71. Test data from tha supplier's quality
control program are sufficient for this purpose.
3.1.2 Silica Gel. Indicating type, 6 to 16 mesh. If pre-
viously used, dry at 175°C (350°F) for 2 hours. New silica gel
may be used as received. Alternatively, other types of desiccants
(equivalent or better) may be used, subject to the approval of
the Administrator.
3.1.3 Water, Deionized, Distilled to :r.sat ASTM specification
D1193-74, Type 3. At the option of the analyst, KMMO^ test for
Gxidizabla organic matter may ba omitted whsn high concentrations
of organic matter are not expected to be present.
3.1 A 10 Percent Hydrogen Poroxide by Weight. Prepare by
diluting 294 ml of reagent gr&de 30 percent hydrogen peroxide to 1
liter with deionized, distilled water.
3.1.5 Crushed Ice.
3.1.6 Stopcock Grease. Heat-stable silicone grease. This
is not necessary if screw-on connectors with Teflon sleeves, or
similar, are used. Alternatively, other types of stopcock grease
may ba used, subject to the approval of the Administrator.
-------
3.2 Sc.-ipie Recovery. 0.1 N Sodium hydroxide. Prepare by
v/aighir.c; out 4.CO grams of reagent grade NaOH and dissolving in
about 500 ml of deionized, distilled water in a 1 liter volume-
tric flask. After dissolution is complete, dilute to the mark
with deicnized, distilled water.
3.3 Analysis
3.3.1 Water. Same as 3.1.3 above.
3.3.2 Sodium Borohydrida, 5 Percent, by Weight-Volume.
Prepare by dissolving 5.00 grams of reagent grade NaBH^ in about
500 ml of 0.1 N NaOH solution In a 1 liter volumetric flask.
When dissolution is complete, dilute to the mark with 0.1 N NaOH
solution.
3.3.3 .Hydrochloric Acid, Concentrated, Reagent Grade.
3*3.4 Potassium Iodide 30 Percent by Weight-Volume. Pre-
pare by dissolving 300 g of reagent grade KI in 500 ml of water
in a 1 liter volumetric flask. When dissolution is complete,
dilute to tfta mark with deionized, distilled water.
3.3.5 Sodium Hydroxide. 0:1 N, Sarae as 3.3 above.
3.3.6 SiVium Hydroxide, 1.0 N. Prepare by dissolving
40.00 g. of reagent grade NaOH in about 500 ml of deionized,
distilled water in a 1 liter volumetric flask. Whan dissolution
is complete, dilute to the mark with deionizad, distilled water.
3.3.7 Phenolahthslein. Prepare by dissolving 0.05 g of
phono*! phthal sin in 50 ml of 90 percent ethar.ol and 50 n\l of
deionizad, distilled water.
-------
3.3.3 Nitric Acid, Concentrated. ACS grada.
3.3.9 Nitric Acid, 0.8 N. Dilute 52 ml of concentrated
nitric acid (59 percent HKO^) to exactly 1 liter with daionized
distilled water.
3.3.10 Hydrochloric Acid, Concentrated. ACS grade.
3.3.1"i Stock Arsenic Standard Solution (1 wg As ^^/ml
Dissolve 1.3203 g primary standard grade, Aso0o in 20 ml of 0.1 N
£ O
ftaOK. Neutralize with concentrated nitric acid. Dilute to 1.0
liter with distilled, deionized water.
3.3.12 Arsenic Working Solutions
3.3.12.1 100 pg As Pipet exactly 10.0 ml of stock
arsenic standard solution into sr. acid-cleaned, appropriately labeled
1C0.0 ml volumetric flask. Dilute to the rcark with deionized,
distilled water.
3.3.12.2 10 pg As Pi pot exactly 10.0 ml of stock
arsenic standard solution into an acid-cleancd, appropriately labeled
1.0 liter volumetric flack containing about 500 ml of deionized,,
distilled water and 5 ml of concentrated KNO^. Dilute to the mark
with deionized, distilled water.
3.3.13 Air. Kust be of a quality suitable for atomic absorption
analysis.
3.3.14 Acetylene. Kust be of a quality suitable for atomic
absorption analysis.
3.3.15 Filter. Paper filters, V,'hatir,un i!41 or equivalent.
4. Procedure
-------
11
4.1 Sampling. The complexity of this method is such that,
in order to obtain reliable results, tasters should be trained
and experienced with'the test procedures.
4-J^l Pretest Preparation. All the components shall be
maintained and calibrated according to the procedure described
in APTD-0576, unless otherwise specified herein.
Weigh several 200 to 300 g portions of silica gel in air-tight
containers to the nearest 0.5 g. Record the total weight of the
silica gel plus container, on each container. As an alternative,
the silica gel need not be preweighed, but may be weighed directly
in its impir.ger or sampling holder just prior to train assembly.
Check filters visually against light for irregularities and
flaws or pinhole leaks. Label filters of the proper diameter on
the back side near the edge using numbering machine ink. As an
alternative, label the shipping containers (glass or plastic petri
dishes) and keep the filters in these containers at all times except
during sampling.
4.1.2 Prelirr.inary Determinations. Select the sampling site
and the minimum number of sampling points according to Method 1 or
as specified by the Administrator. Determine the stack pressure,
temperature, and the range of velocity heads using'Method 2; it is
recommended that a leak-check of the pi tot lines (see Method 2, .
Section 3.1) be performed. Determine the moisture content using
Approximation Method 4 or its alternatives for the purpose of making
isokinetic sampling rate settings. Determine the stack gas dry
-------
12
molecular weight, (sc>o Soction 2.1.10) as described in Method 2,
Section 3.5; if,jja£egrated Method 3^sampling is used for molecular
weight determination", the integrated bag sample shall be taken
simultaneously with, and for the same total length of time, as the
arsenic sample run.
Select a nozzle size based on the range of velocity heads, such
that it is not necessary to change the nozzle size in order to
maintain isokinetic sampling rates. During the run, do not change
the nozzle size. Ensure that the proper differential pressure gauge
is chosen for the range of velocity heads encountered (see Section
2.2 of Method 2).
Select a suitable probe liner and probe length such that ell
traverse points can be sampled. For large stacks, consider sampling
from opposite sides of the stack to reduce the length of probes.
Select a total sampling time greater than or equal to the mini-
mum total sampling time specified in the test procedures for the
specific industry such that (1) the sampling time per point is not
less than 2 minutes (or some greater time interval as specified
by the Administrator), and (2) the sample volume taken (corrected
to standard conditions) will exceed the required minimum total gas
sample volume. The latter is 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 minute, in order to
avoid timekeeping errors. The sampling time at each point should be
the same.
-------
In some circumstances, e.g., batch cycles, it may bo neces-
sary to sample for shorter times at the traverse points and to
obtain smaller gas sample volumes. Ir. these cases, the Administra-
tor's approval must first be obtained.
4.1.3 Preparation of Collection Train. During preparation
and assembly of the sampling train, keep all openings where con-
tamination can occur covered until just prior to assembly or until
sampling is about to begin.
„ Place_JL5IUwl-^of water in each of the first two ir.ioingsrs and
200 ml of 10 percent KgOg ^ha third, fourth, and fifth impin-
gers. Weigh and record the weight of each impinger and liquid.
Transfer approximately 200 to 300 g of preweighed silica gel from
its container to the sixth impinger. More silica gel may be used,
but care should be taken to ensure that it is not entrained and
carried out from the impinger during sampling. Place the container
in a clean place for later use in the sample recovery. Alternatively,
the weight of the silica gel plus impinger may be determined to the
nearest 0.5 g and recorded.
Using a tweezer or clean disposable surgical gloves, place a
labeled (identified) filter in the filter holder. Be sure that the
filter is properly centered and the gasket properly placed so as to
prevent the sample gas stream from circumventing the filter. Check
the filter for tears after assembly is completed.
When glass liners are usad, install the selected nozzle using
a Viton A 0-ring when stack temperatures are less than 2oO°C (500°F)
and an asbestos string gasket when temperatures are higher. See
-------
14
APTD-0575 for details. Other connecting systems using either 316
stainless steel or Teflon ferrules may be used. Whan metal liners
are used, install the nozzle as above or by a leak-free direct
mechanical connection. Mark the probe with heat resistant tape
or by some other method to denote the proper distance into the
stack or duct for each sampling point.
Set up the train as in Figure 103-1, using (if necessary)
a very light coat of silicone grease on all ground glass joints,
greasing only the the outer portion (see APTD-0576) to avoid
possibility of contamination by the silicone grease. Subject to
the approval of the Administrator, a glass cyclone may be used
between the probe and filter holder whan the total particulate
catch is expected to exceed 100 mg or when water droplets are
present in the stack gas.
Place crushed ice around the impingers.
4.1.4 Leak-Check Procedures.
4.1.4.1 Pretest leak-Check. A pretest leak-check is recom-
mended, but not required. If the tester opts to conduct the pre-
test leak-check, the following procedure shall be used.
After the sampling train has been assembled, turn on and set
the filter and probe heating systems at the desired operating
temperatures. Allow time for the temperatures to stabilize. If
a Viton A 0-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 330 mm Hg
(15 in. rig) vacuum.
-------
.Note: A lower vacuui mav be used, provided that it is not
exceeded daring the test.
If an asbestos string is used, do not connect the probe to
the train curing tne ieai<-check. Instead, leak-check the train
by first plugging the inlet to the filter holder (cyclone, if
applicable) and pulling a 380 mm Hg (15 in. Hg) vacuum (see
Note ir.madiately above). Then connect the probe to the train
and leak-check at about 25 mm Hg (1 in. Hg) vacuum*, alternatively,
the probe may be leak-checked with the rest of the sampling train,
in one step, at 380 rr,m Hg (15 in. Hg) vacuum. Leakage rates in
3
excess of 4 percent of the average sampling rate or 0.00057 m /rnin
(0.G2 cftn), whichever is less, are unacceptable. ^
The following leak-check instructions for the sampling train
described in APTD-0576 and APTD-0581 may be helpful. Start the
purr.p with bypass valve fully open and coarse adjust valve completely
closed. Partially ooen the coarse adjust valve and slowly close
the bypass valve until the desired vacuum is reached. Do not
reverse direction of bypass valve; this will cause water 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.
When the leak-check is completed, first slowly remove the plug
from the inlet to the probe, filter holder, or cyclone (if applicable)
and iarf.ediately turn off the vacuum pu;ap. This prevents the solutions
in the impingers from being forced backward irito the filter holder
-------
»o
and silica gel from being entrained backward into the fifth
impinger.
4.1.4.2 Leak-Checks During Sample Run. If, during the
sampling run, a component (e.g., filter assembly or impinger)
change becomes necessary, a leak-check shall be conducted
•immediately before the change is made. The leak-check shall
be done according to the procedure outlined in Section 4.1.4.1
above, except that it shall ba done at a vacuum equal to or
greater than the maximum value recorded up to that point in the
test. If the leakage rate is found to be no greater than
q
0.00057 m /min (0.02 cfm) or 4 percent 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 shall either record the leakage rate and plan to
correct the sample volume as shown in Section 6.3 of Method 5,
or shall void the sampling run.
Immediately after component changes, leak-checks are optional;
if such leak-checks are done, the procedure outlined in Section 4.1.4.1
above shall be used.
4.1.4.3 Post-test Leak-Check. A leak-check is mandatory at
the conclusion of each sampling run. The leak-check shall be done
in accordance with the procedures outlined in Section 4.1.4.1,
except that it shall ba^conducted at a vacuum equal to or greater
than the maximum value reached during the sampling run. If the
-------
or 4 percent of the average sanding rate (whichever is less), the
results arc- acceptable, and no correction need L»e applied to the
is obtained, the tester shall either record the leakage rate and
correct the sample volume as shown in Section 6.3 of Method 5, or
sr.nil void the samolir.ci run.
4.1.5 Arsenic Train Operation. During the sampling run, main-
tain ar. isokinetic sampling rate (within 10 percent of true isokine-
tic unless otherwise specified by the Administrator) and a tempera-
Fcr each run, record the data required on a data sheet such as
the one shown in Figure 103-2. Be sure to record the initial dry
gas meter reading. Record the dry gas meter readings at the
beginning and end of each sampling time increment, when changes in
flow rates are made, before and after each leak check, and when
sampling is halted. Take other readings required by Figure 103-2
at least once at each sample point during each time increment and
additional readings when significant changes (20 percent variation
in velocity head readings) necessitate additional adjustments in
flow rate. Level and zero the manometer. Because the manometer
level and zero may drift due to vibrations and temperature changes,
make periodic checks during the traverse.
Clean the portholes prior to the test run to minimize the
chance of sampling deposited material. To begin sampling, remove
total volume of dry gas metered. If, however, a higher leakage rate
ture range around the filter
r of 110-135°C
-------
I ..iV'T
IDCATlC'J
OPERATOR
_ DATE
nu^No
¦SA.V.PLE EOX i\0..
meter eoxNo._
f.'ETER AHp
C FACTOR.
flTOT TUSE COEFFlCIENT.Cn
SCHEMATIC OF STACK CROSS SECTION
AMSiEHT TE-VPCRAIURE,
tAROMETRiC PRESSURE.
ASSUMED,V.G!STUP.E.%_
PROBE LE.'i'CTH.n (ft]
fcOZZLE IDENTIFICATION NO..
AVERAGE CALIBRATED NOZZLE DIAMETER, cm (in.].
THOSE HEATER SETTING.
LEAK PATE. " "
PROBE LINER MATERIAL ' " " '
STATIC PRESSURE . nvn Hg [in.Hgi,
FILTER no:
traverse point
WUM2ER
SAMPLING
TIME.
(f). run.
vacuum"*
. mm fig
{in -Hg)
stack'
Tcf.'PtKATUSE
*C (°fj
•\
VELOCITY
HEAD
(APS).
S " PRESSURE
i DIFFERENTIAL
-ACROSS
ORIFICE
METE."
ir/n HjO
\in. J
GAS SA.VPLE
• VOIU.VE
GAS SAWPl E TEMPERATURE
AT DP.V GAS METER
FILTER HOLDER
TEMPERATURE.
°C (eFI
"¦TEMPERATURE
¦ OF GAS
LEAVING
CONDENSER OR
LAST IVPINGER.
°C (efl
INLET
°C (eFI
OUTLET
°C {°F)
r
•
. ;
1
.... '
-
*
• • *
. «. .
-
t
•
¦
'
. •
i
• •
'
:
•- ¦»
w , V
•
.' *. •"*
, '
*.
. .
•
TOTAL
Avg,
Avg.
» *
average
Avg.
Figure 108-2. Arsenic field data
-------
the nGzzle cap, verify that the filter ar.d probe heating systems
are up to temperature, and that the pitot tube and probe are
properly positioned. Position the nozzle at the first traverse
point with the tip pointing directly into the gas stream.
Immediately start the pump and adjust the flow to isokinetic con-
ditions. Nomographs are available, which aid in the rapid adjust-
ment of the isokinetic sampling rate without excessive computations.
These nomographs are designed for use when the Type S pitot tube
coefficient is 0.85 +_0.02, and the stack gas equivalent density
(dry molecular weight) is equal to 29 +4. APTD-0576 details the
procedure for using the nomographs. If Cp end are outside the
above stated ranges, do not use the nomographs unless appropriate
steps (see Citation 7 in Section 7) are taken to compensate for the
deviations.
Whan the stack is under significant negative pressure (height
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, the pump may be turned on
with the coarse adjust valve closed.
When the probe is in position, block off the openings around
the probe and porthole to prevent unrepresentative dilution of
the gas stream.
Traverse the stack cross-section, as required by Method 1 or
as specified by the Administrator, being careful not to bump the probe
nozzle into the stack walls when sampling near the walls or when
-------
20
removing or inserting the probe through the portholes; this
mizes the change of extracting deposited material.
During the test run, make periodic adjustments to keep the
temperature around the filter holder at the proper level; add
more ice and, if necessary, salt to maintain a temperature of less
than 20°C (68°F) at the condenser/silica gel outlet. Also,
periodically check the level and zero of the manometer.
If the pressure drop across the filter becomes too high,
making ispkinetic sampling difficult to maintain, the filter may
be replaced in the midst of a sample run. It is recommended that
another complete filter assembly be used rather than attempting
to change the filter itself. Before a new filter assembly is
installed,- conduct a leak-check (see Section 4.1.4.2).
A single train shall be used for the entire sample run, except
in cases where simultaneous sampling is required in two or more
separate ducts or at two or more different locations within the
same'duct, or, in cases where equipment failure necessitates a
change of trains. -In all other situations, the use of two or
mora trains will be subject to the approval of the Administrator.
Note that when tv/o or more trains are used, separate analyses
of the sample fractions from each train shall be performed unless
otherwise specified by the Administrator. Consult with the .
Administrator for details. concerning the calculation of results
when tv/o or more trains are used.
At the end of the sample run, turn off the coarse adjust valve,
-------
21
remove the probe and nozzle from the stack, turn off the pump,
4..
record the final dry gas mater reading, and conduct a post-tes-
leak-check, as outlined in Section 4.1.4.3. Also* leak-check
the pi tot lines as described in Method 2, Section 3.1; the lines ;> rt~f\jD
must pass this leak-check, in order to validate "the velocity ni i$~s
-------
22
from the filter inlet where the probe.was fastened and cap it.
Remove the umbilical cord from the last impinger and cap the impinger.
If a flexible line is used between the first impinger and the filter
holder, disconnect the line at the filter holder and let any condensed
water or liquid drain into the impingers. After wipinq off the sili-
cone grease, cap off the filter holder out.lpt. and impinger inlet.
Either ground-glass stoppers, plastic caps,"or serum caps may be used
to close these openings.
Transfer the probe snd filter-impinger assembly to the cleanup
area. This area should be clean and protected from the wind so that
the chances of contaminating or losing the sample' wiVl be minimized.
Save a. portion of the 0,1. Na.0H used for cleanup as a blank. Take
200 ml of'this solution directly from the wash bottle being uspd aprf
* •
^lace it in a plastic sample container labeled "NaOH blank." Also
save a sample of the distilled deionized water and place it in a
sample container labeled ''tioO^lan^!
Inspect the tra_in prior to and during disassembly and note any
abnormal conditions. Treat the samples as follows:
Container No. 1. Carefully remove the filter from the filter
* 1 1
holder and place it in its identified petri dish container. Use
a pair of tweezers and/or clean disposable surgical gloves to
handle the filter. If it is necessary to fold the filter, do so
such that the particulate,cake is inside the fold. Carefully trans-
fer to the petri dish.any particulate matter and/or filter fibers
:/hich adhere to the filter holder gasket, by using a dry Nylon
jristle brush and/or a sharp-edged blade. Seal the container.
-------
23
Container No. 2. Taking care to see that dust on the out-
side of the probe or other..exterior surfaces does not get into
the sample, quantitatively recover particulate matter or any
condensate from the probe nozzle, probe fitting, probe liner,
and front half of the filter holder by washing these components
¦ —^ .
with 0.1 N NaOHjand placing the wash in a glass container. Mea-
sure^ and record to the nearest ml the total volume of solution
jn container No. 2. Perform-the rinsing as follows:
Carefully remove the probe nozzle and clean-the inside sur-
face by rinsing with 0.1 N NaOH from a wash bottle and brushing
with a Nylon bristle brush. Brush until the "rinse shows no '
visible particles,- after which make a final rinse of the inside
surface with 0.1 N NaOH.
Brush and rinse the inside parts of the Swage!ok fitting
with 0.1- N NaOH in a similar way until no visible particles remain.
Rinse the probe 1 ir.er__wjjLb—P. 1 N NaOH by tilting and rotating
the probe while squirting 0.1 N NaOH into its upper end so that
all inside surfaces will be watted with the rinse solution. Let
the 0.1 N NaOH drain from the lower end into the sample container.
A funnel (glass or polyethylene) may be used to aid in transferring
liquid washes to the container. Follow the 0.1 N NaOH rinse with
a probe brush'. Hold the probe in an inclined position, squirt 0.1 N
NaOH into the upper enu as the probe brush is being pushed with a
twisting action through the probe; holtf'a. sample container under-
neath the lower end of the probe, and catch any liquid and
T
Brand name.
-------
24
particulate matter which is brushed from the probe. Run th.
•brush through the probe three times or more until no visible
particulate matter is carried out with the rinse or until none
remains in the probe liner on visual inspection. With stainless
steel or other metal probes, run the brush through in the above
prescribed manner at least six times since metal probes have
small crevices in which particulate matter can be entrapped.
Rinse the brush with ,0.1 N NaOH, and quantitatively collect
these washings in the sample container. After the brushing,
make a final Q.l N NaOH rinse of the probe as described above.
It is recommended that two people be- used to clean the probe
to minimize sample losses. Between sampling runs, keep brushes
clean and protected from contamination.
After ensuring that all joints have been wiped clean of
silicone grease, clean the inside of the front half of the
filter holder by rubbing the surfaces with a Nylon bristle brush
and rinsing with 0.1 N NaOH. Rinse each surface three times or'
more if needed to remove visible particulate. Make a tinal'rinse
of the brush and filter holder. Carefully rinse out the glass
cyclone, also (if applicable). After all washings and particu-
late matter'have been collected in the sample container, tighten
the lid on the sample container so that liquid will not leak out
when it is shipped to the laboratory. Mark the height of the
fluid level to determine"whether or not leakage occurred during
transport. Label the container to clearly identify its contents.
-------
Rinse the glassware a final time with rir>inni7r-ri, distilled
water to remove residual.NaOft before reassembling. Do not save
the watpr-
Container No. 3. Note the color of the indicating silica
gel to determine if it has been completely sperct and make a nota-
tion of its condition. Transfer the silica oel from the sixth
impinger to its original container and seal. A funnel may make
it easier to pour'the silica gel without spilling. A rubber
policeman may be used as an aid in removing the silica gel from
the impinger. It is not necessary to remnv? the small amount.of
dust particles that way adhere to the impinqer wall and arie dif-
ficult to remove. Since the gain in weight is to be used for
moisture calculations, do not use any water" or other liquids to
transter "ens sinca gei. If a balance is available in'the'
field,- follow the procedure for Container No. 3 fn Section 4.3.
Container No. 4. Transfer the contents of impingers 1 and
2 to this container. Clean each of the first two impingers and .
connecting glassware in the following manner:
1. Wipe the impinger ball joints free of silicone grease
and cap the joints.
2. Rotate and agitate each impinger, so that the impinger
contents might serve as a rinse solution.
3. Transfer the contents of the impingers to a graduated
cylinder. The outlet ball joint cap "Should be removed and the
contents drained through this opening. The impinger parts (inner
and outer tubes) must not be separated while transferring their
-------
contents to the cylinder.
Welsh' the impinger and liquid to within + 1.0 g. The v/eight
of "liquid present along with a notation of any color or film
observed in the impinger catch is recorded in the log. This in-
formation is needed along with the silica gel data to calculate
the stack gas moisture content.
4. Transfer the contents of the first two imoinners to
Container No. 4.
5. ^Pour approximately 30 ml of 0.1 N NaOH into each of the
first two impingers and apitate the impingers.^ Drain the 0.1 N
NaOH,through the outlet arm of each impinger into the No; 4. sam-
ple container. Repeat this operation a second time; inspect tne
impingers for any abnormal conditions.
6. Wipe"..the ball joints of the glassware connecting the
impingers and the back half of the filter'holder free of silicone
grease and rinse each piece of glassware twice with 0.1 N NaOH;
this rinse is collected in Container No. 4. (Do not rinse
or brush the glass-frit'ted filter support.)
Mark the height of the fluid level to determine whether
leakage occurred during transport. Label the container to clearly
identify.its contents.
Container No. 5. Due to the large quantity of liquid
involved, the impinger solutions may be placed in
separate containers. However, they may be combined at the
Note: In steps 5 and 6 above, the total amount of 0.1 N
NaOH used for rinsinci must be measured and recorded.
-------
tit'.!2 ov analysis in order to reds;ce tNc ,...«\bzr of an-
•required. Clean the iir.pir.qers according to the six-step pro-
cedure described under Container Mo. 4- using deionized, dis-
ti 11 ed water instead of 0.1 OaQK.as the r1nsing lifjuid.
4.3 Analysis.
4.3.1 Container No. 3. This step may be conducted in
the field. Weigh the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 gram; record this weight.
4.3.2 Arsenic Sample Preparation and Analysis.
4.3.2.1 Container No. 1 (Filter). Place the filter and
loose particulate matter in a 150 ml beaker. Also add the .filtered
material from container No. 2. (see Sect i ui| 4.3.2.3). Add
50 ml 0.1 N NaOH, stir and warm for about 15 minutes. Add 10 ml
of concentrated HNO,, bring to a boil, thert" simmer for about
15 minutes. Filter the solution through a Whatman #41 filter
paper and wash with hot ..water, catching the filtrate in a clean
150 ml beaker. Bring the filtrate to boiling and evaporate to
dryness. Cool, add 5 ml of'1:1 (v/v) HNOg and then warm and
stir. Allow to cool, and transfer to a 50 ml volumetric flask;
dilute to volume with.deionized, distilled water and mix well.
Any undissolved solids retained by the filter must be fur-
ther treated to dissolve them. Place the filter in a PARR acid
digestion borib and add 5 ml each of concentrated nitric and
hydrofluoric acids. Seal the bomb and heat it in an oven at
-------
"i50°C for 5 hours.
Remove the bomb from the oven ancl allow it to cool.
Quantitatively transfer the contents of the bomb to a 50 ml
polypropylene volumetric flask and di'lute to exactly 50 ml
with deionized distilled water.
4.3.2.2 Container No. 4 (Impinger Samples). Transfer the
contents of container No. 4 to a 500 ml volumetric flask and
dilute to exactly 500 ml with deionized, distilled water. Pipet
50 ml of the solution into a 150 ml beaker. Add 10 ml of con-
centrated HNO^.' bring to a boil ar.d evaporate nearly to dryness
(approximately 1 ml). Allow to cool, add 5 ml of 1 :T (v/v)
¦{i\03 and then warm and stir. Allow the solution. to cool, trans-
fer to a 50 ml volumetric flask, dilute to volume with deionized,
iistilled water and mix well.
L3.2.3 Container No. 2 (Probe Wash).* Filter the contents
)f container No. 2 into a 200 ml volumetric flask. Dilute the
filtrate to exactly 200 ml with deionized, distilled v/ater. Coi;i-
)ine the filtered material with the contents of Container No. 1.
Pipet 50 ml of the diluted filtrate into a 150 ml beaker,
vdd 10 ml of concentrated HNO^, bring to a boil and evaporate
learly to dryness (approximately 1 ml). Allow to cool, add
» ml of 1:1 (v/v) HN03 and then warm and stir. Allow the solu-
;ion to cool, transfer to a 50 ml volumetric flask, dilute to
oluma with deionized, distilled v/ater and mix well.
Note: Prior to analysis, the liquid level in container No. 2
-------
/or Mo. 4 shall beN checked; confirmation is to whether or not
.leakage occurred during transport shall be made or. the analysis ,
sheet. If a noticeable amount of leakage has occurred, either void
the sample or take steps, subject to the approval* of the administra-
tor, to correct the final results.
4.3.2.4 Filter Blank. Determine a filter blank using two
filters from each lot of filters used in the sampling train. Cut
each filter into strips and. treat each filter individually as
directed in Section 4.3.2.1.
4.3.2.5 0.1 N NaOH Blank. Treat 50 ml of 0.1 N NaOH as
directed beginning with sentence two of Section 4.3.2.2.
4.3.2.6 Water 31ar.k. Treat 50 ml of-the deionized, distilled
water blank as directed beginning with sentence 2 of Section 4.-3.2.2.
4.3.2.7 Spectrophotometer Preparation.' Turn on the power,
set the wavelength,' slit width, lamp current, and adjust the back-
ground corrector as instructed by the manufacturer's manual for
the particular atomic absorption spectrophotometer. Adjust the
burner and flame characteristics as necessary.
4.3.2.8 Arsenic Determination. After the absorbance values
have been obtained for the standard solutions (Section 5), determine
the absorbances of the filter blank and each sample against the
0.8 N H:\'0_j If the sample concentration falls above the limits
of the curve, make an appropriate dilution with 0.8 N HN03, such
that the final concentration fall's within the range of the curve.
»
Determine the arsenic concentration in the filter blank (i.e., the
-------
average of tr.e two blank values fro.v, .each lot). Next, u
appropriate standard curve, determine the arsenic conce . ...on
in each sample fraction.
4.3.2.9 Arsenic Determination at Low Concentration. Flame
atomic absorption spectrophotometry is a very good analytical
method for arsenic concentrations as low as 10 mg/1. If it is
necessary to determine quantities of arsenic at a lower level,
.the vapor generator, available as an accessory component to an
atomic absorption spectrophotometer, must be used. Manufac-
. turer's instructions should be followed in the use of such equip-
ment. A sample containing between 0 and 5 pg of As should be,
placed in the reaction tube and diluted to 15 ml'with deionized.
distilled water. There is some trial and error involved in this
so that 'it may be necessary to screen the samples until an approxi-
mate concentration is determined. After determining the approxi-
mate concentration, the volume of the sample'can be adjusted
accordingly. Pipet 15 ml of concentrated HC1 into each.tube.
Add 1 ml of 30 percent KI solution. Place the reaction tube
into a 50°C water bath for 5 minutes. Cool to room temperature.
Connect the reaction tube to the vapor generator assembly. When
the instrument response has returned to baseline, inject o.u mj- or
sodium borohydride solution and integrate the resulting spectro-
photometer signal over a 30 second time period.
4.3.2.10 Mandatory Check for Matrix Effects on the Arsenic
Results. The analysis for arsenic by atomic absorption is sensi-
tive to the chemical composition and to the physical properties
-------
(viscosity, pH) of the sample (i&utrix effects). S. >rseoic
procedure described..ht\re will be applied to many different "sources,
it can be anticipated that many different sample matrices will be
encountered. Thus, it is mandatory that at least one sample from
each source be chocked using the "Method of Additions" to ascertain
that the chemical composition and physical properties of the sample
did not cause erroneous analytical results.
Three acceptable "Method of Additions" procedures are described
in the General Procedure Section of the Perkin Elmer Corporation
Manual (Citation 10 in Section 7). If the results of the Method
of Additions procedure on the source sample do not agree to within
5 percent of the value obtained by the'conventional atomic absorp-
tion analysis, then all samples from the-source must be reanalyzed
using the Method of Additions procedure.
4A Analysis for SO,,. Note level of liquid in Container 5
r
and confirm whether any sample was lost during shipping; note this
on analytical data sheet. If a noticeable amount of leakage has
occurred, either void the sample or use methods, subject to the
a}.r. _val of the Administrator, to correct the final results.
Transfer the contents of the Container(s) No. 5 to a 1 liter
volumetric flask and dilute to exactly 1 liter with deionized,
distilled water. Pipette a 10 ml aliquot of this solution into
a 250 ml Erlenmeyer flask and add two to four drops of phenolphtha-
lein indicator. Titrate the sampVe to a faint pink endpoint using
1 N NaOH. Repeat and average the titration volumes. Run a blank
with each series of samples.
-------
5. Calibration
Maintain a laboratory log of all calibrations.
5.1 Standard Solutions. Determine the absorbance of the
standards against a reagent blank of 0.8 N MNOj.
Standards for the normal flame procedure are prepared by
III
pipeting 1, 3, 5, 8 and 10 ml aliquots of the 100 pg As Vml
standard solution into separate 100 ml volumetric flasks, each
containing 5 ml of concentrated HNO^. Dilute to the mark with
deionized distilled water.
Standards- for the low level procedure are prepared by
pipeting 1, 2, 3, 4, and 5 ml aliquots of. 1.0 pg As*.**/ml standard
solution into separate reaction tubes. These are then treated
in the same manner as the samples, (Sec. 4.3.2.8).
These absorbances should be checked frequently during the
analysis to insure that baseline drift has. not occurred. Prepare
a standard curve of absorbance versus concentration. (Note: For
instruments equipped with direct concentration readout devices,,
preparation of a standard "curve v/ill not be necessary.) In all
cases, the manufacturer's instruction manual should be consulted
for proper calibration and operational procedures.
5.2 Sampling Train Calibration. Calibrate the satr.pl ir.q
train components'according to the indicated sections of Method 5;
probe nozzle (Section 5.1); pitot tube assembly (Section 5.2);
metering system (Section 5.3); probe heater (Section 5.4);
temperature gauges (Section 5.5)v, barometer (Section 5.7). Note
that the leak check of the metering system (Section 5.6) applies
to this method.
-------
5.3 1 N Sidum Hydroxide; Solution. Standardize the; sodium
hydroxide titrant against..25 ml of standard sulfuric acid.
6. Calculations
6.1 Nomenclature
2 2
An = Cross sectional area of nozzle,, m (ft )
B = Water in the gas stream, proportion by volume.
C3 = Concentration of arsenic as read from the standard
a
curve, ng/ml.
C$o = Concentration of sulfur dioxide, % volume.
C$ = Arsenic concentration in stack gas, dry basis,
converted to standard conditions, g/dscm (jg/dscf).
E„ ='Arsenic mass emission rate* g/hr.
= Dilution factor « 1 if the''sample has not been
diluted.
I = Percent of isokinetic sampling
= Maximum acceptable leakage rate for either a pre-
test leak check or for a leak check following a
1 O
component change; equal to 0.0057 m /min (0.02 CFM)
or 4 percent of the average sampling rate, which-
ever is less.
= Individual leakage rate observed during the leak
;check conducted prior to the "ith" component
3
change (i = 1, 2, 3, ...N), m /min (CFM).
Lp = Leakage rate observed^'during the post-test leak
check, m^/min (CFM).
= Total mass of all six Impingers and contents before
sampling, g.
-------
- Total mass of all six impingers and contents
after sampling, g
- Total mass of arsenic collected in a specific
part of the sampling train, pg.
= Mass of SO^ collected in the sampling train* g.
Mt = Total mass of arsenic collected in the sampling
train, ug.
Mw Molecular weight of water, 18.0 g/g-mole
(18.0 Ib/lb-mole)
N . = Normality of sodium hydroxide titrant, mg/ml.
P. = Barometric pressure of the sampling site,
bsr
mm Hg (in Hg).
P = Absolute stack gas pressure, mm Hg (in Hq).
s
Pstd = Standard absolute pressure, 760 mm Hg (29.92
in Hg).
R = Ideal gas constant, 0.06236 mm Hg-m^K-g-mole
(21.85 in Hg - ft3/Vlb-mole).
••= Absolute average dry gas meter temperature
(see Figure 100-2). °K(°R).
T = Absolute stack gas temperature (see Figure 108-2).
"Tstd ^Standard absolute temperature, 293°K (528°R).
V ' = Volume of sample aliquot titrated.
d
Vm = Volume of gas sample as measured bv the dry gas
meter, dcm(dcf).
V s Volume of gas sample as measured by the dry gas
(std) .
meter collected to standard conditions SCM, (SCF)
Vs = Stack gas velocity, calculated by Method 2,
Equation 2.9, using data obtained from Method 108,
jU/se? (ft/sec)-.
-------
35
V ^ = Total solution volume for any specific p^rt.
of the sample train, ml.
V ¦, c Total volume of solutiorl in which the sulfur
soln
dioxide is contained, 1 liter.
V$q 83 Volume of SC^ collected in the sampling train,
DSCM (SCF).
Vt ° Volume of sodium hydroxide titrant used for
the sample, ml (average of replicate titrations).
Vtb 85 Volume of sodium hydroxide used for the blank, ml.
V^0^. = Volume of gas sampled corrected to standard con-
ditions, DSCM, (DSCF).
\(std) = ^°^ume wa^er vapor collected in the sampling
train, corrected :'to standard conditions, SCM(SCF).
V » Dry gas meter calibration factor.
aH » Average pressure differential across the orifice
meter (see Figure 1-8-a), mm H20 (in HgO).
Pw = Density of water, 0.9982 g/ml (0.00220/lb/ml).
g = Total sampling time, min.
G-j = Sampling time interval, from the beginning of a
run until the first component change, rivin.
O. = Sampling time interval, between two successive
component changes, beginning with the interval
between -the t?rst arK* second changes, min. .
B.6 ¦= Specific gravity of mercury.
60 = Sec/min.
100 = Conversion to percent.
6.2 Calculate the volume of sulfur dioxide gas collected
by the sampling train.
-------
36
VS02 - K, (Vt -,Vtb) N ,(Vsoln/Va)
108-1
Where:
K-j = 1.203 x 10"5 m3/maq, for metric units
K, « 4.248 x 10~C ft^/meq. fnr English units
.6.3 Calculate the sulfur dioxide concentration in the
stack gas (dry basis adjusted to standard conditions)
ac •fnnows:
6.4 Calculate the mass of sulfur dioxide collected by the
sampling train.
6.5 -Average dry gas meter temperature and average orifice
pressure drop. See data sheet (Figure 10S-2).
6.6 Dry Gas Volume. Correct the sample volume measured
by the dry gas meter to standard conditions (20°C,
760 mm Hg or 68°F, 29.92 in Hg) and add the.volume of
collected sulfur dioxide.
X 100 108-2
32 ms/meg (Vt - Vtb) N (Vsoln/Vn) 108-3
-------
37
+ VSq Equation 108-4
»
+ V
SO.
2
lOj = 0.3858°K/(rw Hg for metric units
c 17.64° R/in Hg for English units
Note: Equation 108-4 can be used as written unless the
leakage,rate observed during any.of the mandatory leak
checks (i.e. post test leak checu or leak checks prior
to component changes exceeds L. 'If L or L. exceeds
G pi
• , equation 108-4 must be modified as follows:
(a) Case I. Wo component changes made during
sampling run. In this case, replace in equation 108-4
by the expression:
(b) Case II. One or more component changes made
dur.ing the sampling run. In this case, replace in
Equation 108-4 by the expression.
n
[V„ - (Ln - LJ e]
1 m 1 p a
lwm Vlrl a' 1 i=2 ^i ua'ui W
and substitute only for-those leakage rates(L^ or Lp)
which exceeds L .
-------
33
6.7 Volume of water vaQor.
"w(std) ' v"fi "bi "S02) ~pS'*^M Equation 108-5
c std %
Where:
Kj » 0.001333 m3/ml tor "letHc un1ts
" 0.04707 ft3/ml for English units
6.8 Moisture content
" vv"-^«td) Equat1on ,08-6
•6.9 Amount of'Arsenic Collected
6.9.1 Calculate the amount of arsenic collected in each
part of the sampling train, as follows:
Kn " Ca Fd Vsol„
6.9.2 Calculate the total amount of arsenic collected in
the sampling train as follows:
Kt * Mn(f?1ter) +Mn(probe) + Kn(1mp1ngers) - Mn(filter blank}"- «n(NaOH)-Mr(HgO)
6.10 Calculate the arsenic concentration in the stack gas
(dry basis, adjusted to standard conditions) as follows:
cs c (1 x 10 g/ng) Equation 108-7
-------
39
6.11 Pollutant Kass Rate. Calculate the arsenic mass emission
rate using the following equation.
= CsQscj Equation 108-8
The volumetric flow rate, Q^, should be calculated
as indicated in Method 2.
6.12 Conversion Factors.
From To Multiply by
scf m3 0.02832
S/ft3 gr/ft3 15.43
9/ft3 lb/ft3 2.205 x 10"*3
g/ft3 g/m3'- 35.31
6.13 Isokinetic Variation
Ts Vtot p— 100
1' EsuaWon 10M
T V
_ „ s tot
4 P" V A 0 U-b )
s s n v ws'
Where: = 4.320 for metric units
» 0.09450 for English units
6.14 Acceptable Results. If 90 percent <_ I 5.110 percent,
the results are acceptable.... If the results are low in
comparison to the standard and I Is beyond the acceptable
-------
40
range, or 1f I is less than SO percent the Administrator
may opt' to accept the results. Use Citation 4 to make
judgements. Otherwise, reject the results and repeat the
test.
Bibliography
1. Addendum to Specifications for Incinerator Testing
at. Federal Facilities. PHS, NCAPC; Dec. 6, 1967.
2. Martin, Robert M. Construction Details of Isokinetic
Source-Sampling Equipment. Environmental Protection Agency,
Research Triangle Park, N. C. APTD-0581. April, 1971.
3. Rom, Jerome J. Maintenance, Calibration, and Opera-
tion of Isokinetic Spurce Sampling Equipment. Environmental
Protection Agency. Research Triangle Park, N. C. APTD-0576.
March, 1972.
4. Smith, W. S., R. T. Shigehara, and W. F. Todd. A
Method of Interpreting Stack Sampling Data. Paper Presented
at the 63rd, Annual .fleeting of the Air Pollution Control
Association, St. Louis, Mo. June 14-19, 1970.
5. Smith, W. 5., et al. Stack Gas Sampling Improved and
Simplified With New Equipment. APCA Paper No. 67-119. 1967.
6. Specifications for Incinerator Testing at Federal
Facilities. PHS, NCAPC. 1967.
7. Shigehara, R. T. Adjustments in the EPA Nomograph for
Different Pi tot Tube Coefficients and Dry Molecular Weights.
Stack Sampling New 2:4-11. October, 1974.
-------
41
8. Vollaro,.fU.F., A Survey of Cohere laity Available:
Instrumentation for the Measurement of Low-Range Gas Velocites,
U. S. Environmental Protection Agency, Emission Measurement
Branch. Research Triangle Park, N. C. November, 1976 (unpublished
paper).
9. Annual.Book of ASTM Standards. Part 26. Gaseous Fuels;
Coal and Coke; Atmospheric Analysis. American Society for
Testing and Materials. Philadelphia, Pa. 1974. pp. 617-622.
10. Analytical Methods for Atomic Absorption Spectrophoto-
metry. Perkin Elmer Corporation. Norwalk. Connecticut.
September, 1976.
11. Annual Book of ASTM btandartfs, part 31; Water,
Atmospheric Analysis. American Society for Testing and Materials.
Philadelphia. Pa. 1974. pp. 40-42.
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/?iTc?r
ii ¦ ..I. - ^
united states district COURT
WESTERN DISTRICT OF NEW YORK
DONNER HANNA COKE CORPORATION
Plaintiff
-vs-
Civ-77-232
DOUGLAS M. COSTLE, Administrator of
the United States Environmental
Protection Agency,
Defendant
APPEARANCES: HODGSON, RUSS, ANDREWS, WOODS & GOODYEAR
(STEPHEN H. KELLY, ESQ. and ROBERT B.
CONKLIN, ESQ., of Counsel), Buffalo, New
York, for the Plaintiff.
RICHARD J. ARCARA, ESQ., United States
Attorney (JAMES A. FRONK, ESQ., Special
Assistant to united States Attorney,
Buffalo, New York; WALTER E. MUGDAN, ESQ.
& STEPHEN A. DVORKIN, ESQ., United States
Environmental Protection Agency, New York,
New York; and DOUG FARNSWORTH, ESQ.,
United States Environmental protection
Agency, Washington, D. C., OF COUNSEL),
for the Defendant.
In this action, the plaintiff seeks judicial
review of an administrative order issued by the Adminis-
trator of the Environmental Protection Agency [EPA] di-
recting the plaintiff to permit EPA to inspect the
plaintiff's coko oven batteries. The EPA has counter-
claimed for enforcement of its order of inspection. The
*
-------
-2-4 V>
case was tried before the court, what follows is the
court's findings of fact and conclusions of law, made
in accordance with Rule 52 of the Federal Rules of Civil
Procedure.
I. BACKGROUND
Donner Hanna is a New York corporation engaged
in the business of operating a by-product coke plant, its
coke oven batteries are located in Buffalo, New York, a
short distance inland from Lake Erie. its three batteries
are in line, running west southwest to east northeast. Bat-
tery A-B is the westernmost battery, battery #3 is immed-
iately east of battery A-B, and battery #4 is immediately
east of battery #3. The batteries are black in color and
are exposed to wind, sun, snow, and rain.
Each battery consists of approximately 50 ovens
measuring about 17 inches wide, 13 feet high, and 32 feet
long. Between each oven are heating ducts which permit
the heating of a special mixture of coal in the absence of
oxygen to very high temperatures (about 2000°) to produce
coke. The operation of each oven is cyclical and is per-
formed in established regular order throughout the'battery.
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-3-
On top of each battery is a larry car, which
operates on rails ary3 carries coal from a storage facil-
ity to the individual oven. The coal is discharged from
the larry car into the oven to be "charged" through lid-
ded openings in the top of the oven. After the individ-
ual oven is charged, the lids are replaced and the
volatile components of the coal driven off by the heating
process are removed by a "standpipe" to a "collector
main" to a by-product recovery plant.
When the coking cycle is completed (16-17 hours),
the coal in the oven has been transformed into coke. At
that time the doors on each end of the oven are opened and
a ram-like device is inserted from the "pusher side" in or-
der to push the coke out the other end ("coke side") into
a railroad car. The railroad car carries the hot coke un-
der a "quench towar" where the hot coke is drenched with
water.
coke oven batteries do not continuously discharge
smoko into the atmosphere but rather emit smoke for short
periods of time from a lar.je number of discrete sources.
Vh'-y 'ire therefore class!f L^d ft a intermittent sources of
a.ir pollution.
*
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-4-
When the damp coal is charged into the hot oven
from the larry car, emissions may occur at the charging
holes, the larry car hoppers, the larry car control sys-
tem, and the standpipe lid. This group of emissions is
referred to as "charging emissions" and can be reduced
or eliminated by carefully controlling the sequence of
charging and creating a negative pressure in the oven
with an aspiration system. Another group of emissions
may occur at the doors, lids and standpipes located at
each end of the oven when the volatile components of the
coal are removed from the oven after charging. A third
group of emissions may occur during the pushing operation.
and is caused by burning coal which has not been completely
converted to coke at the time that it is pushed out of the
oven. Finally, if there are defects or leaks in the oven
walls, volatile materials may escape into the heating ducts,
causing emissions from the waste heat stack. Charging and
pushing emissions are typically of very short duration and
rarely exceed six minutes.
As a result of a state inspection in 1974 indi-
cating that battery A-n was not in compliance with the
three-minute rule, Donner Hanna improved its pushing emis—
I
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-5-
sion controls on battery A-B. At trial, testimony v/as
introduced to the effect that Donrier Hanna now uses
state of the art pollution control technology on all of
its operations and is in good condition compared to other
coke plants in the United States. Barnes at 452, 454-56.
This testimony was not challenged by EPA.
In September of 1976, EPA attempted to inspect
Donner Hanna*s coke oven batteries for the purpose of de-
termining compliance with emission standards contained in
New York's State Implementation Plan [SIP], 6 N.Y.C.R.R.
§214.3. Donner Hanna refused to allow the inspection be-
cause it disputed the reliability of the testing method
which EPA proposed to use. This testing method is the
focal point of the controversy between the parties.
Under the Clean Air Act, EPA is authorized to
inspect sources of air pollution to determine compliance
1/
with the Act. 42 U.S.C. §7414(a)(2)(A). It is also
authorized to order compliance %^ith its inspection re-
quests. Id. §7413 (a) (3). On October 1, 3.976, EPA xsauad
cin order pursuant to its statutory povars directing Donner
Hanna to a]low the proposed inspection." At that tine and
on all later occasions pertinent to this litigation, E?A
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-6-
has made clear that it intended to conduct the proposed
inspection in accordance with the testing procedures set
forth in "EPA Visible Emission Inspection Procedures
(August 1975)" (1975 EPA Guidelines)(Ex. 2), and that it
would use the "stopwatch" technique of measuring the dura-
tion of emissions. See EPA's Counterclaim 519; Ogg at 23-
32.
After a conference pursuant to 42 U.S.c.
§7413 (a) (4) proved unsuccessful, Donner Hanna filed an
action in this court seeking judicial review of the October
1, 1976 order. Donner Hanna v. Costie. Civ. NO. 76-567.
This action was discontinued without prejudice when EPA
withdrew its October 1, 1976 order.
On April 12, 1977, EPA issued a new order substan-
tially restating the provisions of the order of October 1,
1976.
On May 23, 1977, a conference hearing was held
in the EPA Region II offices, and representatives of Donner
Hanna and EPA attended. At the hearing, EPA refused to
modify the order of April 12, 1977. it also advised Donner
Hanna that EPA intended to seek criminal sanctions against
the plaintiff and its officers and employees in the event
I
-------
2/
of noncompliance with the order.
Immediately thereafter, Donner Hanna filed this
action in the district court, seeking a declaratory judg-
ment as to the constitutionality of the proposed inspec-
tion under the fourth amendment and judicial review of the
April 12, 1977 order under the Administrative Procedure
Act. EPA answered the complaint and also asserted a coun-
terclaim pursuant to 42 U.S.C. §7413(b) seeking a mandatory
injunction directing the plaintiff to grant access to its
plant. EPA's motion for summary judgment was denied and
the case proceeded to trial.
II. JURISDICTION AND SCOPE OF REVIEW
Jurisdiction over the complaint and the counter-
claim is alleged under 28 U.S.C. §§1331, 1345, and 2201;
5 U.S.C. §702; and 42 U.S.C. §7413 (b). Although EPA origi-
nally objected to the court's jurisdiction to grant the re-
lief requested by Donner Hanna, this objection was withdrawn
in open court in order to have this court rule on the testing
method. In turn, Donner Hanrui withdrew its objection to tho
inspection based on the fourth amendment. The only issue
now before the court is the validity of the April 12, 1977
order seeking inspection o[ the plaintiff's coke oven
-------
batteries.
Although the parties now agree that the court
has jurisdiction to review EPA's order, the court recog-
nizes its obligation to engage in an independent inquiry
into subject matter jurisdiction. For the reasons stated
below, 1 find that the district court has jurisdiction
over EPA's counterclaim under 42 U.S.C. §7413 (b) and that
this jurisdiction includes the power to decide whether
EPA's proposed testing method is subject to rulemaking
1/
requirements.
As previously mentioned, the Clean Air Act gives
EPA the power to enter onto the premises of persons opera-
ting emission sources and to sample the emissions in order
to determine compliance with emission standards. Id.
§7414(a) (2). Where permission to inspect is denied, the
EPA "may issue an order requiring such person to comply"
with the inspection request. _Id. §7413 (a) (3). if the per
son "violates or fails or refuses to comply with any order
issued under (§7414 (a) 1," KP.\ may cogence a .civil action
for a permanent or temporary injunction "in the district
court of the united States for the district in which the
violation occurred or in which the defendant resides or ha
his principal place of business .Id. §7413 (b). Thes
-------
-9-
provisions expressly give the court jurisdiction to enforce
EPA's order of April 12, 1977.
Although EPA's right to enter Donner Hanna's
plant and its right to use a particular test method are
conceptually distinct, under the circumstances of this case
the two questions are inextricably connected. Donner Hanna
has from the outset been willing to permit EPA to inspect
using the "remote" method. EPA states that it seeks per-
mission to inspect for the sole purpose of using its
proposed method. EPA's counterclaim, 5(19. The government
has stipulated to the determination of the proper inspec-
tion method by the district court, in its brief filed on
June 24, 1977, EPA states:
EPA believes that its right to enter
and insp ect_the Donner-Hanna facility
"pursuant to §114 of the Act is entirely
Independent of the applicability, as a.
matter of law, of a particular test
method. The latter question, the Agency
believes, relates strictly to the eviden-
tiary value of any resulting measurements,
and like any other evidentiary natter, is
therefore not ripo for revicv.v until EP*.
socks to assert those measure.::-;;!ts as evi-
dence against the company. F.av-:-vor, rais-
ing the issue of ripeness in this connec-
tion would seem to be inconni:.: tont with
the stipulation between the Agency and
Donner-Hanna. Therefore, while the stipu-
lation might not strictly bo viewed as
-------
-10-
governing this issue, as a matter of
good faith EPA will not assert a lack
of ripeness as a bar to review at this
time of the applicability, as a matter
of law, of Reference Method 9 as op-
posed to the company's suggested ob-
servation method.
Brief at 26 n.12.
It would serve no useful purpose to allow the
inspection without giving some consideration to EPA's
testing method because EPA has made clear its intent to
seek criminal sanctions against Donner Hanna if the plant
does not permit the inspection on EPA's terms. The manner
in which EPA intends to conduct the inspection therefore
should be considered in this proceeding.
In connection with the court's jurisdiction, two
additional points should be noted. First, one of the de-
fects in EPA's proposed testing method alleged by Donner
na is that it was never adopted pursuant to rulemaking
procedures, either as part of New York's SIP or as part of
EPA's testing methods for nev emission sources. See
40 C.F.R. §§52.12(c)(1), GO Appendix A. As a rcpui:, the
method was never subject to judicial review by the aooro-
priate Court of Appeals as expressly provided in ?,2 u.S.c.
§7607 (b)(1). Thus 57607(b)(2), which prcwidos that actions
1:
-------
-11-
reviewable under (b) (1) cannot be reviewed in civil or
criminal enforcement proceedings, does not preclude the
district court from reviewing the method in enforcement
proceedings. West Penn Power Co. v. Train, 522 F.2d 302,
309, 312 (3d Cir. 1975), cert, denied. 426 U.S. 947 (1976).
Second, several courts have found that preen-
forcement review of the validity of §7413 orders is barred
by the Clean Air Act. Lloyd A. Fry Roofing Co. v. EPA.
554 F.2d 885 (8th Cir. 1977); West Penn Power Co. v. Train.
supra; Getty Oil Co. v. Ruckelshaus, 467 F.2d 349 (3d Cir.
1972), cert, denied, 409 U.S. 1125 (1973). But these cases
do not preclude judicial review of the counterclaim because
the counterclaim was brought under tne teaerai enforcement
provisions of the Clean Air Act, 42 U.S.C. §7413, and can
be classified as an enforcement proceeding.
Having found that the court has jurisdiction to
review EPA's proposed testing method, the next question is
the scope of review. This is governed by the Administra-
tive Procedure Act, 5 U.S.C. §706. See, e.g., Citizens to
Preserve Overtop v. Vo.' ¦- , 401 U.S. 402, 413-14 (1971)
Texas v. EPA. 499 F.2d 209, 296 (3th Cir. 1974), cert.
denied, 427 U.S. 905 (1976). Under §700, the court rroist
-------
-12-
determine whether EPA followed lawful procedures in decid-
ing to use its proposed testing method for insnectinci
Donner Hanna and whether use of its method would be arbi-
trary, capricious, an abuse of discretion, or otherwise
not xn accordance with law.
III. STATUTORY AND REGULATORY BACKGROUND
Under the Clean Air Act, each state must submit
to EPA for its approval an SIP providing for the attainment,
maintenance and enforcement of national ambient air quality
standards. 42 U.S.C. §7410 (a). If a state fails to submit
a plan, or if the plan submitted does not meet federal re-
quirements, EPA is authorized to promulgate an implementa-
tion plan for the state, J^d. §7410(c)(1).
New York submitted an SIP in accordance with these
provisions in 1972, and it was approved by EPA. Both the
adoption of the SIP and its approval by EPA followed rule-
making procedures and could have been subjected to judicial
review. The portion of trie New York SIP relevant to this
action providers as follows:
Smoke emissions.
(a) After December 31, 1974, or such
later date as determined by ari order of
the commissioner, no person shnll oper-
ate a by-product coke oven battery which
-------
13-
emits a smoke equal to Ringlemann No. 1
or 20 percent opacity.
(b) Such person who operates a by-
product coke oven battery shall be al-
lowed an emission of smoke from the
battery of greater than Ringlemann No. 1
or 20 percent opacity if such emission
continues for a period or periods aggre-
gating no more than three minutes of any
consecutive 60 minute period.
6 N.Y.C.R.R. §214.3.
This regulation, referred to as the "three-minute rule,"
does not specify the method to be used in measuring smoke
ODacity nor does any other part of the SIP.
The three-minute rule is knowh as an "aggregate
opacity" regulation because it allows emissions from the
coke oven battery in excess of the regulatory opacity limi-
tation (20% opacity) for a period or periods aggregating
no more than three minutes out of any consecutive 60 min-
utes. By contrast, some opacity standards prohibit any
emissions in excess of a certain opacity limitation, for
any amount of time. This sort of standard is typically
applied to industrial source-, which have smoke stack a qlk!
which emit smoke fairly steadily and without great variance
in the opacity level.
1
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-14-
Where the SIP does not sDecifv testinq proced-
ures, federal regulations allow EPA to determine compli-
ance by means of "appropriate procedures and methods
prescribed in Part 60 of this chapter ...." 40 C.F.R.
§52.12(c)(1). Part 60 sets forth the new source perfor-
mance standards established by EPA for newly constructed
or modified sources of air pollution. Appendix A of part
60 contains certain "Reference Methods" for determining
compliance with the new source performance standards.
One of these methods is Method 9, which establishes a
procedure by which human observers can determine the opac-
ity of emissions from stationary sources.
Method 9 was originally promulgated in December,
1971. 36 Fed.Reg. 24,895 (Dec. 23, 1971). In response to
the court's direction in Portland Cement Association v.
Ruckelshaus, 486 F,2d 375 (D.C.Cir. 1973), cert, denied.
417 U.S. 921 (1974), it was revised in November, 1974 in
an effort to increase its accuracy. 39 Fed.Reg. 39,973
(Njv. 12, 1974) . Revised ?\othod 9 requires the dfc^rtaina-
tion of co." piiaace v/i t:h cu.-.civy stand::-.!.; to bo bayod on
an average or '?A consecutive: readings? t.iken at iS-s«co«d
intervals. A finding of violation can b-:? made only if the
-------
-15—
average of 24 observations exceeds the applicable emission
standard by 7.5%. The observer must be positioned in such
a manner that the sun is oriented in the 140° sector to
his back, his line of vision is perpendicular to the
plume direction, and no more than one plume is in his line
of vision. The observer must have a clear view of the
plume and must estimate opacity at its darkest point. If
visible water vapor is present with the smoke, opacity
cannot be estimated until the water vapor has dissipated.
in addition to setting forth a method for measur-
ing opacity, Method 9 establishes a program for training
observers to correctly associate an observed contrast with
opacity and for certifying observers who successfully com-
plete the training program. Observers are not trained or
certified for the use of the stopwatch technique, discussed
below. Ogg at 86.
The 1975 EPA Guidelines (Ex. 2), which EPA seeks
to use along with the stopwatch technique to determine com-
p]ianco with the three—minuto rule, are not contained in
Part 00 of the rc±cjulations arid v.'erc not promulgated by for-
mal rulemaking procedures. They represent KPA's attempt
to "adapt" Method 0 to the testing of various typor, of
-------
-16-
stationary sources of air pollution, including coke oven
batteries.
The 1975 EPA Guidelines translate the general
positioning requirements of Method 9 into specific proced-
ures applicable to coke oven batteries. Thus, the Guide-
lines suggest that particular contrasting backgrounds be
used for viewing the various types of emissions produced
by coke oven batteries. They also specify where observers
should stand in order to obtain a "clear and unobstructed"
view of the various emissions. fix. 2 at 25-27.
The 1975 EPA Guidelines do not specify whether
averaging or direct unaveraged measurements should be used
in testing coke oven emissions. According to the testimony
of Robert N. Ogg, the chief EPA engineer responsible for
stationary source compliance in Region II (New York and the
Virgin Islands), inspectors in this region are instructed
to use the "stopwatch" technique for timing coke oven emis-
sions. Ogg at 22-25. Rather than averaging opacity read-
, the in:-: viowr; i •v.iisr-.io;- ::"nnouvily "':vl
tV.fi toLi-no the- ion > or cx::cn:*:= 20..'
opacity. Two s topwatches ore: : o:v: to record violation
tim^s and the other to record the time of clay when the vio-
lation boyin.s and ends. During a poric;.: no Led as a violation,
*
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-17-
only three readings are required: the first is at the time
that the emission equals or exceeds 20% opacity, the sec-
ond is the highest reading during a period of violation,
and the third is when the violation ends (i.e., the opac-
ity of the emission falls below 20%). The inspection team,
which consists of a minimum of three observers, views the
battery for one hour and then totals the emissions exceed-
ing 20% opacity. Overlapping observations are excluded by
referring to the exact time of day at which the observa-
tions were made. A violation is found if the total exceeds
the three minutes allowed in Part 214 o"f the SIP. Ogg at
23-32.
The stopwatch technique was apparently devised
by regional EPA officials in order to address the particu-
lar problems of monitoring coke oven compliance with New
York's three-minute rule. It is used to time emissions
which are too short in duration to use 15-second averaging
As the record stands in this case, the stopwatch technique
h c z not boon officially aclopto-3 by f-'?.".. None of th«- in-
r>i><':ction manuals or other exhibits intvouucod into evidenc
describe the details of the technique. The inspection
method which Donner Hanna claims should be used in lieu of
-------
-18-
EPA's proposed method is referred to as the "remote" or
5/
"off-site" method. It was used by the new York State
Department of Environmental conservation in inspecting
Donner Hanna in 1974 after Donner Hanna objected to the
use of topside observers. It differs from EPA's proposed
method in that observers are not placed on top of the bat-
tery to observe charging and topside leak emissions but
rather stand on the catwalk approximately 200 feet away
from the battery. The remote method apparently uses the
stopwatch technique to measure the duration of emissions.
The parties agree that it is much easier for Donner Hanna
to meet the state emission standard using the remote tes-
6/
ting method than using the 1975 EPA Guidelines.
The issue in this case is whether EPA can test
Donner Hanna1s compliance with the three-minute rule by
using the 1975 EPA Guidelines in conjunction with the stop-
watch technique. Donner Hanna maintains that it cannot for
a number of reasons. First, it argues that EPA's proposed
testing method is not merely an interpretation or ac>.ota-
ziori c.»; Method rJ 0 t'oos n.*• »•
• • f £" *• ,k I I L .. «
wittont sources, such 2s c;oko oven batL'.vji.es. Secor.-'.
Donner Hanna maintains that the proposed testing method
nr.st bo' formally Copied in ordor to y with t'no regu-
*
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-19-
latory scheme of the clean Air Act and with the due process
clause of the Constitution. Finally, the plaintiff contends
that the proposed testing method is arbitrary and unreliable
and that EPA should use the "remote" method in inspecting
coke oven batteries.
EPA contends that Method 9 provides a basic frame-
work for determining opacity but does not purport to set
forth specific testing procedures for each major type of
air pollution source, coke oven batteries, EPA argues,
present various problems which must be solved on a case-
by-case basis due to the complexity of Che industrial pro-
cesses involved, the numerous types of emissions encoun-
tered, their widely varying durations and other charac-
teristics, and (in the case of the New York SIP) the lack
of a promulgated set of procedures for determining compli-
ance with regulatory standards. EPA's position is that it
is entitled to develop a method applicable to intermittent
emissions and to enforcement of a stat'.o SIP containing a
tiiiv: c;v;:-vpt;iov., v. nc3 th~.t it ::».>«/ do so v/itl'Out vcr.-rsrt to
rulemaking and without fcrii'.'i 1. revision io .•.;otiiod . The
Agency characterizes its proposed testing method as an
adaptation or interpretation of Method 9 and argucr thnt
-------
-20-
its interpretation is entitled to great deference.
IV. FINDINGS
I have carefully considered the positions of
both parties in light of the evidence produced at trial
and make the following findings.
First, I find that Revised Method 9, which re-
quires averaging of 24 consecutive readings, is not an
appropriate method or procedure for determining compliance
with an aggregate-type standard such as New York's three-
minute rule. By EPA's own admission, utilization of the
averaging technique in Method 9 would preclude tho aggre-
gation of the durations of all emissions in excess of 20%
opacity observed during a given 60-minute period. This
fact is acknowledged in the preamble to revised Method 9:
In developing this regulation we have
taken into account the comments received
in response to the September 11, 1974
(39 FR 35852) notice of proposed rule-
making which proposed among other things
certain minor changes to Reference Method 9.
This regulation repr.^r.cn.hr. Uv; rulenvn.k\r.<-:
v/i Lh resc'ict to fchrs rev Ik to 0.
The dctr-rr.i.in"> t\c:\ -j,: 00 1 a V;ith
applicable opacity s tandards -..-11.1 be ba«c tr
readings taken at 1-j second intervals. This
approach is a satisfactory means of enforcing
-------
-21-
opacity standards in cases where the
violation is a continuing one and time
exceptions are not part of the appli-
cable opacity standard. However, the
opacity standards for steam electric
generators in 40 CFR 60.42 and fluid
catalytic cracking unit catalyst re-
generators in 40 CFR 60.102 and numer-
ous opacity standards in State imple-
mentation plans specify various time
exceptions.. Many State and local air
pollution control agencies use a dif-
ferent approach in enforcing opacity
standards than the six-minute average
period specified in this revision to
Method 9. EPA recognizes that certain
types of opacity violations that are
intermittent in nature require a dif-
ferent approach in applying the opacity
standards than this revision to Method 9.
It is EPA's intent to propose an addi-
tional revision to Method 9 specifying an
alternative method to enforce opacity
standards. It is our intent that this
method specify a minimum number of read-
ings that must be taken, such as a mini-
mum of ten readings above the standard in
any one hour period prior to citing a vio-
lation. EPA is in the process of analyz-
ing available data and determining the
error involved in reading opacity in this
manner and will propose this revision to
Method 9 as soon as this analysis is com-
pleted. The Agency solicits comments and
recommendations on the need for this addi-
tional revision to Method 9 ar.d would v.-o I -
coinc any surges t'.u.-t!:: par tic a 1 ^ ly £ro;i: ;; L •;
pollution control un »ov; v/<: r.vL'jh I
mciV.:.' Ma Uiod 9 m<">r*.v i.v to tilt! noo^.s
of those: agencies.
39 fed.Keg. 39,873 (Nov. 12, 1974) (emphasis added). See
also r.x. 20 at 7-8. Since the 1974 revision, thoro has
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-22-
been no additional revision oC Method 9 to make it appli-
cable to intermittent sources or to opacity standards
with time exceptions. It is therefore clear as EPA ad-
mits that Method 9 itself cannot be used to test Donner
Hanna's compliance with the three-minute rule.
EPA nevertheless argues that its proposed tes-
ting method is merely an interpretation or adaptation of
Method 9. In other words, the agency argues that it can
adopt the applicable parts of Method 9, reject the inap-
plicable parts, and substitute the stopwatch technique
for six-minute averaging.
For a number of reasons, I find EPA's position
untenable. Finst, it is internally inconsistent. On the
one hand, EPA admits that Method 9 cannot be used because
the averaging technique cannot be applied to coke oven
batteries. On the other hand, at trial it characterizes
the rejection of averaging as merely an interpretation of
or in?;iqri.i f irit deviation from M.etho--! 9. The ii".v<:?•¦>Le
racoon i.:je ?, her.-.", vc s:, rha f. V.'.i:-; •v.vr."**;... ; c: -i': cc- i*'.: .urr. -t
1 L>-;;oco:vri .in tor vai?; is t.tu i. to i cr. ;x- li-tbili-y - Sinc;^
proposed testing method dou\> iu'c include one ofc Line contr
tur-'.s wf .Ve tho.l T, it t ;).|t : !•;» rcnw.-jotii an i
tcrprutation or adaptation of :'.othod 9.
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Second. a tcstina method which contains an aver-
aging technique is fundamentally different from a testing
method which aggregates unaveraged readings. Under the
stopwatch technique, a single reading exceeding 20% opac-
ity would count toward the three minutes allowed under the
New York opacity standard, thereby increasing the proba-
bility that the source will be found to be in violation
of the standard. If, however, readings taken at fifteen-
second intervals are averaged over six minutes, a single
high reading would not necessarily contribute toward a
finding of a violation because it could'- well be offset or
at least reduced by lower readings.
The difference between averaging and straight
aggregation is exacerbated where human observers are used
to make the readings, because averaging makes it possible
to assess the observers' general patterns of accuracy and
to reduce the impact of occasional erroneous opacity esti-
mates. Government *s Post-Trial Brief at 11. EPA's own
•./i toons aitL :••'! that com; :ir n.j the stop-.-.'u:h tec'1.!:I.tjc: to
:: i -ii. j. ri u t.''1 i :in»j •.¦.•'is "r:ii. • r apple-.; oranrp.iis. " Ogg
, • ') *)
• I s- -i S- .
Tn an attempt to tnto trot the stopwatch
technique and vethod 9 woro not significantly different in
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-24-
terms of quantifying coke oven emissions, EPA presented
at trial an analysis of emission data, which compared
observations made at 15-second intervals v/ith observations
made in accordance v/ith the stopwatch technique. Ex. 29.
Mr. Hopkins, who performed the analysis, testified that
there was no significant difference between the two types
of readings. Because of several serious flaws in the an-
alysis, however, it cannot be accepted in support of EPA's
position. First and most important, tihe readings taken
over 15-second intervals were never averaged as contem-
plated by Method 9. As a result, the analysis did not
compare Method 9 to the stopwatch technique and cannot be
used to demonstrate the insignificance of averaging. In
addition, as EPA acknowledges, the data base used for the
analysis was small, it was gathered for other purposes,
and it was not in a form which was useful for purposes of
this litigation. Finally, the analysis did not take into
account a nutr.bor of rsicjni f icon t var inhl os, such n-i v/oather
'.:o:vi.i tion:--. anr! o'cr.Tvur co:'iti.i"i!"v.
C iucil_..roayou i'w, r:; jccLii.w . • • ' a pro: v>;.- -u U*s-
! mcLho-: c»s an a>-1apta tio;i o t MoLhov. j i r- ' s failure
t:o justify its adaptation. V/ i th the oxennti on of Hopkins'
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-25-
analysis, no studies were introduced supporting the relia-
bility of the stopwatch technique or its relationship to
averaging. Although the agency was granted an adjournment
in the trial in order to call an expert witness to rebut
the testimony of Donner Hanna's expert, Dr. Ensor, it
failed to do so. It also failed to call the author of
the 1975 EPA Guidelines, Kenneth B. Malmberg.
EPA argues that an agency's judgment in inter-
preting its own regulations is normally entitled to judi-
cial deference. This is an accurate statement of the law.
See, e.g.. Train v. NP.DC. 421 U.S. 60, 87 (1975); Udall v.
Tallman, 380 U.S. 1, 4 (1964). But from this it does not
follow that EPA is entitled to deference in this case. A
well-established corollary to the above principle is that
no deference is in order where the agency's interpretation
is plainly erroneous or inconsistent with the regulation.
See, e.g., Bowles v. Seminole Rock Co.. 325 U.S. 410, 413-
14 (1975).
Here, E?A ' s position t tri-n1 ii :co,rn. r.t
wi th its published position in tjin prect:r.r>!^ t.o ?•;•?t:.ho:! y.
'lorcovsr, the evidence intro:!-.i ¦:c;d at trial wnde clear that
the test procedures which EPA intended to use wore not
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-26-
adopted by EPA at its higher levels but were more akin
to on-the-spot x at 19. The
data which was available indicated that accumulation of non-
contiguous high readings, such as would be necessary in de-
termining compliance with a time exception emission stan-
: i:"], i.: ic-'.p. t !¦/ i - • :.i r>c I.:: r i':>: *.»f errc r . H:-:.
"i e.x ! V-.TfJ. in I i.gh t of Li i ¦.« circusr:: •. Jsrv.'O-i, I rind that
i-'-Vi-.' r, interprets tion if. noi. entitle'! 'c > judicial deference
onci, in the absence of supporting evidence, cannot stand.
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-27-
Th e cases cited by EPA in support of judicial
deference are readily distinguishable. McLaren v.
Fleischer, 256 U.S. 477 (1921), involved a practical
construction of a federal statute which was adopted by
the Secretary of the Department of interior, had been
in effect long before the controversy arose, and was
later converted into a regulation, udall v. Tallman,
supra, involved the Secretary of interior's interpreta-
tion of an executive order. The interpretation was a
matter of public record and had been applied on a number
of prior occasions. In Train v. NRDC. supra, the admin-
istrative decision was made by the top officials in EPA
and was publicized. In none of these cases was the agen-
cy's published position plainly inconsistent with the
administrative interpretation upheld by the court.
Having found that EPA's proposed testing method
is not an interpretation of Method 9, I now turn to the
t.ion of. whether rulcrna!: ir.g is required he Tore n?.\ can
use its propo-;c.:l testing method in clctvrr-.ini.n'j whet::en* oo>:
ovon batteries 'ire in compliance with applicable omission
standards. I find that under the Administrative Procedure
Act. nnri F.PA'f; ova regulations, rulemaking is necessary.
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It is undisputed that the method of determining
compliance with an emission standard can affect the level
of performance required by the standard, even though the
standard itself has not changed. See Ex. 12; Portland
Cement Association v. Ruckelshaus, supra at 400-01. The
performance standard for smoke opacity, which was promul-
gated by the state and approved by EpA in New York's SIP,
cannot be changed without following rulemaking procedures
under state lav/. 42 U.S.C. §7410 (a) (3) (A). Similarly,
EPA's regulations, including new source, performance stan-
dards and reference methods, cannot be 'changed without
following rulemaking procedures. 42 U.S.C. §7607 (d);
Detroit Edison Co. v. E.P.A.. 496 F.2d 244, 249 (6th Cir.
1974). Enforcement officials cannot circumvent the rule-
making requirements of the Clean Air Act by making substan-
tial changes in testing methods without notice and a hear-
ing. The importance of developing an objective method of
to sting opacity has b"en recognized in Pot 11 and_ Cedent,
¦ •nc. the clonr i.-iOli"'' tj C tlv* t .-i': ".i rl 'V. is th it- owelty
L.; .-ry iiub t. to r a iM f i r2.12 (c) ir.r. tructs
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-29-
EPA in determining compliance with the Act to use the test
procedures specified in the SIP or, if none are specified,
the test procedures and methods applicable to new source
performance standards. Regardless of which test methods
are used, both would have been subjected to rulemaking,
either at the state or the federal level. Moreover, the
preamble to revised Method 9 specifically recognizes that
further rulemaking is necessary in order to develop a tes-
ting method for intermittent sources or emission standards
containing a time exception.
phasized. It gives parties affected by a decision an oppor-
tunity to participate in the decision-ninV.ing process and
forces EPA to articulate the bases for its decisions. See
Buckeye Power, Inc. v. K?A, 481 F.2d 162, 170-73 (6th Cir.
1973). These procedures tend to produce more objective
testing methods. Portland Cement, supra. it also enables
nrjqr !• nnvt v:s3 to spo% -i > i ' i. : i nl r<»v! •• : I'v.-
i r 1 . -1 ? u.."i.e. ^ • .: i l.j < \.y _ <>'J'yy_ '.ori
Park v. Vol no, r. up 'ira it 41^.
In finding that rulemaking nr-ocssary in order
to clov'ilap -m anprouri'i t« tor; tiny met: Tor cok«„» ovoa
The significance of rulemaking cannot be underem-
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-30-
batteries, I do not intend to suggest that regional repre
sentatives of EPA should not be given some leeway in adap
ting formally promulgated guidelines to local conditions.
It must be emphasized that the finding in this case is
premised on my conclusion that the agency, in "adapting"
Method 9, strayed so far from the original substance and
intent of Method 9 that it in effect created a new and
different method, not subject to the scrutiny of rulemak-
ing procedures.
Since the remote method has not been subjected
to rulemaking proceedings and is not part of New York's
SIP, Donner Hanna is not entitled to an order requiring
EPA to use the remote method in testing smoke opacity.
But as an interim measure pending completion of rulemak-
ing on a testing method for coke ovens, and in order to
enable EPA to continue its enforcement efforts, EPA may
use the remote method at the Donner Hanna facility.
At trial, Donner Hanna introduced considerable
•.-••v? rlor.cf! chal] n.iginq the ; • ••:*:! v.l lv •-:vv IvV > ?::\\
Tt C'< 11 C'1 in oxpjr c . Kti'sor,
a r, tiidy of Mothod 0 ar.'; tho ]')/'• '•? A Gui'*:r>? i (
26), t.o testify fit length about his fin^-'.ngr. Dr. Lnsor
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-31-
concluded that the EPA Guidelines for the application of
Method 9 to coke ovens "result in serious compromises
which cause significant errors overestimating the opacity
and duration of coke oven emissions." Ex. 26 at 8. The
primary difficulty involves the positioning of the obser-
vers as specified in the Guidelines, which affects the
background against which the plume is observed and conse-
quently the accuracy of the estimate. An additional source
of unreliability concerns the 15% margin of error allowed
in the observer training school and its effect on the re-
ported duration of emissions observed continuously rather
than at fifteen-second intervals. Although the trial was
-a- f*
adjourned for several weeks in order to give EPA an oppor-
tunity to respond to Dr. Ensor's report, EPA decided not
to attempt to rebut the testimony or report.
Although Donner Manna's evidence on this point
was persuasive, I find that it would be inappropriate at
this stage to make a determination as to the validity of
-i 197:5 V.T A : i.dulino:i n .1 • i • ' '¦: i * Cn>- • .*. > *.i i a h'V p": >;>c-2"
joct of rul I r;q proco'.-" i u-:x i»tv! i \ 'vic-w-:V:.>" c: ~.ijy
by the Court of Appeals. 42 r.r. S . c. (1) .
-------
Dormer Hanna is directed to prepare a proposed
judgment on notice to defendant.
So ordered.
v
yfjA { LaaaJa-ia^
JOHN T. CURTIN
United States District Judge
DATED: February 12, 1979
2
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7*4"
FOOTNOTES
The Clean Air Act was amended in 1977 and the
provisions were renumbered. Although the parties'
briefs refer to the old section numbers, references
throughout this decision shall be to the new numbers.
This fact is alleged in the Complaint (529)
and admitted in EPA's Answer (19).
See order of September 21, 1977, denying EPA's
motion for summary judgment.
As discussed in greater detail infra, EPA's
proposed testing method had what amounts to two
separate components. First, the 1975 F.PA Guidelines
specified observer positioning and background re-
quirements. Second, the stopwatch "technique, rather
than an averaging technique, was used to time the
duration of pushing and charging emissions. Unless
otherwise indicated, references in this opinion to
EPA's proposed testing method are intended to encom-
pass both components.
At trial, the parties disagreed about whether
the "remote" method had been endorsed by the state
and could be referred to as the "state" method. Since
they agreed that it had not been promulgated by the
state in accordance with rulemaking procedures, see
discussion infra, X find it unnecessary to make a
finding of fact on this; issue.
Th" jua'ce condu'j«¦¦¦ second \n-s:vjefciOrt c«£
iianna in 197 / uairrj boM-. '. in; r«.»mc: '• 'chocl ?-u-: J'.i A's
proposed method. Exhibit: 12 sirarnr.rii'.ca the observation
.an*! a the ro-jul. . Over it: inu r. .'.vit:
the remote method resulted in one finding of violation
and the riPA method in five.
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