Selected Smart Growth Publications from the Smart Growth Network

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This report is available online at (click on "publications").

For additional hard copies of this report, call EPAs National Center for Environmental Publications
at 513 891-6561 and ask for publication number EPA231-R-02-001.
-------
SMART GROWTH
N
WORK
Selected Smart Growth
Publications
From the Smart Growth Network
The United States Environmental Protection Agency (EPA) is publishing this information
in an effort to increase public understanding of how Smart Growth can further efforts to
protect our environment. The Agency has selected the publications listed here on that basis.
However, EPA does not necessarily endorse the views expressed in any particular publica-
tion and does not promote the purchase of any organization's publications. You are urged to
contact vendors who charge a fee prior to ordering these publications.

If you or your organization want EPA to consider listing additional Smart Growth publica-
tions in the next edition of "Selected Smart Growth Publications," please contact Tim Torma
at 202 566-2864.
Printed on paper that contains at least 50 percent postconsumer fiber.
-------
Table of Contents

Within categories, publications appear in order of publication date, most recent
publications listed first. Prices given do not include mailing costs. For more informa-
tion about the Smart Growth Network, see .

Smart Growth Primers 1

Smart Growth Planning and Policy 2

Land Use and Local Planning 4

Smart Growth Design and Development 4

Smart Growth Economics 7

Smart Growth and Community Development 7

Smart Growth and Environmental Quality 8

Farmland Preservation and Rural Conservation 10

Open Space Design \\

Smart Growth and Brownfields Redevelopment 11

Smart Growth and Transportation 12
-------
Smart Growth Primers
Local Tools for Smart
Growth: Practical
Strategies and Techniques
to Improve Our
Communities. National
Association of Counties
(NACo) & the U.S.
Conference of Mayors,
The Joint Center for Sustainable Communities,
2001. For copies of this report (no charge), contact
NACo, 440 First Street, NW; Washington, DC
2000; phone: 202 393-6226; fax: 202 393-2630.
Available online at .

Smart Growth Tool Kit. David O'Neill. Urban Land
Institute, 2000. Call 800 321-5011 (fax: 202 624-
7140) or order online at
(click on "Bookstore"). Cost: $35.95; discounted
ULI member price: $29.95.

Covering Urban Sprawl:
Rethinking the American
Dream — A Primer for
Reporters Covering the
Social, Economic, and
Environmental Impacts of
Sprawl. David Goldberg.
Environmental
Journalism Center.
Reprinted for the Smart
Growth Network, 1999.
May be downloaded at
no charge from . Hard copies may be purchased from
The Radio and Television News Directors
Foundation at 202 467-5241. Cost: $20.00 per
booklet ($10.00 for RTNDA members).
BEST DEVELOPMENT j
PRACTICES:

A Primer for Smart Growth
Smart Growth: Myth and
Fact. David O'Neill.
Urban Land Institute,
1999. Call 800 321-5011
(fax: 202 624-7140) or
order online at
(click on
"Bookstore"). Cost:
$15.00 per packet of 10
copies.
Best Development
Practices: A Primer for
Smart Growth. Reid
Ewing with Robert
Hodder. International
City/County
Management Association,
1998. Call 800 745-8780
or order online at .
Cost: $9.00.
ULI on the Future:
Smart Growth —
Economy, Community,
Environment. Urban
Land Institute, 1998.
Call 800 321-5011
(fax: 202 624-7140) or
order online at (click on
"Bookstore"). Cost:
$24.95; ULI member
discount price: $19.95
Why Smart Growth: A
Primer. International
City/County Management
Association with Geoff
Anderson, 1998. A Smart
Growth Network
Publication. Call 800 745-
8780 or order online at
. Cost: $8.00.
Smart Growth Primers
-------
Smart Growth Planning and
Policy
Getting to Smart Growth
Getting to Smart Growth:
100 Policies for
Implementation. The
Smart Growth Network
and the International
City/County
Management Association,
2002. Hard copies may
be obtained at no charge, while supplies last, by
sending an e-mail request to smith.juanita@epa.gov,
by faxing your request to 202 566-2868, or calling
202 566-2860. Also available online at
or
.

Solving Sprawl: Models of
Smart Growth in
Communities Across
America. F. Kaid
Benfield, Jutka Terris, and
Nancy Vorsanger. Natural
Resources Defense
Council, 2001, with a
preface by Maryland
Governor Parris
Glendening (Sequel to
Once There Were
Greenfields, 1999.) Call
800 828-1302 or order online at
or
. Cost: $20.00.
THE COMING DEMAND
'
The Coming Demand.
Congress for the New
Urbanism. Pamphlet
based on research by
Dowell Myers, Elizabeth
Gearin, Tridib Banerjee,
and Ajay Garde.
University of Southern
California School of
Policy, Planning, and
Development, 2001. Call
GNU at 415 495-255 for
a hard copy free of charge, or download from
(click on "GNU
Reports").

Challenging Sprawl: Organizational Responses to a
National Problem. Constance Beaumont, Ed.
National Trust for Historic Preservation, 1999. Call
202 588-6296 (fax: 202 588-6223) or order online
at . Cost:
$10.00.

Once There Were
Greenfields: How Urban
Sprawl is Undermining
America's Environment,
Economy and Social
Fabric. F. Kaid Benfield,
Matthew D. Raimi, and
Donald D.T. Chen.
Natural Resources
Defense Council, 1999.
Call NRDC s
Publications Department
at 212 727- 4486 or
order online at .
Cost: $20.00.
Smart Growth Planning and Policy
-------
Planning Communities for the 21st Century: A
Special Report of the American Planning
Associations Growing SmarfM Project. American
Planning Association, 1999. Call 202 872-0611
(fax: 202 872-0643) or order online at
(click on "APA Store,"
then "Planners Book Service") No charge.

Sprawl Busting: State Programs to Guide Growth.
Jerry Weitz. American Planning Association.
Planners Press, 1999. Call 202 872-0611 (fax: 202
872-0643) or order online at (click on "APA Store" and choose
"Planners Book Service"). Cost: $48.00; APA mem-
ber discount: $43.00.

Cities Back from the Edge: New Life from
Downtown. Roberta Brandes Gratz. National Trust
for Historic Preservation. John Wiley &
Sons/Preservation Press, 1998. Call 202 588-6296
(fax: 202 588-6223) or order online at . Cost: $19.95; NTHP
member discount price: $17.95.

Growing Smart?M Legislative Guidebook: Model
Statutes for Planning and Management of Change.
Phases I (revised) and Phase II. American Planning
Association, September 1998. Call 202 872-0611
(fax: 202 872-0643) or order online at
(click on "APA Store,"
then "Planners Book Service"). Cost: $32.00.
___
Balancing
aCoi
^Gateway Gonunmuties
' wm^^xmw^as=M^ ***/•* '"'•» ?? g" ~» »
-_"•"_. 7,' .:
)im Hows, Eel McMalion, and Luther Propst
Balancing Nature and
Commerce in Gateway
Communities. Jim Howe,
Ed McMahon, and
Luther Propst. The
Conservation Fund and
Scenic America. Island
Press, 1997. Call 800
828-1302 (fax: 707 983-
6414) or order online at
. Cost: $13.95;
with NTHP member discount: $12.55.

Smart States, Better
Communities: How State
Governments Can Help
Citizens Preserve their
Communities. Constance
Beaumont. National
Trust for Historic
Preservation, 1996. Call
202 588-6296 (fax: 202
588-6223) or order
online at . Cost: 20.00; with NTHP discount: $18.00.

Growth Management Principles and Practices.
Arthur C. Nelson and James B. Duncan. American
Planning Association. Planners Press, 1995. Call 202
872-0611 (fax: 202 872-0643) or order online at
(click on "APA Store,"
then on "Planners Service"). Cost: $48.95; APA
members discount price: $40.95.
Smart Growth. Planning and Policy
-------
Land Use and Local
Planning
Glossary of Zoning, Development, and Planning
Terms. Michael Davidson and Fay Dolnick, eds.
American Planning Association. Planners Advisory
Service (PAS) Report #491/492, 2000. Call 202
872-0611 (fax: 202 872-0643) or order online at
(click on "APA Store,"
then "Planners Book Service" and choose "PAS
Report" option at left). Cost: $34.00.
The Practice of Local
Government Planning,
third edition. Linda C.
Dalton, Charles J. Hoch,
and Frank S. So.
International City/
County Management
Association, 2000. Call
800 745-8780 or order
online at . Cost:
$42.95.
Land Use in America. Henry L. Diamond and
Patrick F. Noonan. The Conservation Fund. Island
Press, 1996. Call 202 872-0611 (fax: 202 872-0643)
or order online at (click
on "APA Store," then "Planners Book Service"). Also
available at . Cost:
$29.95.

Small Town Planning Handbook, second edition.
Thomas Daniels, John Keller, and Mark Lapping.
American Planning Association. Planners Press,
1995. Call 202 872-0611 (fax: 202 872-0643) or
order online at (click
on "APA Store," then "Planners Book Service").
Cost: $43.95; APA member discount price: $36.95.

Save Our Land, Save Our Towns. Thomas Hylton.
RB Books, 1995. Call 800 497-1427 or order online
at . Cost: $29.95.
Citizens Guide to Planning, third edition. Herbert
Smith. American Planning Association. Planners
Press, 1993. Call 202 872-0611 (fax: 202 872-0643)
or order online at (click
on "APA Store," then "Planners Book Service").
Cost: $29.95; with APA member discount: $26.95.
Smart Growth Design and
Development
Building Livable Communities: A Policymaker's
Guide to Infill
Development, Expanded
Second Edition. The
Local Government
Commission/Center for
Livable Communities,
2001. Call 916 448-1198
or order online at
.
Cost: $20.00.

Real Towns: Making Your Neighborhood Work.
Harrison Bright Rue.
Local Government
Commission/Center for
Livable Communities,
2001. Call 916 448-1198
Real Towns
-- Making your neighborhood work
or order online at
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Strategies for Successful
Infill Development.
Charles Bartsch,
Elizabeth Collaton, Ann
Eberhart Goode,
Christopher Hudson,
Shelley Poticha, and
Andy Shafer. Northeast-
Midwest Institute and
Congress for New
Urbanism, 2001. May be
downloaded at no charge
at . For hard
copies, call Heather Lockridge at 202 544- 5200
(fax: 202 544-0043). Cost: $29.00.
Ten Principles for
Reinventing America's
Suburban Strips. Michael
Beyard and Michael
Pawlukiewicz. Urban
Land Institute, 2001. Call
800321-5011 (fax: 202
624-7140) or order
online at
(click on "Bookstore").
Cost: $19.95.

Historic Schools in the
Age of Sprawl: Why
Johnny Can't Walk to
School. Constance E.
Beaumont with Elizabeth
G. Pianca. National Trust
for Historic Preservation,
2000. Download full
report or executive sum-
mary at no charge at
.
Better Models for Development in Virginia. Ed
McMahon, Sara Hollberg, and Shelley Mastran. The
Conservation Fund, 2000. Order online at . Cost:
$15.00. (For information on volume discounts, call
703 525-6300.)
Density by Design: New
Directions in Residential
Development. Steven
Fader. Urban Land
Institute, 2000. Call 800
321-5011 (fax:202624-
7140) or order online at
.
Cost: $69.95; with ULI
member discount:
$59.95.
Incentive Zoning: Meeting Urban Design and
Affordable Housing Objectives. Marya Morris, AICP.
American Planning Association. PAS Report #494,
2000. May be ordered online at (click on "APA Store," then "Planners
Book Service" and choose "PAS Report" option).
Cost: $32.00.

The Practice of Sustainable Development. Douglas
R. Porter. Urban Land Institute, 2000. Call 800
321-5011 (fax: 202 624-7140) or order online at
. Cost: $59.95;
with ULI member discount: $49.95.

Better Models for Chain Drugstores. Anne Stillman.
National Trust for Historic Preservation, 1999.
Order online at . Cost: $6.00; with NTHP member discount:
$5.40.
Smart Growth Design and Development
-------
^ t
, I Itutt let. Village. Town |:
Crossroads, Hamlet,
Village, Town: Design
Characteristics of
Traditional Neighbor-
hoods, Old and New.
Randall Arendt.
American Planning
Association. PAS Report
#487/488, 1999. Call
202872-0611 (fax: 202
872-0643) or order
online at
(click on "APA Store,"
then "Planners Book Service" and choose "PAS
Report" option). Cost: $34.00.

Charter of the New Urbanism. Michael Leccese &
Kathleen McCormick, Eds. Congress for the New
Urbanism. McGraw-Hill Professional Publishing,
1999. Call 800 321-5011 (fax: 202 624-7140) or
order online at (click on
"GNU Store").

Growing Together: City/County Smart Growth
Profiles. National Association of Counties and the
U.S. Conference of Mayors. The Joint Center for
Sustainable Communities, 1999. May be down-
loaded (no charge) at (click on
"Resources and Links" at left, then scroll down and
click on "Publications").
Better Models for
Superstores. Constance
Beaumont. National
Trust for Historic
Preservation, 1997.
Order online at
. Cost:
$ 10.00; with NTHP
member discount: $9.00.
Best Development Practices: Doing the Right Thing
and Making Money at the Same Time. Reid Ewing
American Planning Association. Planners Press,
1996. Call 202 872-0611 (fax: 202 872-0643 or
order online at (click
on "APA Store," then "Planners Book Service" and
choose "Planners Press" option at left). Cost:
$48.95; with APA member discount: $40.95.

Rural by Design: Maintaining Rural Character.
Randall Arendt. American Planning Association.
Planners Press, 1994. Call 202 872-0611 (fax: 202
872-0643) or order online at (click on "APA Store," then "Planners
Book Service" and choose "Planners Press" option at
left). Cost: $62.95; with APA member discount:
$52.95.

How Superstore Sprawl Can Harm Communities
(And What Citizens Can Do About It). Constance
Beaumont. National Trust for Historic Preservation,
1994. Order online at . Cost: $20.00; with NTHP member
discount: $18.00.
Smart Growth Design and Development
-------
Visions for a New American Dream: Process,
Principles, and an Ordinance to Plan & Design Small
Communities, 2nd edition. Anton C. Nelessen.
American Planning Association. Planners Press, 1994.
Call 202 872-0611 (fax: 202 872-0643) or order
online at (click on "APA
Store," then "Planners Book Service" and choose
"Planners Press" option). Cost: $58.95; with APA
member discount: $49.95.

Smart Growth Economics
Smart Growth and Affordable Housing: Making the
Connection. Report of
the Smart Growth
Network Subgroup on
Affordable Housing,
2001.See
(click on
"Resources") to download
the report (PDF format)
at no charge. For a hard
copy (no charge), call
202 566-2878.
Affordable Housing
and SMART GROWTH:
AfatixgtifGaaafcfioit
Smart Growth Funding
Resource Guide
Smart Growth Funding
Resource Guide, June
2001. An EPA/Smart
Growth Network publica-
tion. Available online at
or call
202 566-2878 for a hard
copy free of charge.
Linking Vision with Capital: Challenges and
Opportunities in Financing Smart Growth. Robert
W. Burchell and David Listokin. Research Institute
for Housing America, 2001. Download executive
summary or full report at no charge from
.
Profiles of Business
Leadership on Smart
Growth: New Partnerships
Demonstrate the Economic
Benefits of Reducing
Sprawl. National
Association of Local
Government Environment
Professionals, 1999. May
be ordered online at
. Cost:
$20.00 plus $4.00 shipping/handling.

Developments and Dollars: An Introduction to Fiscal
Impact Analysis in Land Use Planning. Natural
Resources Defense Council, 2000. May be down-
loaded at no charge from . Hard copies
may be ordered at . Cost: $5.00.

The Ahwahnee Principles for Smart Economic
Development: An Implementation Guidebook. The
Local Government Commission. Center for Livable
Communities, 1997. May be purchased online at
. Cost: $25.00.

Smart Growth and
Community Development
Smart Growth for
Neighborhoods:
Affordable Housing and
Regional Vision. National
Neighborhood Coalition,
2001. Download at no
charge from (click on
"Smart Growth Page").
Smart Growth and Community Development
-------
Urban Infill Housing: Myth and Fact. Richard M.
Haughey. Urban Land Institute, 2001. Call 800
321-5011 (fax: 202 624-7140) or order online at
. Cost: $15.00.

Smart Growth, Better Neighborhoods: Communities
Leading the Way. National Neighborhood Coalition.
2000. Order a free summary by e-mailing
or calling
202 408-8553 (fax 202
408-8551). Order full
report online at
(click
on "Smart Growth
Page"). Cost of full
report: $25.00; $12.00
for NNC members.
Smart Growth and
Environmental Quality
Connecting Neighborhood and Region for Smarter
Growth. National Neighborhood Coalition, 1999.
Download at no charge from (click on "Smart Growth Page")
or call 202 408-8553 (fax 202 408-8551).
"Sss.
EPA Guidance:
Improving Air Quality
Through Land Use
Activities. EPA
Publication # 420-R- 01-
001, 200 I.May be
downloaded at no charge
from .
Hard copies available at no charge by calling EPA's
National Service Center for Environmental
Publications at 513 891-6561.
Smart Growth and Environmental Quality
-------
Smart Growth and the
Clean Air Act. Curtis
Moore. Northeast-
Midwest Institute & the
Environmental Law
Institute, 2001. May be
downloaded at no charge
from .
Hard copies may be pur-
chased from Northeast-Midwest Institute, Attn:
Publications, 218 D Street, SE; Washington, DC
20003; phone: 202 544-5200; fax: 202 544-0043.
Cost: $21.00 plus postage/handling ($5.00 for the
first title; $1.00 each for additional titles).
Environmental Characteristics of Smart Growth
Neighborhoods: An Exploratory Case Study. Natural
Resources Defense Council, 2000. May be down-
loaded at no charge from .
Sffift
Potonlfai Rotas for Clean Wator Slate RevoMng Fund
Programs to Smart Growth Initiatives

Profiles of Clean Air Innovation: Empowering Local
Communities to Meet the Air Quality Challenges of
the 21st Century. National Association of Local
Government Environment Professionals, 2000. May
be ordered online at . Cost: $20.00 plus $4.00 ship-
ping/handling.

S" ? Potential Roles for Clean
Water State Revolving
Fund Programs in Smart
Growth Initiatives.
EPA Publication
# 832-R-00-010, 2000.
Report may be down-
loaded at no charge from
. Hard
copies available at no
charge by calling EPA's National Service Center for
Environmental Publications at 513 891-6561.
Project XL and Atlantic
Steel: Supporting
Environmental Excellence
and Smart Growth. EPA,
1999. Download at no
charge from
or call
202 566-2878 to request
a free copy.
Project XL and Atlantic Ste
5*^ Supporting Environmental
Excellence and Smart Growth
Smart Growth and Environmental Quality
-------
Redeveloping Brownfields
with Federal
Transportation Funds.
EPA and the Association
of Metropolitan Planning
Organizations, 2001.
PDF file may be down-
loaded at no charge at
(click on
"publications"). Limited
number of free hard
copies available by calling 202 566-2841.

Turning Brownfields into Greenbacks. Robert A.
Simons. Urban Land Institute, 1998. Call 800 321-
5011 (fax: 202 624-7140) or order online at
. Cost: $59.95;
with ULI member discount: $49.95.
Smart Growth and
Transportation
Residential Streets. Walter M. Kulash. Urban Land
Institute, 2001. Call 800 321-5011 (fax: 202 624-
7140) or order online at . Cost: $39.95; with ULI member
discount: $29.95.

Driven to Spend: The Impact of Sprawl on
Household Transportation Expenses. Surface
Transportation Policy Project and the Center for
Neighborhood Technologies, 2000. Download at no
charge from (click on "Bookstore"). Cost: $10.00
(special discounts for bulk orders).

Streets and Sidewalks,
People and Cars: A
Citizens' Guide to Traffic
Calming. The Local
Government
Commission/Center for
Livable Communities,
2000. To purchase, call
916448-1198 (fax: 916
448-8246) or order
online at (click on
"Bookstore"). Cost: $10.00 (special discounts for
bulk orders).
PEDESTRIAN-
AND TRANSIT-FRIENDLY
DESIGN;
A Primer for Smart Growth
Pedestrian and Transit-
Friendly Design: A
Primer for Smart
Growth. International
City/County
Management Association,
1999. To purchase, call
800 745-8780 and ask
for Item 42473 or order online at . Cost: $8.00.
12 Smart Growth and Transportation
-------
Street Design
Guidelines
for Healthy
Neighborhoods
Street Design Guidelines
for Healthy
Neighborhoods. Dan
Burden. Local
Government
Commission, 1999. To
purchase, call 916 448-
1198 (fax: 916 448-
8246) or order online at

(click on "Bookstore").
Cost: $25.00.

Traffic Calming: State of
the Practice. Reid Ewing.
Institute of Transpor-
tation Engineers and
Federal Highway
Administration, August
1999. Download (PDF
format) at no charge at

(click on "Technical
Information, then on
"Traffic Calming"). To
purchase a hard copy, call 202 289-0222 (extension
130 or 149). Cost: $50.00 ($40.00 with ITE mem-
ber discount).

Rail-Trails and Safe Communities: The Experience
of 372 Trails. Tammy Tracy and Hugh Morris. Rails
to Trails Conservancy and the National Park Service,
1998. Download PDF file at (click on "Technical Assistance,"
then on "Full-text References"). Those who do not
have Internet access may call 877-476-9297 and
request a photocopy.
Saving Historic Roads:
Design and Policy
Guidelines. Paul Daniel
Marriott. National Trust
for Historic Preservation.
John Wiley & Sons/
Preservation Press, 1998.
To purchase, call 292
588-6296 (fax: 202 588-
6223) or order online
(specify publication #
2SAV) at . Cost: $40.45.

Traditional
Neighborhood
Development: Street
Design Guidelines. Local
Government
Commission and the
Institute of
Transportation Engineers,
1997. To purchase, call
916448-1198 (fax: 916
448-8246) or order
online at (click on "Bookstore"). Cost: $35.00.

Transportation and Land Use Innovations. Reid
Ewing. American Planning Association. Planners
Press, 1997. May be ordered online at
(click on "APA Store,"
then "Planners Book Service" and choose "Planners
Press" option). Cost: $42.95; with APA member dis-
count: $34.95.
Smart Growth and Transportation 13
-------
BULMN9
UVKH.C

A POUCVMAXEITX
6UBSE TO ;
fiMMSiT-OMIKTED
Building Livable
Communities: A
Policymaker's Guide to
Transit- Oriented
Development. Local
Government
Commission/Center for
Livable Communities,
1996. To purchase, call 916 448-1198 (fax: 916
448-8246) or order online at
(click on "Bookstore"). Cost: $25.00.

Transit Villages in the 21st Century. Michael
Bernick, Micheal S. Bernick, Robert Burke Cervero.
Urban Land Institute. McGraw-Hill, 1996. Call 800
321-5011 (fax: 202 624-7140) or order online at
. Cost: $42.95.
Greenivays: A Guide to Planning, Design, and
Development. Chuck Flink, Loring Schwarz, and
Robert Searns. The Conservation Fund. Island Press,
1993. Order online at . Cost: $30.00. (For infor-
mation on volume discounts, call 703 525-6300.)
14 Smart Growth and Transportation
-------
The United States Environmental Protection Agency (EPA) is publishing this information
in an effort to increase public understanding of how Smart Growth can further efforts to
protect our environment. The Agency has selected the publications listed here on that basis.
However, EPA does not necessarily endorse the views expressed in any particular publica-
tion and does not promote the purchase of any organizations publications. You are urged to
contact vendors who charge a fee prior to ordering these publications.

If you or your organization want EPA to consider listing additional Smart Growth publica-
tions in the next edition of "Selected Smart Growth Publications," please contact Tim Torma
at 202 566-2864.
United States Environmental Protection Agency
Development, Community, and Environment Division
(1808T)
EPA231-R-02-001
http://www.epa.gov/smartgrowth
September 2002
-------
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(2) For AOX and chloroform limitations and

standards specified in §ubparts B and E of this part:

Production shall be defined as the annual unbleached pulp

production entering the first stage of the bleach plant

divided by the number of operating days during that year.

Unbleached pulp production shall be measured in air-dried-

metric-tons (10% moisture) of brownstock pulp entering the

bleach plant at the stage during which chlorine or chlorine-

containing compounds are first applied to the pulp. In the

case of bleach plants that use totally chlorine free

bleaching processes, unbleached pulp production shall be

measured in air-dried-metric tons (10% moisture) of

brownstock pulp entering the first stage of the bleach plant

from which wastewater is discharged. Production shall be

determined for each mill based upon past production

practices, present trends, or committed growth.

(o) TCDD. 2,3,7,8-tetrachlorodibenzo-p-dioxin.

(p) TCDF. 2,3,7,8-tetrachlorodibenzo-p-furan.

(q) Totally chlorine-free (TCP) bleaching. Pulp

bleaching operations that are performed without the use of

chlorine, sodium hypochlorite, calcium hypochlorite,

chlorine dioxide, chlorine monoxide, or any other

chlorine-containing compound.

(r) Wet Barking. Wet barking operations shall be

defined to include hydraulic barking operations and wet drum

barking operations which are those drum barking operations

801
-------
that use substantial quantities of water in either water

sprays in the barking drums or in a partial submersion of

the drums in a "tub" of water.

§ 430.02 Monitoring requirements.

This section establishes minimum monitoring frequencies

for certain pollutants. Where no monitoring frequency is

specified in this section or where the duration of the

minimum monitoring frequency has expired under paragraphs

(b)-(e) of this section, the permit writer or pretreatment

control authority shall determine the appropriate monitoring

frequency in accordance with 40 CFR 122.44 (i) or 40 CFR Part

403, as applicable.

(a) BAT, NSPS, PSES, and PSNS monitoring frequency for

chlorinated organic pollutants. The following monitoring

frequencies apply to discharges subject to Subpart B or

Subpart E of this part:
802
-------
CAS
number
1198556
2539175
2539266
2668248
32139723
56961207
57057837
58902
60712449
87865
88062
95954
1746016
51207319
67663
59473040
Pollutant
Tetrachlorocatechol
Tetrachloroguaiacol
Trichlorosyringol
4,5, 6-trichloroguaiacol
3,4, 6-trichlorocatechol
3 , 4 , 5 - trichlorocatechol
3 , 4 , 5-trichloroguaiacol
2,3,4, 6-tetrachlorophenol
3,4, 6-trichloroguaiacol
Pentachlorophenol
-------
CAS number
1198556
2539175
2539266
2668248
32139723
56961207
57057837
58902
60712449
87865
88062
95954
1746016
51207319
67663
Pollutant
Tetrachlorocatechol
Tetrachloroguiacol
Trichlorosyringol
4,5, 6-trichlorqguaiacol
3,4, 6-trichlorocatechol
3,4, 5 - trichlorocatechol
3,4,5 - trichloroguaiacol
2,3,4, 6-tetrachlorophenol
3 , 4 , 6 -trichloroguaiacol
Pentachlorophenol e
2,4, 6-trichlorophenol e
2,4, 5 - trichlorophenol e
2,3,7,8-TCDD
2,3,7,8-TCDF
Chloroform
Minimum Monitoring
Frequency
non-ECFa
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
weekly
Advanced
ECF b'f
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
TCF c
d
d
d
d
d
d
d
d
d
d
d
d
d
d
d
non-ECF: Pertains to any fiber line that does not use exclusively
ECF or TCF bleaching processes.
Advanced ECF: Pertains to any fiber line that uses exclusively
Advanced ECF bleaching processes, or exclusively ECF and TCF
bleaching processes as disclosed by the discharger in its permit
application under 40 CFR 122.21(g)(3) and certified under 40 CFR
122.22. Advanced ECF consists of the use of extended
delignification or other technologies that achieve at least the
Tier I performance levels specified in § 430.24(b) (4) (i) .
TCF: Pertains to any fiber line that uses exclusively TCF
bleaching processes, as disclosed by the discharger in its permit
application under 40 CFR 122.21(g)(3) and certified under 40 CFR
122.22.
This regulation does not specify a limit for this pollutant for
TCF bleaching processes.
Monitoring frequency does not apply to this compound when used as
a biocide. The permitting authority must determine the
appropriate monitoring frequency for this compound, when used as a
biocide, under 40 CFR 122.44(i).
805
-------
f Monitoring requirements for these pollutants by mills certifying
as Advanced ECF in their NPDES permit application or other
communication to the permitting authority will be suspended after
one year of monitoring. The permitting authority must determine
the appropriate monitoring frequency for these pollutants beyond
that time under 40 CFR 122.44 (i).

(d) Reduced, monitoring frequencies for AOX under the

Voluntary Advanced Technology Incentives Program (year one).

The following monitoring frequencies apply to direct

dischargers enrolled in the Voluntary Advanced Technology

Incentives Program established under Subpart B of this part

for a duration of one year after achievement of the

applicable BAT limitations specified in § 430.24(b)(4)(i) or

NSPS specified in § 430.25(c)(2):
CAS
Number
59473040
Pollutant
AOX
Non-ECF , any
Tier a
daily
Advanced
ECF, any
Tier b
weekly
TCF , any
Tier c
none
specified
a non-ECF: Pertains to any fiber line that does not use exclusively
ECF or TCF bleaching processes.
b Advanced ECF: Pertains to any fiber line that uses exclusively
Advanced ECF bleaching processes or exclusively ECF and TCF
bleaching processes, as disclosed by the discharger in its permit
application under 40 CFR 122.21(g)(3) and certified under 40 CFR
122.22. Advanced ECF consists of the use of extended
delignification or other technologies that achieve at least the
Tier I performance levels specified in § 430.24(b) (4) (i) .
c TCF: Pertains to any fiber line that uses exclusively TCF
bleaching processes, as disclosed by the discharger in its permit
application under 40 CFR 122.21(g)(3) and certified under 40 CFR
122.22.

(e) Reduced monitoring frequencies for AOX under the

Voluntary Advanced Technology Incentives Program (years two

through five). The following monitoring frequencies apply
806
-------
to mills enrolled in the Voluntary Advanced Technology

Incentives Program established under Subpart B of this part

for a duration of four years starting one year after

achievement of the applicable BAT limitations specified in §

430.24(b) (4) (i) or NSPS specified in § 430.25 (c) (2) :
807
-------

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CX3
-------
(3) Immediate Process Area: The location at the mill

where pulping, screening, knotting, pulp washing, pulping

liquor concentration, pulping liquor processing, and

chemical recovery facilities are located, generally the

battery limits of the aforementioned processes. "Immediate

process area" includes spent pulping liquor storage and

spill control tanks located at the mill, whether or not they

are located in the immediate process area.

(4) Intentional Diversion; The planned removal of

spent pulping liquor, soap, or turpentine from equipment

items in spent pulping liquor, soap, or turpentine service

by the mill for any purpose including, but not limited to,

maintenance, grade changes, or process shutdowns.

(5) Mill: The owner or operator of a direct or

indirect discharging pulp, paper, or paperboard

manufacturing facility subject to this section.

(6) Senior Technical Manager: The person designated by

the mill manager to review the BMP Plan. The senior

technical manager shall be the chief engineer at the mill,

the manager of pulping and chemical recovery operations, or

other such responsible person designated by the mill manager

who has knowledge of and responsibility for pulping and

chemical recovery operations.

(7) Soap; The product of reaction between the alkali

in kraft pulping liquor and fatty acid portions of the wood,

809
-------
turpentine that do occur. BMPs must be developed according

to best engineering practices and must be implemented in a

manner that takes into account the specific circumstances at

each mill. The BMPs are as follows:

(1) The mill must return spilled or diverted spent

pulping liquors, soap, and turpentine to the process to the

maximum extent practicable as determined by the mill,

recover such materials outside the process, or discharge

spilled or diverted material at a rate that does not disrupt

the receiving wastewater treatment system.

(2) The mill must establish a program to identify and

repair leaking equipment items. This program must include:

(i) Regular visual inspections (e.g., once per

day) of process areas with equipment items in spent pulping

liquor, soap, and turpentine service;

(ii) Immediate repairs of leaking equipment

items, when possible. Leaking equipment items that cannot

be repaired during normal operations must be identified,

temporary means for mitigating the leaks must be provided,

and the leaking equipment items repaired during the next

maintenance outage;

(iii) Identification of conditions under which

production will be curtailed or halted to repair leaking

equipment items or to prevent pulping liquor, soap, and

turpentine leaks and spills; and

(iv) A means for tracking repairs over time to

811
-------
identify those equipment items where upgrade or replacement
may be warranted based on frequency and severity of leaks,
spills, or failures.
(3) The mill must operate continuous, automatic
monitoring systems that the mill determines are necessary to
detect and control leaks, spills, and intentional diversions
of spent pulping liquor,' soap, and turpentine. These
monitoring systems should be integrated with the mill
process control system and may include, e.g., high level
monitors and alarms on storage tanks; process area
conductivity (or pH) monitors and alarms; and process area
sewer, process wastewater, and wastewater treatment plant
conductivity (or pH) monitors and alarms.
(4) The mill must establish a program of initial and
refresher training of operators, maintenance personnel, and
other technical and supervisory personnel who have
responsibility for operating, maintaining, or supervising
the operation and maintenance of equipment items in spent
pulping liquor, soap, and turpentine service. The refresher
training must be conducted at least annually and the
training program must be documented.
(5) The mill must prepare a brief report that
evaluates each spill of spent pulping liquor, soap, or
turpentine that is not contained at the immediate process
area and any intentional diversion of spent pulping liquor,
soap, or turpentine that is not contained at the immediate

" 812
-------
containment for spent pulping liquor bulk storage tanks.

(8) The mill must install•and maintain secondary

containment for turpentine bulk storage tanks.

(9) The mill must install and maintain curbing, diking

or other means of isolating soap and turpentine processing

and loading areas from the wastewater treatment facilities.

(10) The mill must conduct wastewater monitoring to

detect leaks and spills, to track the effectiveness of the

BMPs, and to detect trends in spent pulping liquor losses.

Such monitoring must be performed in accordance with

paragraph (i) of this section.

(d) Requirement to develop a BMP Plan. (1) Each mill

subject to this section must prepare and implement a BMP

Plan. The BMP Plan must be based on a detailed engineering

review as described in paragraphs (d)(2) and (3) of this

section. The BMP Plan must specify the procedures and the

practices required for each mill to meet the requirements of

paragraph (c) of this section, the construction the mill

determines is necessary to meet those requirements including

a schedule for such construction, and the monitoring program

(including the statistically derived action levels) that

will be used to meet the requirements of paragraph (i) of

this section. The BMP Plan also must specify the period of

time that the mill determines the action levels established

under paragraph (h) of this section may be exceeded without

triggering the responses specified .in paragraph (i) of this

814
-------
section.

(2) Each mill subject to this section must conduct a

detailed engineering review of the pulping and chemical

recovery operations --- including but not limited to process

equipment, storage tanks, pipelines and pumping systems,

loading and unloading facilities, and other appurtenant

pulping and chemical recovery equipment items in spent

pulping liquor, soap, and turpentine service -- for the

purpose of determining the magnitude and routing of

potential leaks, spills, and intentional diversions of spent

pulping liquors, soap, and turpentine during the following

periods of operation:

(i) Process start-ups and shut downs;

(ii) Maintenance;

(iii) Production grade changes;

(iv) Storm or other weather events;

(v) Power failures; and

(vi) Normal operations.

(3) As part of the engineering review, the mill must

determine whether existing spent pulping liquor containment

facilities are of adequate capacity for collection and

storage of anticipated intentional liquor diversions with

sufficient contingency for collection and containment of

spills. The engineering review must also consider:

(i) The need for continuous, automatic monitoring

systems to detect and control leaks and spills of spent

815
-------
pulping liquor, soap, and turpentine;

(ii) The need for process wastewater diversion

facilities to protect end-of-pipe wastewater treatment

facilities from adverse effects of spills and diversions of

spent pulping liquors, soap, and turpentine;

(iii) The potential for .contamination of storm water

from the immediate process areas; and

(iv) The extent to which segregation and/or collection

and treatment of contaminated storm water from the immediate

process areas is appropriate.

(e) Amendment of BMP Plan. (1) Each mill subject to

this section must amend its BMP Plan whenever there is a

change in mill design, construction, operation, or

maintenance that materially affects the potential for leaks

or spills of spent pulping liquor, turpentine, or soap from

the immediate process areas.

(2) Each mill subject to this section must complete a

review and evaluation of the BMP Plan five years after the

first BMP Plan is prepared and, except as provided in

paragraph (e)(1) of this section, once every five years
^) .
thereafter. As a result of this review and evaluation, the

mill must amend the BMP Plan within three months of the

review if-the mill determines that any new or modified

management practices and engineered controls are necessary

to reduce significantly the likelihood of spent pulping

liquor, soap, and turpentine leaks, spills, or intentional

816
-------
(ii) Records of initial and refresher training

conducted in accordance with paragraph (c)(4) of this

section;

(iii) Reports prepared in accordance with

paragraph (c)(5) of this section; and

(iv) Records of monitoring required by paragraphs

(c)(10) and (i) of this section.

(h) Establishment of wastewater treatment system

influent action levels. (1) Each mill subject to this

section must conduct a monitoring program, described in

paragraph (2) of this section, for the purpose of defining

wastewater treatment system influent characteristics (or

action levels), described in paragraph (3) of this section,

that will trigger Requirements to initiate investigations on

BMP effectiveness and to take corrective action.

(2) Each mill subject to this section must employ the

following procedures in order to develop the action levels

required by paragraph (h) of this section:

(i) Monitoring parameters. The mill must collect

24-hour composite samples and analyze the samples for a

measure of organic content (e.g., Chemical Oxygen Demand

(COD) or Total Organic Carbon (TOC)). Alternatively, the

mill may use a measure related to spent pulping liquor

losses measured continuously and averaged over 24 hours

(e.g., specific conductivity or color).

(ii) Monitoring locations. For direct

818
-------
dischargers, monitoring must be conducted at the point
influent enters the wastewater treatment system. For
indirect dischargers monitoring must be conducted at the
point of discharge to the POTW. For the purposes of this
requirement, the mill may select alternate monitoring
point(s) in order to isolate possible sources of spent
pulping liquor, soap, or turpentine from other possible
sources of organic wastewaters that are tributary to the
wastewater treatment facilities (e.g., bleach plants, paper
machines and secondary fiber operations).
(3) By the date prescribed in paragraph (j)(1)(iii) of
this section, each existing discharger subject to this
section must complete an initial six-month monitoring
program using the procedures specified in paragraph (h)(2)
of this section and must establish initial action levels
based on the results of that program. A wastewater
treatment influent action level is a statistically
determined pollutant loading determined by a statistical
analysis of six months of daily measurements. The action
levels must consist of a lower action level, which if
exceeded will trigger the investigation requirements
described in paragraph (i) of this section, and an upper
action level, which if exceeded will trigger the corrective
action requirements described in paragraph (i) of this
section.
819
-------
(4) By the date prescribed in paragraph (j)(1)(vi) of

this section, each existing discharger must complete a

second six-month monitoring program using the procedures

specified in paragraph (h)(2) of this section and must

establish revised action levels based on the results of that

program. The initial action levels shall remain in effect

until replaced by revised action levels.

(5) By the date prescribed in paragraph (j) (2) of this

section, each new source subject to this section must

complete a six-month monitoring program using the procedures

specified in paragraph (h) (2) of this section and must

develop a lower action level and an upper action level based

on the results of that program.

(6) Action levels developed under this paragraph must

be revised using six months of monitoring data after any

change in mill design, construction, operation, or

maintenance that materially affects the potential for leaks

or spills of spent pulping liquor, soap, or turpentine from

the immediate process areas.

(i) Monitoring, corrective action, and reporting

requirements. (1) Each mill subject to this section must

conduct daily monitoring of the influent to the wastewater

treatment system in accordance with the procedures described

in paragraph (h)(2) of this section for the purpose of

detecting leaks and spills, tracking the effectiveness of

the BMPs, and detecting trends in spent pulping liquor

820
-------
once per year.

(j) Compliance deadlines. (1) Existing direct and

indirect dischargers. Except as provided in paragraph

(j)(2) of this section for new sources, indirect discharging

mills subject to this section must meet the deadlines set

forth below. Except as provided in paragraph (j)(2) of this

section for new sources, NPDES permits must require direct

discharging mills subject to this section to meet the

deadlines set forth below. If a deadline set forth below

has passed at the time the NPDES permit containing the BMP

requirement is issued, the NPDES permit must require

•immediate compliance with such BMP requirement(s).

(i) Prepare BMP Plans and certify to the

permitting or pretreatment authority that the BMP Plan has

been prepared in accordance with this regulation not later

than [insert date 12 months after date of publication];

(ii) Implement all BMPs specified in paragraph

containment or diversion structures or the installation of

monitoring and alarm systems not later than [insert date 12

months after date of publication].

(iii) Establish initial action levels required by

paragraph (h)(3) of this section not later than [insert date

12 months after date of publication].

(iv) Commence .operation of any new or upgraded

822
-------
after commencement of discharge, based on six months of

monitoring data obtained prior to that date in accordance

with the procedures specified in paragraph (h) (2) of this

section.

Subpart A-Dissolving Kraft Subcategory

§ 430.10 Applicability; description of the dissolving kraft

subcategory.

The provisions of this subpart apply to discharges

resulting from the production of dissolving pulp at kraft

mills.

§ 430.11 Specialized definitions.

For the purpose of this subpart, the general

definitions, abbreviations, and methods of analysis set

forth in 40 CFR part 401 and § 430.01 of this part shall

apply to this subpart.

§ 430.12 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

(a) Except as provided in 40 CFR 125.30 through

125.32, any existing point source subject to this subpart

must achieve the following effluent limitations representing

the degree of effluent reduction attainable by the

application of the best practicable control technology

currently available (BPT), except that non-continuous

dischargers shall not be subject to the maximum day and

824
-------
average of 30 consecutive days limitations but shall be

subject to annual average effluent limitations:

Subpart A
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
23.6
37.3
(l)
Average of daily
values for 30
consecutive days
12.25
20.05
(l)
Non - cont inuous
dischargers
6.88
11.02
H.
^Within the range of 5.0 to 9.0 at all times.

(b) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of wet barking

operations, which may be discharged by a point source

subject to the provisions of this subpart. These

limitations are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated using

the proportion of the mill's- total production due to use of

logs which are subject to such operations. Non-cont inuous

dischargers shall not be subject to the maximum day and

average of 30 consecutive days limitations, but shall be

subject to annual average effluent limitations:
825
-------
Subpart A
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
3.2
6.9
C1)
Average of daily
values for 30
consecutive days
1.7
3.75
(a)
Non-continuous
dischargers
(Annual Average)
0.95
2.0
H
JWithin the range of 5.0 to 9.0 at all times.

or quality of pollutants or pollutant parameters, controlled

by this section, resulting from the use of log washing or

chip washing operations, which may be discharged by a point

source subject to the provisions of this subpart. These

limitations are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs and/or chips which are subject to such operations. Non-

continuous dischargers shall not be subject to the maximum

day and average of 30 consecutive days limitations, but

shall be subject to the annual average effluent limitations:
826
-------
Subpart A
Pollutant
or
pollutant
property
BODS
TSS
pH
-. . BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
, Continuous dischargers
Maximum for any 1
day
0.35
0.70
H
Average of daily
values for 30
consecutive days
0.2
0.4
(*)
Non-continuous
dischargers
(Annual Average)
0.1
0.2
H
tne range of 5.0 to 9.0 at air times.

(d) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of log flumes or log

ponds, which may be discharged by a point source subject to

the provisions of this subpart. These limitations are in

addition to the limitations set forth in paragraph (a) of

this section and shall be calculated using the proportion of

the mill's total production due to use of logs which are

subject to such operations. Non-continuous dischargers

shall not be subject to the maximum day and average of 30

consecutive days limitations but shall be subject to the

annual average effluent limitations:
827
-------
Subpart A
Pollutant
or
pollutant
property •
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.6
1.45
(x)
Average of daily
values for 30
consecutive days
0.35
0.8
t1)
Non-continuous
dischargers
(Annual Average)
0.2
0.4
(x)
Within the range of 5.0 to 9.0 at all times.

§ 430.13 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart shall achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT): The

limitations shall be the same as those specified for

conventional pollutants (which are defined in 40 CFR 401.16)

in § 430.12 of this subpart for the best practicable control

technology currently available (BPT).

§ 430.14 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any
828
-------
existing point source subject to this subpart where

chlorophenolic-containing biocides are used must achieve the

following effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT). Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg (lb/1000 Ib) but shall be

subject to concentration limitations. Concentration

limitations are only applicable to non-continuous

dischargers. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

Subpart A
Pollutant or
pollutant property
Pentachlorophenol
Tri chlorophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0025
0.016
Milligrams/liter
(0.011) (55.1)/y
(0.068) (55.1)/y
y = wastewater discharged in kgal per ton of product
§ 430.15 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the

following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BOD5 and TSS, but shall be subject to annual
829
-------
average effluent limitations. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply,

where provided. Concentration limitations will only apply

to non-continuous dischargers. Only facilities where

chlorophenolic-containing biocides are used shall be subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are not

using these biocides:

Subpart A
Pollutant or
pollutant property
BODS
TSS
PH

Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
15.6
27.3
t1 )
Average of
daily
values for
30
consecutive
days
8.4
14.3
(x )
Non-continuous
Dischargers
(Annual Average)
4.4
7.5
(x )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0025
0.016
Milligrams/liter
(0.012) (50.7)/y
(0.074) (50.7)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
830
-------
§ 430.16 Pretreatment standards for existing sources

(PSES).

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants, into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides. Permittees not

using chlorophenolic-containing biocides must certify to the

permit-issuing authority that they are not using these

biocides. PSES must be attained on or before July 1, 1984:

Subpart A
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.011) (55.1)/y
(0.082) (55.1)/y
Kg/kkg (or pounds per
1,000 lb) of product3
0.0025
0.019
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
§ 430.17 Pretreatment standards for new sources (PSNS).

Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works "must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources (PSNS) if it uses chlorophenolic-containing
831
-------
biocides. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

Subpart A
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.012) (50.7)/y
(0.089) (50.7)/y
Kg/kkg (or pounds per
1,000 Ib) of producta
0.0025
0.019
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart B-Bleached Papergrade Kraft and Soda Subcategory

§ 430.20 Applicability; description of the bleached

papergrade kraft and soda subcategory.

The provisions of this subpart apply to discharges

resulting from: the production of market pulp at bleached

kraft mills; the integrated production of paperboard, coarse

paper, and tissue paper at bleached kraft mills; the

integrated production of pulp and fine papers at bleached

kraft mills; and the integrated production of pulp and paper

at soda mills.

§ 430.21 Specialized definitions.

(a) The general definitions, abbreviations, and

methods of analysis set forth in 40 CFR part 401 and §

430.01 of this part apply to this subpart.
832
-------
(b) Baseline BAT limitations or NSPS means the BAT

limitations specified in §430.24(a)(1) or (2), as

applicable, and the NSPS specified in § 430.25(b)(1) or (2),

as applicable, that apply to any direct discharger that is

not "enrolled" in the "Voluntary Advanced Technology

Incentives Program."

that a mill intends to participate in the "Voluntary

Advanced Technology Incentives Program." A mill can enroll

by indicating its intention to participate in the program

either as part of its application for a National Pollutant

Discharge Elimination System (NPDES) permit, or through

separate correspondence to the permitting authority as long

as the mill signs the correspondence in accordance with 40

CFR 122.22.

(d) Existing effluent quality means the level at which

the pollutants identified in § 430.24(a)(1) are present in

the effluent of a mill "enrolled" in the "Voluntary Advanced

Technology Incentives Program."

(e) Kappa number is a measure of the lignin content in

unbleached pulp, determined after pulping and prior to

bleaching.

(f) Voluntary Advanced Technology Incentives Program

is the program established under § 430.24(b) (for existing

direct dischargers) and § 430.25 (c) (for new direct

dischargers) whereby participating mills agree to accept

833
-------
enforceable effluent limitations and conditions in their

NPDES permits that are more stringent than the "baseline BAT

limitations or NSPS" that would otherwise apply, in exchange

for regulatory- and enforcement-related rewards and

incentives.

§ 430.22 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

(a) Except as provided in 40 CFR 125.30 through

125.32, any existing point source subject to this subpart

must achieve the following effluent limitations representing

the degree of effluent reduction attainable by the

application of the best practicable control technology

currently available (BPT):

Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where market pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
15.45
30.4
D
Average of daily
values for 30
consecutive days
8.05
16.4
(l)
Non-continuous
dischargers
(Annual Average)
4.52
9.01
C1)
*Within the range of 5.0 to 9.0 at all times.
834
-------
Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
13.65
24.0
(l)
Average of daily
values for 30
consecutive days
7.1
12.9
C1)
Non- continuous
dischargers
(Annual Average)
3.99
7.09
H
tne range or 5.0 to 9.0 at all times.

Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where pulp and fine papers are
produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
10.6
22.15
(l)
Average of daily
values for 30
consecutive days
5.5
11.9
(*)
Non - cont inuous
dischargers
(Annual Average)
3.09
6.54
C1)
tne range or 5.0 to 9.0 at all times.
835
-------
Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
soda facilities where pulp and paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any
1 day
13.7
24.5
C1)
Average of daily
values for 30
consecutive days
7.1
13.2
H
Non-continuous
dischargers
(Annual Average)
3.99
7.25
H
Within the range of 5.0 to 9.0 at all times.

(b) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of wet barking

operations, which may be discharged by a point source

subject to the provisions of. this subpart. These

limitations are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs which are subject to such operations:
836
-------
Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
, .BPT effluent limitations for
bleached kraft facilities where market pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1 day
2.3
5.3
t1.).
Average of daily
values for 30
consecutive days
1.2
2.85
C1)
Non - cont inuous
dischargers
(Annual Average)
0.70
1.55
f1)
Within the range of 5.0 to 9.0 at all times.

Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
2.25
5.75
C1)
Average of daily
values for 30
consecutive ,days
1.2
3.1
(')
Non- cont inuous
dischargers
(Annual Average)
0 . 65
1.70
H
aWithin the range of 5.0 to 9.0 at all times.
837
-------
Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where pulp and fine papers are
produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
1.95
5.3
C1)
Average of daily
values for 30
consecutive days
1.0
2.85
(l)
Non-continuous
dischargers
(Annual Average)
0 . 55
"l.55
H
Within the range of 5.0 to 9.0 at all times.

Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
soda facilities where pulp and papers are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
2.05
5.25
(l)
Average of daily
values for 30
consecutive days
1.1
2. 8
(l)
Non- continuous
dischargers
(Annual Average )
0.60
1.55
H
lWithin the range of 5.0 to 9.0 at all times.

or quality of pollutants or pollutant parameters, controlled

by this section, resulting from the use of log washing or

chip washing operations, which may be discharged by a point

source subject to the provisions of this subpart. These

limitations are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated using
838
-------
the proportion of the mill's total production due to use of

logs and/or chips which are subject to such operations:

Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.25
0.65
D
Average of daily
values for 30
consecutive days
0.15
0.35
C1)
Non-continuous
dischargers
(Annual Average)
0.05
0.20
(*)
Within the range of 5.0 to 9.0 at all times.
839
-------
Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where pulp and fine papers are
produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.2
0.55
H
Average of daily
values for 30
consecutive days
0.1
0.3
(l)
Non- continuous
dischargers
(Annual Average)
0.05
0.15
(l)
Within the range of 5.0 to 9.0 at all times.

Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
soda facilities where pulp and papers are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.5
H
Average of daily
values for 30
consecutive days
0.1
0.25
(*)
Non-continuous
dischargers
(Annual Average)
0.05
0.15
(x)
Within the range of 5.0 to 9.0 at all times.

(d) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of log flumes or log

ponds, which may be discharged by a point source subject to

the provisions of this subpart. These limitations are in

addition to the limitations set forth in paragraph (a) of
840
-------
this section and-shall be calculated using the proportion of

the mill's total production due"to use of logs which are

subject to such operations:

Non-continuous
dischargers
(Annual Average)
0.15
0.35
P)
xWithin the range of 5.0 to 9.0 at all times.

841
-------
Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH,
BPT effluent limitations for
bleached kraft facilities where pulp and fine papers are
produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.35
1.15
(x)
Average of daily
values for 30
consecutive days
0.2
0.6
C1)
Non- continuous
dischargers
(Annual Average)
0.10
0.30
(*)
xWithin the range of 5.0 to 9.0 at all times.
Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
soda facilities where pulp and papers are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.3
1.1
C1)
Average of daily
values for 30
consecutive days
0.2
0.55
H
Non- continuous
dischargers
(Annual Average)
0.10
0-.35
t1)
Within the range of 5.0 to 9.0 at all times.

§ 430.23 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve
842
-------
the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT). The

limitations shall be the same as those specified in § 430.22

of this subpart for the best practicable control technology

currently available (BPT).

§ 430.24 Effluent limitations representing the degree of

effluent reduction attainable by the application of best

available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best available technology economically achievable (BAT).

(a) Except as provided in paragraph (b) of this

section--(1) the following effluent limitations apply with

respect to each fiber line that does not use an exclusively

TCF bleaching process, as disclosed by the discharger in its

NPDES permit application under 40 CFR 122.21(g)(3) and

certified under 40 CFR 122.22:
843
-------
Subpart B
Pollutant
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5-
trichloroguaiacol
3,4,6-
tri chloroguaiacol
4,5,6-
trichloroguaiacol
2,4, 5-trichlorophenol
2,4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol

AOX
COD
BAT effluent limitations
Maximum for any
1 day
-------
This regulation does not specify this type of limitation for this
pollutant; however, permitting authorities may do so as
appropriate.
picograms per liter.
grams per 1,000 kilograms (g/kkg).
[Reserved].
(2) The following effluent limitations apply with

respect to each fiber line that uses exclusively TCP

bleaching processes, as disclosed by the discharger in its

NPDES permit application under 40 CFR 122.21(g)(3) and

certified under 40 CFR 122.22:

Subpart B
Pollutant or
pollutant
property
AOX
COD
BAT effluent limitations (TCP)
Continuous dischargers
Maximum for
any 1 day
Monthly
average
Non- continuous
dischargers
Maximum for
any 1 day
Annual
Average
kg/kkg(or pounds per 1,000 Ib) of product
-------
quality or the discharger's current effluent limitations

established under CWA section 301(b)(2), whichever are more

stringent, for the pollutants identified in paragraph (a)(1)

of this section (with the exception of COD). For AOX, the

permitting authority must determine existing effluent

quality for each fiber line enrolled in the Voluntary

Advanced Technology Incentives Program at the end of the

pipe based on loadings attributable to that fiber line. For

the remaining pollutants, with the exception of COD, the

permitting authority must determine existing effluent

quality for each fiber line enrolled in the Voluntary

Advanced Technology Incentives Program at the point where

the wastewater containing those pollutants leaves the bleach

plant. These limitations must be recalculated each time the

NPDES permit of a discharger enrolled in the Voluntary

Advanced Technology Incentives Program is reissued, up to:

(i) [insert date 6 years from date of

publication] for all pollutants in paragraph (a)(1) of this

section except AOX; and

(ii) The date specified in paragraph

(b) (4) (ii) of this section for achieving the applicable AOX

limitation specified in paragraph (b)(4)(i).

(2) Best Professional Judgment Milestones:

Narrative or numeric limitations and/or special permit

conditions, as appropriate, established by the permitting
846
-------
authority on the basis of his or her best professional

judgment that reflect reasonable interim milestones toward

achievement of the effluent limitations specified in

paragraphs (b) (3) and (b)(4) of this section, as applicable.

(3) Six-year Milestones: By [insert date six

years from the date of publication], all dischargers

enrolled in the Voluntary Advanced Technology Incentives'

Program must achieve the following:

(i) The effluent limitations specified in

paragraph (a)(1) of this section, except that, with respect

to AOX, dischargers subject to Tier I effluent limitations

specified in paragraph (b)(4)(i) of this section must

achieve the AOX limitation specified in that paragraph; or

(ii) For dischargers that use exclusively TCP

bleaching processes as of [insert date six years from the

date of publication}, the effluent limitations specified in

paragraph (a)(2) of this section.
847
-------
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(ii) ^Deadlines. (A) A discharger enrolled
'£ -*"

in Tier I of the Voluntary Advanced Technology Incentives

Program must achieve the Tier I limitations in paragraph

(b) (4) (i) of this section by [insert date six years from the

date of publication].

(B) A discharger enrolled in Tier II of

the Voluntary Advanced Technology Incentives Program must

achieve the Tier II limitations in paragraph (b) (4) (i) of

this section by [insert date eleven years from the date of

publication].

of the Voluntary Advanced Technology Incentives Program must

achieve the Tier III limitations in paragraph (b)(4)(i) of

this section by [insert date sixteen years from the date of

publication].

(d) The following additional effluent limitations

apply to all dischargers subject to this section in

accordance with the previous subcategorization scheme unless

the discharger certifies to the permitting authority that it

is not using these compounds as biocides. Also, for non-

continuous dischargers, concentration limitations (mg/1)

shall apply. Concentration limitations will only apply to

non-continuous dischargers:
849
-------
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0019
0.012
Milligrams/liter
(0.011) (41. 6) /y
(0.068) (41. 6) /y
y - wastewater discharged in kgal per ton of product
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations for
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0016
0.010
Milligrams /liter
(0.011) (35.4)/y
(0.068) (35.4)/y
y " wastewater discharged in kgal per ton of product
850
-------
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0014
0.0088
Milligrams /liter
(0.011) (30.9)/y
(0.068) (30.9)/y
y = wastewater discharged in kgal per ton of product
(e) Pursuant to 40 CFR 122.44(1) and 122.45(h), a

discharger must demonstrate compliance with the effluent

limitations in paragraph (a)(1) or (b)(3) of this section,

as applicable, by monitoring for all pollutants (except for

AOX and COD) at the point where the wastewater containing

those pollutants leaves the bleach plant. The permitting

authority may impose effluent limitations and/or monitoring

requirements on internal wastestreams for any other

pollutants covered in this section as appropriate under 40

CFR 122.44 (i) and 122.45(h). In addition, a discharger

subject to a limitation on total pulping area condensate,

evaporator condensate, and bleach plant wastewater flow

under paragraph (b)(4)(i) of this section, for Tier II and

Tier III, must demonstrate compliance with that limitation

by establishing and maintaining flow measurement equipment

to monitor'these flows at the point or points where they

leave the pulping area, evaporator area, and bleach plant.
851
-------
§ 430.25 New source performance standards (NSPS).

New sources subject to this subpart must achieve the

following new source performance standards (NSPS), as

applicable.

(a) The following standards apply to each new source

that commenced discharge after [insert date 10 years before

the date 60 days from the date of publication] and before

[insert date 60 days from the date pf publication} , provided

that the new source was constructed to meet these standards:

Subpart B
Pollutant
or
pollutant
property
BOD5
TSS
pH
1982 New Source Performance Standards for
bleached kraft facilities where market pulp is produced
Continuous dischargers
Maximum for any 1
day
Average of daily
values for 30
consecutive days
Non- continuous
dischargers
Annual average
kg/kkg (or pounds per 1,000 Ib)
of product
10.3
18.2
C1)
5.5
9.5
H
2.88
5.00
(l)
Within the range of 5.0 to 9.0 at all times.
852
-------
Subpart B
Pollutant
or
pollutant
property
BODS
TSS
pH
19 §2 New Source: Performance Standards for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Continuous dischargers
Maximum for any 1
day
Average of daily
values for 30
consecutive days
Non - cont inuous
dischargers
Annual average
kg/kkg (or pounds per 1,000 Ib)
of product
8.5
14.6
H
4.6
7.6
(x)
2.41
4.00
C1)
Within the range of 5.0 to 9.0 at all times.

Subpart B
Pollutant
or
pollutant
property
BODS
TSS
pH
1982 New Source Performance Standards for
bleached kraft facilities where pulp and fine papers are
produced and soda facilities where pulp and paper are
produced
Continuous dischargers
Maximum for any 1
day
Average of daily
values for 30
consecutive days
Non- continuous
dischargers
Annual average
kg/kkg (or pounds per 1,000 Ib)
of product
5.7
9.1
(l)
3.1
4.8
P)
1.62
2.53
P)
(1) Within the range of 5.0 to 9.0 at all times.

(b) Except as provided in paragraph (c) of this

section--(1) The following standards apply with respect to
853
-------
each new source fiber line that does not use an exclusively

TCP bleaching process, as disclosed by the discharger in its

NPDES permit application under 40 CFR 122.21(g)(3) and

certified under 40 CFR 122.22, and that commences discharge

after [insert date 60 days from publication] :
854
-------
Subpart B
Pollutant
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5-
trichloroguaiacol
3,4,6-
trichloroguaiacol
4,5,6-
trichloroguaiacol
2,4, 5-trichlorophenol
2,4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol

AOX
BOD5 '
TSS
pH
NSPS
Maximum for any
1 day
-------
COD
C1)
"
-------
pollutant; however, permitting authorities may do so as
appropriate.
c [Reserved].
d>, Kilograms per 1,000 kilograms (kg/kkg).
C1) Within the range of 5.0 to 9.0 at all times.

enrolled in the Voluntary Advanced Technology Incentives

Program, dischargers subject to this section must achieve:

(1) The standards specified in paragraph (b)(1) ,

of this section (except for AOX) or paragraph (b)(2) of this

section, as applicable; and
857
-------
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-------
(d) These additional standards apply to all new

sources, regardless of when they commenced discharge, in

accordance with the previous subcategorization scheme unless

the discharger certifies to the permitting authority that it

is not using these compounds as biocides. Also/ for non-

continuous dischargers, concentration limitations (mg/1)

shall apply. Concentration limitations will only apply to

non-continuous dischargers:

Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental NSPS for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0019
0.012
Milligrams /liter
(0.013) (36.6)/y
(0.077) (36. 6)/y
y = wastewater discharged in kgal per ton of product
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental NSPS for ' «
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
lb)of product
0.0016
0.010
Milligrams/liter
(0.012) (31.7)/y
(0.076) (31.7)/y
y = wastewater discharged in kgal per ton of product
859
-------
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental NSPS for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
- kg/kkg
(or pounds per 1,000
Ib) of product
0.0014
0.0088
Milligrams /liter
(0.014) (25.1)/y
. (0.084) (25.1)/y
y = wastewater discharged in kgal per ton of product
(e) Pursuant to 40 CFR 122.44(1) and 122.45 (h), a

discharger must demonstrate compliance with the limitations

in paragraph (b)(1) or (c)(1) of this section, as

applicable, by monitoring for all pollutants (except for

AOX, COD, BOD5, TSS, and pH) at the point where the

wastewater containing those pollutants leaves the bleach

plant. The permitting authority may impose effluent

limitations and/or monitoring requirements on internal

wastestreams for any other pollutants covered in this

section as appropriate under 40 CFR 122.44(i) and 122.45(h).

In addition, a discharger subject to a limitation on total

pulping area condensate, evaporator condensate, and bleach

plant wastewater flow under paragraph (c)(2) of this section

must demonstrate compliance with that limitation by

establishing and maintaining flow measurement equipment

monitoring these flows at the point or points where they

leave the pulping area, evaporator area, and the bleach
860
-------
plant.

§430.26 Pretreatment standards for existing sources (PSES)

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES).

(a) (1) The following pretreatment standards apply

with respect to each fiber line operated by an indirect

discharger subject to this section, unless the indirect

discharger discloses to the pretreatment control authority

in a report submitted under 40 CFR 403.12(b) that it uses

exclusively TCF bleaching processes at that fiber line.

These pretreatment standards must be attained on or before

[insert date 3 years from publication date]:
861
-------
Subpart B
Pollutant
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5-
trichloroguaiacol
3,4,6-
trichlproguaiacol
4,5,6-
trichloroguaiacol
2,4, 5-trichlorophenol
2,4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol
AOX
PSES
Maximum for any
1 day
-------
with respect to each fiber line operated by an indirect

discharger subject to this section if the indirect

discharger discloses to the pretreatment control authority

in a report submitted under 40 CFR 403.12(b) that it uses

exclusively TCP bleaching processes at that fiber line.

These pretreatment standards must be attained on or before

[insert date 3 years from publication date] :

Subpart B
Pollutant or
pollutant
parameter
AOX
PSES (TCF)
Maximum for any 1 day
-------
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0019
0.014
Milligrams /liter
(0.011) (41.6)/y
(0.082) (41. 6) /y
y = wastewater discharged in kgal per ton of product
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES for
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0016
. 0.012
Milligrams /liter
(0.011) (35.4)/y
(0.082) (35.4)/y
y = wastewater discharged in kgal per ton of product
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0014
0.011
Milligrams /liter
(0.011) (30.9)/y
(0.082) (30.9)/y
y =- wastewater discharged in kgal per ton of product
(c) An indirect discharger must demonstrate compliance
864
-------
with the pretreatment standards in paragraph (a)(1) of this

section by monitoring at the point where the wastewater

containing those pollutants leaves the bleach plant.

§ 430.27 Pretreatment standards for new sources (PSNS).

Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources (PSNS).

(a) (1) The following pretreatment standards apply

with respect to each fiber line that is a new source, unless

the indirect discharger discloses to the pretreatment

control authority in a report submitted under 40 CFR 403.12

that it uses exclusively TCF bleaching processes at that

fiber line:
865
-------
Subpart B
Pollutant
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5-
trichloroguaiacol
3,4,6-
trichloroguaiacol
4,5,6-
trichloroguaiacol
2,4, 5-trichlorophenol
2,4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol
AOX
PSNS
Maximum for any
1 day
-------
indirect discharger subject to this section if the indirect

discharger discloses to the pretreatment control authority

in a report submitted under 40 CFR 403.12(b) that it uses

exclusively TCP bleaching processes at that fiber line:

Subpart B
Pollutant or
pollutant
parameter
AOX
PSNS (TCF)
Maximum for any 1 day
-------
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSNS for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
lb)of product
0.0019
0.014
Milligrams /liter
(0.013) (36. 6) /y
(0.093) (36.6)/y
y — wastewater discharged in kgal per ton of product
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSNS for
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0016
0.012
Milligrams /liter
(0.012) (31.7)/y
(0.092) (31.7)/y
y « wastewater discharged in kgal per ton of product
Subpart B
Pollutant or pollutant
parameter
Pentachlorophenol
Trichlorophenol
Supplemental PSNS for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0014
0.011
Milligrams /liter
(0.014) (25.1)/y
(0.101) (25.1)/y
y - wastewater discharged in kgal per ton of product
(c) An indirect discharger must demonstrate compliance

with the pretreatment standards in paragraph (a) (1) and of
868
-------
this section by monitoring at the point where the wastewater

containing those pollutants leaves the bleach plant.

§430.28 Best management practices (BMPs).

The definitions and requirements set forth in 40 CFR

430.03 apply to facilities in this subpart.

Subpart C--Unbleached Kraft Subcategory

§ 430.30 Applicability; description of the unbleached kraft

subcategory.

The provisions of this subpart are applicable to

discharges resulting from: the production of pulp and paper

at unbleached kraft mills; the production of pulp and paper

at unbleached kraft-neutral sulfite semi-chemical (cross

recovery) mills; and the production of pulp and paper at

combined unbleached kraft and semi-chemical mills, wherein

the spent semi-chemical cooking liquor is burned within the

unbleached kraft chemical recovery system.

§ 430.31 Specialized definitions.

For the purpose of this subpart, the general

definitions, abbreviations, and methods of analysis set

forth in 40 CFR part 401 and § 430.01 of this part shall

apply to this subpart.

§ 430.32 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).
869
-------
Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best practicable control technology currently available

(BPT):

Subpart C
Pollutant
or
pollutant
property
BOD5
TSS
pH
BPT effluent limitations for
unbleached kraft facilities
Kg/kkg (or pounds per 1,000 Ib) of product
Maximum for any 1
day
5.6
12.0
- (*)
Average of daily values for 30
consecutive days
2.8
6.0
t1)
1Within the range of 6.0 to 9.0 at all times.

Subpart C
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
unbleached kraft facilities producing pulp and paper using
the unbleached kraft-neutral sulfite semi-chemical (cross
recovery) process
Kg/kkg (or pounds per 1,000 Ib) of product
Maximum for any 1
day
8.0
12.5
C1)
Average of daily values for
consecutive days
30
4.0
6.25
C1-)
Within the range of 6.0 to 9.0 at all times
870
-------
Subpart C
Pollutant
or
pollutant
property
BOD5
TSS
pH
BPT effluent limitations for
unbleached kraft facilities where pulp and paper are
-produced using a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical cooking
liquor is burned within the unbleached kraft chemical
recovery system
Kg/kkg (or pounds per 1,000 Ib) of product
Maximum for any 1
day
a
a
a
Average of daily values for 30
consecutive days
a
a
a
a [Reserved].

§ 430.33 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125,30 through 125.32, any

existing point source subject to this subpart shall achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT), except

that non-continuous dischargers shall not be subject to the

maximum day and average-of-30-consecutive-days limitations,

but shall be subject to annual average effluent limitations:
871
-------
Subpart C
Pollutant
or
pollutant
property
BODS
TSS
pH
BCT effluent limitations for
unbleached kraft facilities
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
5.6
12.0
(l)
Average of daily
values for 30
consecutive days
2.8
6.0
C1)
Non-continuoxis
di s chargers
(Annual Average)
1.9
3.6
H
Within the range of 6.0 to 9.0 at all times.

Subpart C
Pollutant
or
pollutant
property
BODS
TSS
PH
BCT effluent limitations for unbleached kraft -neutral
sulfite semi-chemical (-cross recovery) process and/or a
combined unbleached kraft and semi-chemical process,
wherein the spent semi-chemical cooking liquor is burned
within the unbleached kraft chemical recovery system
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
8.0
12.5
0)
Average of daily
values for 30
consecutive days
4.0
6.25
(l)
Non- continuous
dischargers
(Annual Average)
2.9
3.57
t1)
Within the range of 6.0 to 9.0 at all times.

§ 430.34 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart where
872
-------
chlorophenolic-containing biocides are used must achieve the

following effluent limitations representing the degree of

effluent reduction.attainable by the application of the best

available technology economically achievable (BAT). Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg (lb/1000 Ib), but shall be

subject to concentration limitations. Concentration

limitations are only applicable to non-continuous

dischargers. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Tr i ch.1 or opheno 1
BAT effluent limitations for
unbleached kraft facilities
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00058
0.00053
Milligrams/liter
(0.011) (12. 6) /y
(0.010) (12.6)/y
y = wastewater discharged in kgal per ton of product
873
-------
Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
• BAT effluent limitations for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft-neutral
sulfite semi -chemical (cross recovery) process
and/or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00064
0.00059
Milligrams/liter
(0.011) (14.0)/y
(0.010) (14.0)/y
y = wastewater discharged in kgal per ton of product
§ 430.35 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the

following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BODS and TSS, but shall be subject to annual

average effluent limitations. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply.,

where provided. Concentration limitations will only apply

to non-continuous dischargers. Only facilities where

chlorophenolic-containing biocides are used shall be subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are not

using these biocides:
874
-------
Subpart C
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
unbleached kraft facilities where
linerboard is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.4
5.8
(x )
Average of
daily
values for
30
consecutive
days
1.8
3.0
t1 )
Non-continuous
Dischargers
(Annual Average)
0 . 94 -
1.6
t1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00058
0.00053
Milligrams/
liter
(0.015) (9.4)/y
(0.013) (9.4)/y
y = wastewater discharged in kgal per ton at all times
cne range or 5.0 to 9.0 at all times.
875
-------
Subpart C
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
unbleached kraft facilities where
bag paper and other mixed products are produced)
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
5.0
9.1
t1 )
Average of daily
values for 30
consecutive days
2.7
4.8
t1 )
Non-
continuous
Dischargers
(Annual
Average )
1.4
2.5
0 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00058
0.00053
Milligrams/
liter
(0.012) (11.4)/y
(0.011) (11. 4) /y
y = wastewater discharged in kgal per ton at all times
aWithin the range of 5.0 to 9.0 at all times.
876
-------
Subpart C
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft -neutral
sulfite semi -chemical (cross recovery) process
and/or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.9
7.3
(x )
Average of
daily
values for
30
consecutive
days
2.1
3.8
(1 )
Non-continuous
Dischargers
(Annual Average)
1.1
1.9
C1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00064
0.00059
Milligrams/
liter
(0.013) (11. 5) /y
(0.012) (11.5)/y
y = wastewater discharged in kgal per ton at all times
Wtn the range of 5.0 to 9.0 at all times.

§ 430.36 Pretreatment standards for existing sources

(PSES).

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following
877
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pretreattnent standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides. Permittees not

using chlorophenolic-containing biocides must certify to the

permit-issuing authority-that they are not using those

biocides. PSES must be attained on or before July 1, 1984:

Subpart C
Pollutant or1
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
unbleached kraft facilities
Maximum for any 1 day
Milligrams/ liter
(0.011) (12. 6) /y
(0.010) (12. 6) /y
Kg/kkg (or pounds per 1,000
Ib) of product*
0.00058
0.00053
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases where POTWs find it necessary to impose mass effluent limitations.

Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Tr i chlorophenol
PSES for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft -neutral
sulfite semi-chemical (cross recovery) process
and/or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
Maximum for any 1 day
Milligrams/liter
(0.011) (14.0)/y
(0.010) (14.0) /y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00064
0.00059
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided ,as guidance in
cases where POTWs find it necessary to impose mass effluent limitations.
878
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§ 430.37 Pretreatment standards for new sources (PSNS).
(a) Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources (PSNS) if it uses chlorophenolic-containing

biocides. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they, are not using these biocides:

Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
unbleached kraft facilities where linerboard
produced
is
Maximum for any 1 day
Milligrams /liter
(0.015) (9.4)/y
(0.013) (9.4)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00058
0.00053
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in •
cases where POTWs find it necessary to impose mass effluent limitations
879
-------
Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
unbleached kraft facilities where bag paper
other mixed products are produced
and
Maximum for any 1 day
Milligrams/liter
(0.012) (11. 4) /y
(0.011) (11.4)/y
Kg/kkg (or pounds per 1,
Ib) of product2
000
0.00058
0.00053
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases where POTWs find it necessary to impose mass effluent limitations.

Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft -neutrsil
sulfite semi-chemical (cross recovery) process
and/or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
Maximum for any 1 day
Milligrams/liter
(0.013) (11.5)/y
(0.012) (11. 5) /y
Kg/kkg (or pounds per 1,000
Ib) of product*
0.00064
0.00059
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases where POTWs find it necessary to .impose mass effluent limitations.

Subpart D--Dissolving Sulfite Pulp Subcategory

§ 430.40 Applicability; description of the dissolving

sulfite pulp subcategory.

The provisions of this subpart are applicable to

discharges resulting from the production of pulp at
880
-------
dissolving sulfite mills.

§ 430.41 Specialized definitions.

For the purpose of this subpart, the general

definitions, abbreviations, and methods of analysis set

forth in 40 CFR part 401 and § 430.01 of this part shall

apply to this subpart.

§ 430.42 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

(a) Except as provided in 40 CFR 125.30 through

125.32, any existing point source subject to this subpart

must achieve the following effluent limitations representing

the degree of effluent reduction attainable by the

application of the best practicable control technology

currently available (BPT), except that non-continuous

dischargers shall not be subject to the maximum day and

average of 30 consecutive days limitations but shall be

subject to annual average effluent limitations:
881
-------
Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
dissolving sulfite pulp facilities where nitration grade
pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
41.4
70.65
(x)
Average of daily
values for 30
consecutive days
21.5
38.05
H
Non-continuous
dischargers
(Annual Average)
12.1
20.9
(*)
xWithin the range of 5.0 to 9.0 at all times
Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
dissolving sulfite pulp facilities where viscose grade
pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
44.3
70.65
t1)
Average of daily
values for 30
consecutive days
23.0
38.05
(x)
Non-continuous
dischargers
(Annual Average)
12.9
20.9
H
Within the range of 5.0 to 9.0 at all times
882
-------
S.ubpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
dissolving sulfite pulp facilities where cellophane grade
pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
48.05
70.65
(l) ' '
Average of daily
values for 30
consecutive days
24.95
38.05
(x)
Non-continuous
dischargers
(Annual Average)
14.0
20.9
P)
^Within the range of 5.0 to 9.0 at all times.
'Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
dissolving sulfite pulp facilities where acetate grade
pulp is produced
Kg/kkg (or pounds per 1,000 1'b) of product
Continuous dischargers
Maximum for any 1
day
50.80 D
70.65
(2)
Average of daily
values for 30
consecutive days
26.40 C1)
38.05
(2)
Non - c ont inuous
dischargers
(Annual Average)
14.83 (*)
20.9
(2)
BODS effluent limitations were remanded (Weyerhaeuser Company, et al v.
Costle, 590 F. 2nd 1011; D.C. Circuit 1978).
2Within the range of 5.0 to 9.0 at all times

(b) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of wet barking

operations, which may be discharged by a point source

subject to the provisions of this subpart. These
883
-------
limitations are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs which are subject to such operations. Non-continuous

dischargers shall not be subject to the maximum day and

average of 30 consecutive days limitations, but shall be

subject to annual average effluent limitations:

Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.7
0.15
C1)
Average of daily
values for 30
consecutive days
0.35
0.1
t1)
Non-continuous
dischargers
(Annual Average)
0.2
0.05
H
aWithin the range of 5.0 to 9.0 at all times.

or quality of pollutants or pollutant parameters, controlled

by this section, resulting from the use of log washing or

chip washing operations, which may be discharged by a point

source subject to the provisions of this subpart. These

limitations are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs and/or chips which are subject to such operations. Non-

continuous dischargers shall not be subject to the maximum

884
-------
day and average of 30 consecutive days limitations, but

shall be subject to the annual average effluent limitations

Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.15
C1)
Average of daily
values for 30
consecutive days
0.1
0.1
(l)
Non-continuous
dischargers
(Annual Average)
0.05
0.05
(l)
'•Within the range of 5.0 to-9.0 at all times.

(d) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of log flumes or log

ponds, which may be discharged by a point source subj ect to

the provisions of this subpart. These limitations are in

addition to the limitations set forth in paragraph (a) of

this section and shall be calculated using the proportion of

the mill's total production due to use of logs which are

subject to such operations. Non-continuous dischargers

shall not be subject to the maximum day and average of 30

consecutive days limitations but shall be subject to the

annual average effluent limitations:
885
-------
Subpart D
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.15
(*)
Average of daily
values for 30
consecutive days
0.1
0.1
(l)
Non- continuous
dischargers
(Annual Average)
0.05
0.05
C1)
aWithin the range of 5.0 to 9.0 at all times.

§ 430.43 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart shall achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT): The

limitations shall be the same as those specified for

conventional pollutants (which are defined in 40 CFR 401.16)

in § 430.42 of this subpart for the best practicable control

technology currently available (BPT).

§ 430.44 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any
886
-------
existing point source subject to this subpart where

chlorophenolic-containing biocides are used must achieve the

following effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT). Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg . (lb/1000 Ib) but shall be

subject to concentration limitations. Concentration

limitations are only applicable to non-continuous

dischargers. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
dissolving sulfite pulp facilities where
nitration, viscose, or cellophane pulps are
produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams /liter
(0.011) (66.0)/y
(0.068) (66.0)/y
y = wastewater discharged in kgal per ton of product
887
-------
Subpart D
Pollutant or
pollutant property
Pent achloropheno 1
Trichlorophenol
BAT effluent limitations for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0033
0.021
Milligrams/liter
(0.011) (72.7) /y
(0.068) (72.7) /y
y = wastewater discharged in kgal per ton of product
§ 430.15 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the

following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BOD5 and TSS, but shall be subject to annual

average effluent limitations. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply,

where provided. Concentration limitations will only apply

to non-continuous dischargers. Only facilities where

chlorophenolic-containing biocides are used shall be ^subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are not

using these biocides:
888
-------
Subpart D
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
dissolving sulfite pulp facilities where
nitration grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
26.9
40.8
f1 )
Average of
daily
values for
30
consecutive
days
14.5
21.3
(x )
Non- continuous
Dischargers
(Annual Average)
7.59
11.2
t1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams /liter
(0.012) (59.0)/y
(0.012) (59.0)/y
y = wastewater discharged in kgal per ton at all times
889
-------
Subpart D
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
dissolving sulfite pulp facilities where viscose
grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
28.7
40.8
(l )
Average of
daily
values for
30
consecutive
days
15.5
21.3
(l )
Non- continuous
Dischargers
(Annual Average)
8.12
11.2
0 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams /liter
(0.012) (59.0}/y
(0.012) (59.0)/y
y - wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
890
-------
Subpart D
Pollutant or
pollutant property
BODS
TSS
PH

Pentachlorophenol
Tr i chl or opheno 1
NSPS for
dissolving sulfite pulp facilities where
cellophane grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
31.2
40.8
't1 )
Average of
daily
values for
30
consecutive
days
16.8
21.3
(l )
Non-continuous
Dischargers
(Annual Average)
8.80
11.2
C1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams/liter
(0.012) (59.0) /y
(0.076) (59.0)/y
y = wastewater discharged in kgal per ton at all times
'•wicnxn tne range or 5.0 to 9.0 at all times.
891
-------
Subpart D
Pollutant or
pollutant property
BOP5
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
39.6
41.1
(i )
Average of
daily
values for
30
consecutive
days
21.4
21.5
C1 )
Non- continuous
Dischargers
(Annual Average)
11.2
11.3
(J )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0033
0.021
Milligrams /liter
(0 .-012) (65.7) /y
(0.075) (65.7)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.

§ 430.46 Pretreatment standards for existing sources

(PSES)..

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic- containing biocides. Permittees not
892
-------
using chlorophenolic-containing biocides must certify to the

permit-issuing authority that they are not using these

biocides. PSES must be attained on or before July 1, 1984:

Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
dissolving sulfite pulp facilities where
nitration, viscose, or cellophane grade pulps are
produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.011) (66.0) /y
(0.082) (66.0) /y
, Kg/kkg (or pounds per
1,000 Ib) of product a
0.0030
0.023
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.

Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.011) (72. 7) /y
(0.082) (72.7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0033
0.025
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to. impose mass effluent limitations.

§ 430.47 Pretreatment standards for new sources (PSNS).

Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part
893
-------
403; and achieve the following pretreatment standards for

new sources (PSNS) if it uses chlorophenolic-containing

biocides. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
dissolving sulfite pulp facilities where
nitration, viscose, or cellophane grade pulps are
produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.012) (59.0) /y
(0.092) (59.0)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0030
0.023
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitation's are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.012) (65.7) /y
(0,091) (65.7) /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0033
0.025
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
894
-------
Subpart E-Papergrade Sulfite Subcategory

§ 430.50 Applicability; description of the papergrade

sulfite subcategory.

The provisions of this subpart apply to discharges

resulting from the: integrated production of pulp and paper

at papergrade sulfite mills, where blow pit pulp washing

techniques are used; and the integrated production of pulp

and paper at papergrade sulfite mills where vacuum or

pressure drums are used to wash pulp.

§ 430.51 Specialized definitions

(a) Except as provided in paragraphs (b) and (c) of

this section, the general definitions, abbreviations, and

methods of analysis set forth in 40 CFR part 401 and

§ 430.01 of this part apply to this subpart.

(t>) Sulfite cooking-liquor is defined as bisulfite

cooking liquor when the pH of the liquor is between 3.0 and

6.0 and as acid sulfite cooking liquor when the pH is less

than 3.0.

sulfite subcategory are defined as follows:

(1) The calcium-, magnesium-, or sodium-based

sulfite pulp segment consists of papergrade sulfite mills

where pulp and paper are produced using an acidic cooking

liquor of calcium, magnesium, or sodium sulfite, unless

those mills are specialty grade sulfite mills;

895
-------
(2) The ammbnium-based sulfite pulp segment

consists of papergrade sulfite mills where pulp and paper

are produced using an acidic cooking liquor of ammonium

sulfite, unless those mills are specialty grade sulfite

mills;

(3) The specialty grade sulfite pulp segment

consists of those papergrade sulfite mills where a

significant portion of production is characterized by pulp

with a high percentage of alpha cellulose and high

brightness sufficent to produce end products such as plastic

molding compounds, saturating and laminating products, and

photographic papers. The specialty grade segment also

includes those mills where a major portion of production is

91 ISO brightness and above.

§ 430.52 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

(a) Except as provided in 40 CFR 125.30 through

125.32, any existing point source subject to this subpart
%>

must achieve the following effluent limitations representing

the' degree of effluent reduction attainable by the

application of the best practicable control technology

currently available (BPT):
896
-------
Subpart E •
[Bisulfite liquor/surface condensers]
Pollutant
or
pollutant
property
BPT effluent limitations
papergrade sulfite facilities where
techniques are used
for.
Blow pit washing
Kg/kkg (or pounds per 1,000 Ib)
Continuous dischargers
Maximum for any 1
day
Average of daily
values for 30
consecutive days
of product
Non-continuous
dischargers
(Annual Average)
BODS
31.8
16.55
9.30
TSS
43.95
23.65
12.99
pH
the range of 5.0 to 9.0 at all times.

Subpart E
[bisulfite liquor/barometric condensers]
Pollutant
or
pollutant
property
BPT effluent limitations tor
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib)
Continuous dischargers
Maximum for any 1
day '
Average of daily,
values for 30
consecutive days
product
Non-continuous
dischargers
(Annual Average)
BODS
34.7
18 .05
10.14
TSS
52.2
28.1
15.44
pH
the range or 5.0 to 9.0 at all times.
897
-------
Subpart E
[Acid sulfite liquor/surface condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
32.3
43.95
(*)
Average of daily
values for 30
consecutive days
16.8
23.65
t1)
Non- continuous
dischargers
(Annual Average )
9.44
12 .99
H
'•Within the range of 5.0 to 9.0 at all times.

Subpart E
[Acid sulfite liquor/barometric condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
35.55
52.2
(l)
Average of daily
values for 30
consecutive days
18.5
28.1
C1)
Non-continuous
dischargers
(Annual Average)
10.39
15.44
(x)
'•Within the range of 5.0 to 9.0 at all times.
898
-------
Subpart E
[Bisulfite liquor/surf.ace condensers]
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
26.7
43.95
P)
Average of daily
values for 30
consecutive days
13.9
23. 65
H
Non-continuous
dischargers
(Annual Average)
7.81
12.99
(l)
^Within the range of 5.0 to 9.0 at all times.
Note:- Limitations above do not apply to mills using continuous
digesters.

Subpart E
[bisulfite liquor/barometric condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
29.4
52.2
(*)
Average of daily
values for 30
consecutive days
15.3
28.1
0)
Non- continuous
dischargers
(Annual Average)
8 .60
15.44
t1)
the range of 5.0 to 9.0 at all times.
Note: Limitations above do not apply to mills using continuous
digesters.
899
-------
Subpart E
[Acid sulfite liquor/surface condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
29.75
43.95
H
Average of daily
values for 30
consecutive days
15.5
23.65
(l)
Non - c ont i nuou s
dischargers
(Annual Average)
8.71
12.99
(l)
Within the range of 5.0 to 9.0 at all times.
Note: Limitations above do not apply to mills using continuous
digesters. •

Subpart E
[Acid sulfite liquor/barometric condensers]
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
32.5
52.2
(l)
Average of daily
values for 30
consecutive days
16.9
28.1
(l)
Non- continuous
dischargers
(Annual Average)
9.49
15.44
(x)
Within the range of 5.0 to 9.0 at all times.
Note: Limitations above do not apply to mills using continuous
digesters.
900
-------
Subpart E
[Continuous '.digesters]
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for papergrade sulf ±te facilities
where vacuum or pressure drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day .
38.15
53.75
(')
Average of daily
values for 30
consecutive days
19.85
28.95
(l)
Non- continuous
dischargers
(Annual Average)
11.15
15.91
n
^•Within the range of 5.0 to 9.0 at all times.

(b) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of wet barking

operations, which may be discharged by a point source

subject to the provisions of this subpart. These
«»

limitations are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs which are subject to such operations:
901
-------
Subpart E
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
2.7
7.5
(*)
Average of daily
values for 30
consecutive days
1.45
3.95
C1)
Non- continuous
dischargers
(Annual Average)
0.80
2.19
C1)
Htfithin the range of 5.0 to 9.0 at all times.

Subpart E
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
3.05
7.5
t1)
Average of daily
values for 30
consecutive days
1.6
3.95
(l)
Non -continuous
dischargers
(Annual Average)
0 .90
2.19
t1)
*Within the range of 5.0 to 9.0 at all times.

or quality of pollutants or pollutant parameters, controlled

by this section, resulting from the use of log washing or

chip washing operations, which may be discharged by a.point

source subject to the provisions of this subpart. These

limitations are in addition to the limitations set forth in
902
-------
paragraph (a) of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs and/or chips which are subject to such operations:

Subpart E
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
2.. 55
(l)
Average of daily
values for 30
consecutive days
0.1
1.35
H
Non - c ont i nuou s
dischargers
(Annual Average)
0.05
0.75
t1)
Within the range of 5.0 to 9.0 at all times.

Subpart E
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.35
2.55
t1)
Average of daily
. values for 30
consecutive days
0.2
1.35
(a)
Non - cont inuous
dischargers
(Annual Average)
0.1
0.75
(l)
'•Within the range of 5.0 to 9.0 at all times.

(d) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of log flumes or log
903
-------
ponds, which may be discharged by a point source subject to

the provisions of this subpart. These limitations are in

addition to the limitations set forth in paragraph (a) of

this section and shall be calculated using the proportion of

the mill's total production due to use of logs which are

subject to such operations:

Subpart E
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulf ite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.35
1.7
n
Average of. daily
values for 30
consecutive days
0.2
0.9
(l)
Non- continuous
dischargers
(Annual Average)
0.1
0.5
(l>
xWithin the range of 5.0 to 9.0 at all times .
Subpart E
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.7
1.70
(l)
Average of daily
values for 30
consecutive days
0.35
0.9
'H
Non- continuous
dischargers
(Annual Average)
0.2 '
0.5
(^
Within the range of 5.0 to 9.0 at all times.
904
-------
§ 430.53 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT). The

limitations shall be the same as those specified for

conventional pollutants in § 430.52 of this subpart for the

best practicable control technology currently available

(BPT).

§ 430.54 Effluent limitations representing the degree of

effluent reduction attainable by the application of best

available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best available technology economically achievable (BAT).

(a) (1) The following effluent limitations apply to

all dischargers in the calcium-, magnesium-, or sodium-based

sulfite pulp segment:
905
-------
Subpart E
Production of Calcium-, Magnesium-, or Sodium-based Sulfite
Pulps•
Pollutant
or
pollutant
property
AOX
COD
BAT effluent limitations
Continuous dischargers
Maximum for
any 1 day
Monthly
Average
Non-continuous dischargers
Maximum for
any 1 day
Annual
average
kg/kkg (or pounds per 1,000 Ib) of product
-------
Subpart E- -Production of Ammonium-based Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Chloroform3
Trichlorosyringola
3,4,5- trichlorocatechol3
3 , 4 , 6-trichlorocatechola
3 , 4 , 5-trichloroguaiacola
3 , 4 , 6- trichloroguaiacol3
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pent achl oropheno 1 a

AOX
COD
BAT effluent limitations
Maximum for any
1 day
-------
the particular pollutant.
This regulation does not specify this type of limitation for this
pollutant; however, permitting authorities may do so as
appropriate.
[Reserved].
(ii) The following effluent limitations

apply to all dischargers in the ammonium-based sulfite pulp

segment with respect to each fiber line that uses

exclusively TCP bleaching processes, as disclosed by the

discharger in its NPDES permit application under 40 CFR

122.21(g)(3) and certified under 40 CFR 122.22:

Subpart E - Production of Ammonium-based Sulfite Pulps
Pollutant or
pollutant
property
AOX
COD
BAT effluent limitations (TCP)
Continuous dischargers
Maximum for
any 1 day
Monthly
average
Non-continuous
dischargers
Maximum for
any 1 day
Annual
Average
kg/kkg (or pounds per 1000 Ib) of product
-------
Subpart E--Production of Specialty Grade Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Chloroform3
Trichlorosyringola
3,4, 5 - trichlorocatechola
3,4, 6-trichlorocatechola
3,4,5 -trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2 , 4 , 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, S-tetrachlorophenola
Pentachlorophenola
.
AOX
COD
.BAT effluent limitations
Maximum for any
1 day
-------
b "
-------
using these compounds as biocides. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply.

Concentration limitations will only apply to non-continuous

dischargers::

Subpart E
Pollutant or
pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations
Maximum for any 1 day
kg/kkg
(or pounds per
1,000 Ib) of
product
0.00058exp(0.017x)
0.0036exp(0.017x)
Milligrams /liter
( (0.011) (12.67)exp(0.017x) ) /y
( (0.068) (12.67)exp(0.017x) ) /y
x = percent sulfite pulp in final product
y = wastewater discharged in kgal per ton of product
(c) Pursuant to 40 CFR 122.44(i) and 122.45(h), a

discharger must demonstrate compliance with the limitations

in paragraphs (a)(2) or (a)(3) of this section, as

applicable, by monitoring for all pollutants (except for AOX

and COD) at the point where the wastewater containing those

pollutants leaves the bleach plant. The permitting

authority may impose effluent limitations and/or monitoring

requirements on internal wastestreams for any other

pollutants covered in this section as appropriate under 40

CFR 122.44 (i) and 122.45(h) .

§ 430.55 New source performance standards (NSPS).

New sources subject to this subpart must achieve the

following new source performance standards (NSPS), as
911
-------
applicable.

(a) The following standards apply to each new source

regardless of when it commenced discharge:

Subpart E
Pollutant
or
pollutant
property
BODS
TSS
pH
1982 NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
4.38exp (0.017x)
5.81exp(0.017x)
H
Average of daily
values for 30
consecutive days
2.36exp (0.017x)
3.03exp(0.017x)
t1)
Non- continuous
dischargers
(Annual Average)
Average of daily
values for 30
consecutive days
divided by 1.91
Average of daily
values for 30
consecutive days
divided by 1.90
(*)
x = percent sulfite pulp in final product
Within the range of 5.0 to 9.0 at all times.

(b) The following standards apply with respect to each

new source fiber line that commences discharge after [insert

date 60 days from publication] .

(1) The following standards apply to all new

sources in the calcium-, magnesium-, or sodium-based sulfite

pulp segment:
912
-------
Subpart E
Production of Calcium-, Magnesium-, or Sodium-based Sulfite
Pulps
Pollutant
or
pollutant
property
AOX
COD
NSPS
Continuous dischargers
Maximum for
any 1 day
Monthly
Average
Non- continuous dischargers
Maximum for
any 1 day
Annual
average
kg/kkg (or pounds per 1,000 lt>) of product
-------
Subpart E--Production of Ammonium-based Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDF"
Chloroform*
Trichlorosyringola
3,4,5 - trichlorocatechola
3,4, 6-trichlorocatechola
3,4,5 -trichloroguaiacol3
3,4, 6 - trichloroguaiacol*
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3

AOX
COD
NSPS
Maximum for any
1 day
-------
40 CFR 122.22.
b "
-------
Subpart E--Production of Specialty Grade Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDF"
Chloroform*
Trichlorosyringol3
3 , 4 , 5- trichlorocatechola
3,4, 6-trichlorocatechola
3,4, 5 - trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechola
Tetrachloroguaiacol
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3

AOX
COD
NSPS
Maximum for any
1 day
-------
b "
-------
dischargers, concentration limitations (mg/1) shall apply.

Concentration limitations will only apply to non-continuous

dischargers:

Subpart E
Pollutant or
pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental NSPS
Maximum for any 1 day
kg/kkg
(or pounds per
1,000 Ib) of
product
0.00058exp (0.017x)
0.0036exp(0.017x)
Milligrams/ liter
( (0.015) (9.12)exp
( (0.094) (9.12) exp
(0.017x) ) /y
(0.017X) ) /y
x = percent sulfite pulp in final product
y » wastewater discharged in kgal per ton of product
(d) Pursuant to 40 CFR 122.44(i) and 122.45(h), a

discharger must demonstrate compliance with the standards in

paragraphs (b) (2) or (b) (3) of this section, as applicable,

by monitoring for all pollutants (except for AOX, COD, BOD5/

TSS, and pH) at the point where the wastewater containing

those pollutants leaves the bleach plant. The permitting

authority may impose effluent limitations and/or monitoring

requirements on internal wastestreams for any other

pollutants covered in this section as appropriate under 40

CFR 122.44 (i) and 122.45(h).

§ 430.56 Pretreatment standards for existing sources (PSES).

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

918 -
-------
comply with 40 CFR part 403; arid achieve the following

pretreatment standards for existing sources (PSES).

(a) The following pretreatment standards must be

attained on or before [insert date 3 years from publication

date] . •

(1) The following pretreatment standards apply to

all indirect dischargers in the calcium-, magnesium-, or

sodium-based sulfite pulp segment:
919
-------
Subpart E
Production of Calcium-, Magnesium-, or Sodium-based Sulfite
Pulps
Pollutant
or
pollutant
property
AOX
PSES
Maximum for any 1 day
Monthly Average
kg/kkg (or pounds per 1,000 Ib) of product:
-------
Subpart E--Production of Ammonium-based Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Trichlorosyringola
3,4, 5 - trichlorocatechola
3 , 4 , 6-trichlorocatechola
3,4, 5-trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguai.acola
2,4, 5-trichlorophenola
2,4, 6 - trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pentachlorophenol8
PSES .
Maximum for any
1 day
-------
40 CFR 403.12(b) that it uses exclusively TCP bleaching

processes at that fiber line:

Subpart E - Production of Ammonium-based Sulfite Pulps
Pollutant or
pollutant
parameter
AOX'
PSNS (TCF)
Maximum for any 1 day
-------
(3)(i) The following pretreatment standards apply

to all indirect dischargers in the specialty grade sulfite

pulp segment:

Subpart E--Production of Specialty Grade Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Trichlorosyringol3
3,4, 5 - trichlorocatechola
3,4, 6-trichlorocatechola
3,4, 5-trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2,4, 6- trichlorophenola
Tetrachlorocatechola
Tetrachloroguaiacola
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3
^PSES
Maximum for any
1 day
-------
apply with respect to each fiber line operated by an ;

indirect discharger producing specialty grade sulfite pulps

if the indirect discharger discloses to the pretreatment

control authority in a report submitted under 40 CFR

403.12(b) that it uses exclusively TCP bleaching processes

at that fiber line. These pretreatment standards must be

attained on or before [insert date 3 years from publication

date]:

Subpart E
Pollutant or
pollutant
parameter
AOX
PSES (TCP)
Maximum for any 1 day
-------
Subpart E
Pollutant or
pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES
Maximum for any 1 day
kg/kkg
(or pounds per
1,000 Ib) of
product
0.00058exp(0.017x)
O.OQ43.exp(0.017x)
Milligrams /liter
( (0.011) (12.67)exp
( (0.082) (12.67)exp
(0.017x) ) /y
(0.017x) )/y
x = percent sulfite pulp in final product
y = wastewater discharged in kgal per ton of product
(c) An indirect discharger must demonstrate compliance

with the pretreatment standards in paragraphs, (a) (2) or

(a)(3) of this section, as applicable, by monitoring for all

pollutants at the point where the.wastewater containing

those pollutants leaves the bleach plant.
925
-------
§ 430.57 Pretreatment standards for new sources (PSNS).

Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources (PSNS).

(a) (1) The following pretreatment standards apply to

each indirect discharger in the calcium-, magnesium-, or

sodium-based sulfite pulp segment that is a new source:

Subpart E
Production of Calcium-, Magnesium-, or Sodium-based Sulfite
Pulps
Pollutant
or
pollutant
property
AOX
PSNS
Maximum for any 1 day
Monthly Average
kg/kkg (or pounds per 1,000 Ib) of product
-------
Subpart E--Production of Atnm6nium-based Sulfite Pulps
Pollutant
or
pollutant property
TCDD3
TCDFa
Trichlorosyringol3
3,4, 5 - trichlorocatechol3
3, 4, 6 -trichlorocatechol3
3,4, 5 -trichloroguaiacol3
3,4, 6 -trichloroguaiacol3
4,5, 6 -trichloroguaiacol3
2,4, 5-trichloroph.enoi3
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3
PSNS
Maximum for any
1 day
-------
pretreatment control authority in a report submitted under

40 CFR 403.12(b) that it uses exclusively TCP bleaching

processes at that fiber line:

Subpart E - Production of Ammonium-based Sulfite Pulps
Pollutant or
pollutant
parameter
AOX
PSNS (TCF)
Maximum for any 1 day
-------
Subpart E--Product!oil of Specialty Grade Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Trichlorosyringola
3,4, 5 - trichlorocatechola
3,4, 6- trichlorocatechola
3,4, 5 - trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2,4, 5 - trichlorophenol3
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacola
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3
PSNS
Maximum for any
1 day
-------
pulps if the indirect discharger discloses to the
F
pretreatment control authority in a report submitted under

40 CFR 403.12(b) that it uses exclusively TCP bleaching

processes at that fiber line:

Subpart E - Production of Specialty Grade Sulfite Pulps
Pollutant or
pollutant
parameter
AOX
PSNS (TCP)
Maximum for any 1 day
-------
Subpart fe
Pollutant or
pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSNS
Maximum for any 1 day
kg/kkg
(or pounds per
1,000 Ib) of
product
0.00058exp(0.017x)
' 0.0043exp(0.017x)
Milligrams /liter
( (0.015) (9.12)exp(0.017x) ) /y
((0.114) (9.12)exp(0.017x) )/y
x = percent sulfite pulp in final product
y = wastewater discharged .in kgal per ton of product
(c) An indirect discharger must demonstrate compliance

with the pretreatment standards in paragraphs (a)(2) or

(a)(3) of this section, as applicable, by monitoring for all

pollutants at the point where the wastewater containing

those pollutants leaves the bleach plant.

§ 430.58 Best management practices (BMPs).

The definitions and requirements set forth in 40 CFR

430.03 apply to facilities in this subpart.

Subpart F--Semi-Chemical Subcategory

§ 430.60 Applicability; description of the semi-chemical

subcategory.

The provisions of this subpart are applicable to

discharges resulting from the integrated production of pulp

and paper at semi-chemical mills.
931
-------
§ 430.61 Specialized definitions.

For the purpose of this subpart, the general

definitions, abbreviations, and methods of analysis set

forth in 40 CFR part 401 and § 430.01 of this part shall

apply to this subpart.

§ 430.62 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

Except as provided in 40 CFR 125.3.0 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best practicable control technology currently available

(BPT) :

Subpart F
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations
ammonia base mills
Kg/kkg (or pounds per 1,000 Ib)
Maximum for any 1 day
8.0
10.0
(l)
for
of product
Average of daily values for
30 consecutive days
4.0 ;
5.0
H
xWithin the range of 6.0 to 9.0 at all times.
932
-------
Subpart F
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations
sodium base mills
Kg/kkg (or pounds per 1,000 Ib)
Maximum for any 1 day
8.7
11.0
(l)
for
of product
Average of daily values for
30 consecutive days
4.35
5.5
(*) .
aWithin the range .of 6.0 to 9.0 at all times.

§ 430.63 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart shall achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT): The

limitations shall be the same as those specified for

conventional pollutants (which are defined in 40 CFR 401.16)

in § 430.62 of this subpart for the best practicable control

technology currently available (BPT), except that non-

continuous dischargers shall not be subject to the maximum

day and average-of-30-consecutive-days limitations, but

shall be subject to annual average effluent limitations

determined by dividing the average-of-30-consecutive-days

limitations for BODS by 1.36 and TSS by 1.36.
933
-------
§ 430.64 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best
* • i
available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart where

chlorophenolic-containing biocides are used must achieve the

following effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT). Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg (lb/1000 Ib), but shall be

subject to concentration limitations. Concentration ;

limitations are only applicable to non-continuous

dischargers. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

Subpart F
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0012
0.00043
Milligrams /liter
(0.029) (10.3)/y
(O'.OIO) (10.3) /y
y = wastewater discharged in kgal per ton of product
§ 430.65 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the
934
-------
following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average.of 30 consecutive days effluent

limitations for BODS and TSS, but shall be subject to annual

average effluent limitations. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply,

where provided. Concentration limitations will only

apply to non-continuous dischargers. Only facilities where

chlorophenolic-containing biocides are used shall be subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are not

using these biocides:
935
-------
Subpart F
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.0
5.8
t1 )
Average of
daily
values for
30
consecutive
days
1.6
3.0
(x )
Non - c ont i nuou s
Dischargers
(Annual Average)
0.84
1.6;
C1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0012
0.00043
Milligrams /liter
(0.041) (7.3)/y
(0.014) (7.3)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.

§ 430.66 Pretreatment standards for existing sources

(PSES) .

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides. Permittees not

using chlorophenolic-containing biocides must certify to the
936
-------
permit-issuing authority that they are not using these

biocides. PSES must be attained on or before July 1, 1984:

Subpart F
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES
Maximum for any 1 day
Milligrams/ liter
(0.032) (10. 3) /y
(0.010) (10.3)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0. 0014
0.00043
y = wastewater discharged in kgal per ton of product
aTne following equivalent mass limitations are provided as guidance-in
cases when POTWs find it necessary to impose mass equivalent
limitations.

§ 430.67 Pretreatment standards for new sources (PSNS).

(a) Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for
*
new sources (PSNS) if it uses chlorophenolic-containing

biocides. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:
937
-------
Subpart F
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/ liter
(0.045) (7.3) /y
(0.014) (7.3)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0014 ;
0.00043
y = wastewater discharged in kgal per ton of product
The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass equivalent
limitations. ,

Subpart G-Mechanical Pulp Subcategory

§ 430.70 Applicability; description of the mechanical pulp

subcategory.

The provisions of this subpart are applicable to '

discharges resulting from: the production of pulp and paper

at groundwood chemi-mechanical mills; the production of pulp

and paper at groundwood mills through the application of the

thermo-mechanical process; the integrated production of pulp

and coarse paper, molded pulp products, and newsprint at

groundwood mills; and the integrated production of pulp arid

fine paper at groundwood mills.

§ 430.71 Specialized definitions.

For the purpose of this subpart, the general :

definitions, abbreviations, and methods of analysis set

forth in 40 CFR part 401 and §430.01 of this part shall
938
-------
apply to this subpart.

§ 430.72 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

(a) Except as provided in 40 CFR 125.30 through

125.32, any existing point source subject to this subpart

must achieve the following effluent limitations representing

the degree of effluent reduction attainable by the

application of the best practicable control technology

currently available (BPT), except that non-continuous

dischargers shall not be subject to the maximum day and

average of 30 consecutive days limitations but shall be

subject to annual average effluent limitations:

Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
13.5
19.75
(*)
Average of daily
values for 30
consecutive days
7. 05
10.65
n
Non-continuous
dischargers
(Annual Average )
3.96
5.85
(*)
^Within the range of 5.0 to 9.0 at all times.
939
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper! at
groundwood mills are produced through the application of
the thermo-mechanical process ;
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
10.6
15.55
(x)
Average of daily
values for 30
consecutive days
5.55
8.35
(l)
Non- continuous
dischargers
(Annual Average)
3.12
4.59
H
Within the range of 5.0 to 9.0 at all times.

Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, ;and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
7.45
12.75
(l)
Average of daily
values for 30
consecutive days
3.9
6.85
(l)
Non-continuous
dischargers
( Annua 1 Ave r age )
2.19
3.76
(*)
'•Within the range of 5.0 to 9.0 at all times.
940
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
6.B5
., 11. .75
(l).
Average, of -daily
values for 30
consecutive days
3.6
. 6.3
P)
NTon - c ont i nuou s
dischargers
(Annual Average)
2.0
3.5
P)
•"•Within the range of 5.0 to 9.0 at all times.

(b) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of wet barking

operations, which may be discharged by a point source

subject to the provisions-of this subpart. These

limitations are in addition, to the limitations set forth in

paragraph (a) of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs which are subject to such operations. Non-continuous

dischargers shall not .be subject to the maximum day and

average of 30 consecutive days limitations, but shall be

subject to annual average effluent limitations:
941
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or -pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.9
2: 6
C1)
Average of daily
values for 30
consecutive days
0.45
1.45
(l)
Non - c ont inuous
dischargers
(Annual Average)
0 .25
0.80
(x)
Within the range of 5.0 to 9.0 at all times.

Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo-mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.9
2.7
(x)
[ Average of daily
values for 30
consecutive days
0.45
1.45
t1) -
Non- continuous
dischargers
(Annual Average)
0.3
0.75
(X)
aWithin the range of 5.0 to 9.0 at all times.
942
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
1.15
2.0
H
Average of daily
values for 30
consecutive days
0.55
1.1
H
Non - c ont i nuou s
dischargers
(Annual Average)
0.30
0.60
i1)
^•Within the range of 5.0 to 9.0 at all times.
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
1^1
l.,95
(x)
Average of daily
values for 30
consecutive days
0.55
1.1
0)
Non -continuous
dischargers
(Annual Average)
0.35
0.60
(l)
^•Within the range of 5.0 to 9.0 at all times.

or quality of pollutants or pollutant parameters, controlled

by this section, resulting from the use of log washing or

chip washing operations, which may be discharged by a point
943
-------
source subject to the provisions of this subpart. These

limitations -are in addition to the limitations set forth in

paragraph (a) of this section and shall be calculated; using

the proportion of the mill's total production due to use of

logs and/or chips which are subject to such operations. Non-

continuous dischargers shall not be subject to the maximum

day and average of 30 consecutive days limitations, but

shall be subject to the annual average effluent limitations:

Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1,000 Ib) of product ;
Continuous dischargers
Maximum for any 1
day
0.05
0.25
(l)
Average of daily
values for 30
consecutive days
0.05
0.15
t1)
Non- continuous
dischargers
(Annual Average)
0.05
0.10
('),
Within the range of 5.0 to 9.0 at all times.
944
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo -mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.05
0.30
H
Average of daily
values for 30
consecutive days
0.05
0.15
C1)
Non-continuous
dischargers
(Annual Average)
0.05
0.05
(x)
1Within the range of 5.0 to 9.0 at all times.

Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.20
H
Average of daily
values for 30
consecutive days
0.05
0.15
P)
Within the range of 5.0 to 9.0 at all times .
Non - cont inuous
dischargers
(Annual Average)
0.05
0 .10
(l)
-
945
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for [
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product ;
Continuous dischargers
Maximum for any 1
day
0.15
0.2
(l)
Average of daily
values for 30
consecutive days
0.05
: 0.15
(l)
Non- continuous
dischargers'
(Annual Average)
0.05
0.10
n;
Within the range of 5.0 to 9.0 at all times.

(d) The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of log flumes or log

ponds, which may be discharged by a point source subject to

the provisions of this subpart. These limitations are in

addition to the limitations set forth in paragraph (a) of

this section and shall be calculated using the proportion of

the mill's total production due to use of logs which are

subject to such operations. Non-continuous dischargers

shall not be subject to the maximum day and average of 30:

consecutive days limitations but shall be subject to the

annual average effluent limitations:
946
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.55
(l)
Average of daily
values for 30
consecutive days
0.05
0.3
H
Non-continuous
dischargers
(Annual Average)
0.05
0.15
f1)
^Within the range of 5.0 to 9.0 at all times.

Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo-mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.60
(l)
Average of daily
values for 30
consecutive days
0.15
0.35
n
Non- continuous
dischargers
(Annual Average)
0.05
0.15
n
'Within the range of 5.0 to 9.0 at all times.
947
-------
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.25
0.45
(l)
Average of daily
values for 30
consecutive days
0.1
0.25 '
t1)
Non- continuous
dischargers
(Annual Average)
0.05
0.15
(l)'
Within the range of 5.0 to 9.0 at all times.
Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.2
0.4
C1)
Average of daily
values for 3 0
consecutive days
0.05
0.25
(')
Non- continuous
dischargers
(Annual Average)
0 .05
0.15
P)
xWithin the range of 5.0 to 9.0 at all times.

(e) For those mills using zinc hydrosulfite as a

bleaching agent in the manufacturing process, the following

effluent limitations are to be added to the base limitations

set forth in paragraph (a) of this section. Permittees not
948
-------
using zinc hydrosulfite as a bleaching agent must certify to

the permit issuing authority that they are not using this

bleaching compound. Non-continuous dischargers shall not be

subject to the maximum day and average of 30 consecutive

days effluent limitations, but shall be subject to annual

average effluent limitations:

Subpart G
Pollutant,
or
pollutant
property
Zinc
• BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1/000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.34
Average of daily
values for 30
consecutive days
0.17
Non- continuous
dischargers
(Annual Average)
0', 11
Subpart
Pollutant
or
pollutant
property
Zinc
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo-mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.26
Average of daily
values for 30
consecutive days
0.13
Non- continuous
dischargers
(Annual Average)
0. 09
949
-------
Subpart G
Pollutant
or
pollutant
property
Zinc
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product ;
Continuous dischargers
Maximum for any 1
day
0.30
Average of daily
values for 30
consecutive days
0.15
Non- continuous
dischargers
(Annual Average)
0 . 10
Subpart G
Pollutant
or
pollutant
property
Zinc
BPT effluent limitations for ;
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.275
Average of daily
values for 30
consecutive days
0.135
Non- continuous
dischargers
(Annual Average)
0.090
950
-------
§ 430.73 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

(a)(1) The following applies to: mechanical pulp

facilities where the integrated production of pulp and

coarse paper, molded pulp products, and newsprint at

groundwood mills occurs; and mechanical pulp facilities

where the integrated production of pulp and fine paper at

groundwood mills occurs:

(2) Except as provided in.40 CFR 125.30 through

125.32, any existing point source subject to this subpart

shall achieve, the following effluent limitations

representing the degree of effluent reduction attainable by

the application of the best conventional pollutant control

technology (BCT): The limitations shall be the same as those

specified for conventional pollutants (which are defined in

40 CFR 401.16) in § 430.72 of this subpart for the best

practicable control technology currently available (BPT).

(b) The following applies to mechanical pulp

facilities where pulp and paper at groundwood chemi-

mechanical mills are produced'and mechanical pulp facilities

where pulp and paper at groundwood mills are produced

through the application of the thermo-mechanical process:

[Reserved]

§ 430.74 Effluent limitations representing the degree of

951
-------
effluent reduction attainable by the application of the best

available technology economically achievable (BAT).

(a) The following applies to mechanical pulp

facilities where pulp and paper at groundwood mills are

produced through the application of the thermo-mechanical

process; mechanical pulp facilities where the integrated

production of pulp and coarse paper, molded pulp products,

and newsprint at groundwood mills occurs; and mechanical

pulp facilities where the integrated production of pulp and

fine paper at groundwood mills occurs: (1) Except as

provided in 40 CFR 125.30 through 125.32, any existing point

source subject to this subpart must achieve the following

effluent limitations representing the degree of effluent

reduction attainable by the application of the best

available technology economically achievable (BAT), except

that non-continuous dischargers shall not be subject to the

maximum day mass limitations in kg/kkg (lb/1000 Ib), but

shall be subject to concentration limitations.

Concentration limitations are only applicable to non- ,

continuous dischargers. Pentachlorophenol and

trichlorophenol limitations are only applicable at

facilities where chlorophenolic-containing biocides are

used. Permittees not using chlorophenolic-containing!

biocides must certify to the permit-issuing authority that
952
-------
they are not using these biocides. Zinc limitations are

only applicable at facilities where zinc hydrosulfite is

used as a bleaching agent. Permittees not using zinc

hydrosulfite as a bleaching agent must certify to the permit

issuing authority that they are not using this bleaching

compound:

Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
BAT effluent limitations for
mechanical pulp facilities where pulp and paper
at groundwood mills are produced through the
application of the thermo-mechanical process
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00097
0.00088
0.26
Milligrams /liter
(0.011) (21.1)/y
. . (0.010) (21.1)/y
(3.0) (21.1)/y
y = wastewater discharged in kgal per ton of product
953
-------
Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
BAT effluent limitations for ;
mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded pulp
products, and newsprint at groundwood mills
occurs
Maximum for any 1 day •
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0011
0.00099
0.30
Mi 1 1 igrams /liter
(0.011) (23. 8) /y
(0.010)' (23. 8)/y
(3.0) (23.8)/y
y '- wastewater discharged in kgal per ton of product
Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
BAT effluent limitations for
mechanical pulp facilities where the integrated
production of pulp and fine paper at groundwood
mills occurs
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0010
0.00092
0.27
Milligrams /liter
(0.011) (21. 9) /y
(0.010) (21.9)/y:
(3.0) (21.9)/y
y = wastewater discharged in kgal per ton of product
(b) The following applies to mechanical pulp

facilities where pulp and paper at groundwood chemi-

mechanical mills are produced:

[Reserved]

§ 430.75 New source performance standards (NSPS).
954
-------
(a) The following applies to mechanical pulp

facilities where pulp and paper at groundwood mills are

produced through the application of the thermo-mechanical

process; mechanical pulp facilities where the integrated

production of pulp and coarse paper, molded pulp products,

and newsprint at groundwood mills occurs; and mechanical

pulp facilities where the integrated production of pulp and

fine paper at groundwood mills occurs: (1) Any new source

subject to this subpart must achieve the following new

source performance standards (NSPS), except that non-

continuous dischargers shall not be -subject to the maximum

day and average of 30 consecutive days effluent limitations

for BOD5 and TSS, but shall be subject to annual average

effluent limitations. Also, for non-continuous dischargers,

concentration limitations (mg/1) shall apply, where

provided. Concentration limitations will only apply to non-

continuous dischargers. Pentachlorophenol and

trichlorophenol limitations are only applicable at

facilities where chlorophenolic-containing biocides are

used. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides. Zinc limitations are

only applicable at facilities where zinc hydrosulfite is

used as a bleaching agent. Permittees not using zinc

hydrosulfite as a bleaching agent must certify to the permit

issuing authority that they are not using this bleaching

955
-------
compound:
Subpart G
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Tr i chlorophenol
Zinc
: NSPS for
mechanical pulp facilities where pulp and .paper
at groundwood mills are produced through the
application of the thermo-mechanical -process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
4.6
8.7
(1 )
Average of
daily
values for
30
consecutive
days
2.5
4.6
t1 )
Non-contx nuou s
Dischargers
(Annual Average)
1.3;
2.4
t1 ).
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib), of
product
0.00097
0.00088
0.17
Milligrams /liter
(0.017) (13.8)/y
(0.015) (13.8)/y
(3.0) (13.8)/y
y = wastewater discharged in kgal per ton at all times
Htfithin the range of 5.0 to 9.0 at all times.
956
-------
Subpart G
Pollutant or
pollutant property
BODS
TSS '_
PH

,
Pentachlorophenol
Trichlorophenol
Zinc
NSPS for
mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded pulp
products, and newsprint at groundwood mills
occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
4.6
7.3
t1 )
Average of
daily
values for
30
consecutive
days
2.5
3.8
(1 )
Non- continuous
Dischargers
(Annual Average)
1.3
2.0
(* )'
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0011
0.00099
0.21
Milligrams/liter
(0. 016) (16. 8) /y
(0.014) (16. 8) /y
(3.0) (16.8)/y
y = wastewater discharged in kgal per ton at all times
JWithin the range of 5.0 to 9.0 at all times.
957
-------
Subpart G
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
Zinc
NSPS for
mechanical . pulp facilities where the integrated
production of pulp and fine paper at groundwood
mills occurs '
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.5
5 .8
• (i )
Average of
daily
values for
30
consecutive
days
1.9
3.0
. (* )
Non - c ont i nuou s
Dischargers
(Annual Average)
0.99
1.58
(x )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0010
0.00092
0.19
Milligrams/liter1
(0.016) (15. 4) /y '
(0.014) ,(15. 4) /y ;
(3.0) (15.4)/y
y = wastewater discharged in kgal per ton at all times
lWithin the range of 5.0 to 9.0 at all times.

(b) The following applies to mechanical pulp

facilities where pulp and paper at groundwood chemi-

mechanical mills are produced:

[Reserved]

§ 430.76 Pretreatment standards for existing sources

(PSES).

(a) The following applies to mechanical pulp
958
-------
facilities where pulp and paper at groundwood mills are
produced through the application of the thermo-mechanical
process; mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded pulp products,
and newsprint at groundwood mills occurs; and mechanical
pulp facilities where the integrated production of pulp and
fine paper at groundwood mills occurs: (1) Except as
provided in 40 CFR 403.7 and 403.13, any existing source
subject to this subpart that introduces pollutants into a
publicly owned treatment works must comply with 40 CFR part
403 and achieve the following pretreatment standards for
existing sources (PSES). Pentachlorophenol and
trichlorophenol limitations are only applicable at
facilities where chlorophenolic-containing biocides are
used. Permittees not using chlorophenolic-containing
biocides must certify to the permit-issuing authority that
they are not using these biocides. Zinc limitations are
only applicable at facilities where zinc hydrosulfite is
used as a bleaching agent. Permittees not using zinc
hydrosulfite as a bleaching agent must certify to the
permit-issuing authority that they are not using this
bleaching compound. PSES must be attained on or before July
1, 1984:
959
-------
Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSES for
mechanical pulp facilities where pulp and paper
at groundwood mills are produced through the
application of the thermo -mechanical process
Maximum for any 1 day
Mi 1 1 igrams / 1 i ter
(mg/1)
(0.011) (21.1)/y
(0.010) (21.1)/y
(3.0) (21.1)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00097
0.00088
0.26 ;
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSES for
mechanical pulp facilities where the integrated
production pf pulp and coarse paper, molded pulp
products,' and newsprint at groundwood mills
occurs
Maximum for any 1 day
Milligrams/ liter
(mg/1).
(0.011) (23. 8) /y
(0.010) (23. 8) /y
(3.0) (23. 8) /y
Kg/kkg (or pounds per 1,000
Ib) of product*
0.0011 ' \
0.00099
0.30
y » wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
960
-------
Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSES for
mechanical pulp facilities where the
production of pulp and fine paper at
mills occurs
integrated
groundwood
Maximum for any 1 day
Milligrams /liter
(mg/1)
(0.011) (21. 9) /y
(0.010) (21. 9) /y
(3.0) (21.9)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.0010
0.00092
0.27
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
(b) The following applies to mechanical pulp

facilities where pulp and paper at groundwood chemi-

mechanical mills are produced:

[Reserved]

§ 430.77 Pretreatment standards for new sources (PSNS).

(a) The following applies to mechanical pulp

facilities where pulp and paper at groundwood mills are

produced through the application of the thermo-mechanical

process; mechanical pulp facilities where the integrated

production of pulp and coarse paper, molded pulp products,

and newsprint at groundwood mills occurs; and mechanical

pulp facilities where the integrated production of pulp and

fine paper at groundwood mills occurs: (1) Except as

provided in 40 CFR 403.7, any new source subject to this
961
-------
subpart that introduces pollutants into a publicly owned

treatment works must comply with 40 CFR part 403 and achieve

the following pretreatment standards for new sources .(PSNS) .

Pentachlorophenol and trichlorophenol limitations are.only

applicable at facilities where chlorophenolic-containing

biocides are used. Permittees not using

chlorophenolic-containing biocides must certify to the

permit-issuing authority that they are not using these

biocides. Zinc limitations are only applicable at

facilities where zinc hydrosulfite is used as a bleaching

agent. Permittees not using zinc hydrosulfite as a bleaching

agent must certify to the permit issuing authority that they

are not using this bleaching Compound:

Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSNS for
mechanical pulp facilities where pulp and paper
at groundwood mills are produced through the
application of the thermo-mechanical process
Maximum for any 1 day
Milligrams/ liter
(mg/1)
(0.017) (13. 8) /y
(0.015) (13.8)/y
(3.0) (13. 8) /y
Kg/kkg (or pounds per 1,000
Ib) of product8
0.00097
0.00088
0.17
y - wastewater discharged in kgal ; per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
962
-------
Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSNS for
mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded pulp
products, and newsprint at groundwood .mills
occurs
Maximum for any 1 day
Milligrams/ liter
(mg/1)
(0.01S) (16.8) /y
(0.014) (16. 8) /y
(3.0) (16. 8) /y
Kg/kkg (or pounds per 1,000
Ib) of product3
0 .0011
0.00099
0.21
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSNS for
mechanical pulp facilities where the
production of pulp and fine paper at
mills occurs
integrated
groundwood
Maximum for any 1 day
Milligrams/ liter
(mg/1)
(0.016) (15.4)/y
(0.014) (15.4)/y
(3.0) (15.4)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.0010
0.00092
0.19
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations,
(b) The following applies to mechanical pulp

facilities where pulp and paper at groundwood chemi-

mechanical mills are produced:
963
-------
[Reserved]

Subpart H-Non-Wood Chemical Pulp

§ 430.80 Applicability; description of the non-wood

chemical pulp subcategory.

The provisions of this subpart are applicable to

discharges resulting from the production of pulp and paper

at non-wood chemical pulp mills. This subcategory includes,

but is not limited to, mills producing non-wood pulps from

chemical pulping processes such as kraft, sulfite, or soda.

§ 430.81 Specialized definitions.

The general definitions, abbreviations, and methods of

analysis set forth in 40 CFR 401 and § 430.01 of this part

shall apply to this subpart.

§ 430.82 Effluent limitations representing the degree of

effluent reduction attainable by the application of best

practicable control technology currently available (BPT).

[Reserved]

§ 430.83 Effluent limitations representing the degree of

effluent reduction attainable by the application of best

conventional pollutant control technology (BCT).

[Reserved]

§ 430.84 Effluent limitations representing the degree of

effluent reduction attainable by the application of best

964
-------
available technology economically achievable (BAT).

[Reserved]

§ 430.85 New source performance standards (NSPS)

[Reserved]

§ 430.86 Pretreatment standards for existing sources (PSES)

[Reserved]

§ 430.8-7 Pretreatment Standards for new sources (PSNS) .

[Reserved]

Subpart I-Secondary Fiber Deink

§ 430.90 Applicability; description of the

deink-subcategory.

The provisions of this subpart are applicable to

discharges resulting from the integrated production of pulp

and paper at deink mills.

§ 430.91 Specialized definitions.

For the purpose of this subpart, the general

definitions, abbreviations, and methods of analysis set

forth in 40 CFR part 401 and § 430.01 of this part shall

apply to this subpart.

§ 430.92 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).
965
-------
Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best practicable control technology currently available

(BPT), except that non-continuous dischargers shall not be

subject to the maximum day and average of 30 consecutive

days limitations but shall be subject to annual average

effluent limitations:

Subpart I
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
18.1
24.05
(l)
Average of daily
values for 30
consecutive days
9.4
12.95
f1)
Non- continuous
dischargers
(Annual Average)
5.3
7.12
(')
Within the range of 5.0 to 9.0 at all times.

§ 430.93 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart shall achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT): The

966
-------
limitations shall be the same as those specified for

conventional pollutants (which are defined in 40 CFR 401.16)

in § 430.92 of this subpart for the best practicable control

technology currently available (BPT).

§ 430.94 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart where

chlorophenolic-containing biocides are used must achieve the

following effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT). Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg (lb/1000 Ib) but shall be

subject to concentration limitations. Concentration

limitations are only applicable to non-continuous

dischargers. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:
967
-------
Subpart I
(Facilities where fine or tissue paper is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product '
0.0030
0.0069 i
Milligrams /liter
(0.029) (24.4)/y
(0.068) (24.4)/y
y = wastewater discharged in kgal per ton of product
Subpart I
(Facilities where newsprint is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0010
Milligrams/liter
(0.029) (24.4)/y
(0.010) (24.4)/y
y = wastewater discharged in kgal ,per ton of product
§ 430.95 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the

following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BOD5 and TSS, but shall be subject to annual

average effluent limitations. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply,
968
-------
where provided. Concentration limitations will only apply

to non-continuous dischargers. Only facilities where

chlorophenolic-containing biocides are used shall be subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are not

using these biocides:

Subpart I
[Facilities where fine paper is produced)
Pollutant or
pollutant property
BOD 5
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
5.7
8.7
C1 )
Average of
daily
values for
30
cons.ecutive
days
3.1
4.6
t1 )
Non- continuous
Dischargers
(Annual Average)
1.6
2 .4
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0069
Milligrams /liter
(0.045) (15. 9) /y
(0.104) (15. 9) /y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
969
-------
Subpart I
(Facilities where tissue paper is produced)
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
9.6
13.1
(x )
Average of
daily
values for
30
consecutive
days
5.2
6.8
t1 )
Non- continuous
Dischargers
(Annual Average)
2 .72
3.58
(x ),
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0069
Milligrams/ liter
(0.036) (19.5)/y
(0.085) (19.5)/yj
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
970
-------
Subpart I
(Facilities where newsprint is produced)
Pollutant or
pollutant property
BODS
TSS
pH '

Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers .
Maximum for any 1
day
' 6.0
12.0
(x )
Average of
daily
values for
30
consecutive
days
3.2
6.3
(l )
Non- continuous
Dischargers
(Annual Average)
1.7
3.3
(x )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0010
Milligrams /liter
(0.044) (16.2)/y
(0.015) (16.2)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
§ 430.96 Pretreatment standards for existing sources

(PSES).

(a) Except as provided in 40 CFR 403.7 and 403.13, any

e'xisting source subject to. this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides. Permittees not

using chlorophenolic-containing biocides must certify to the

971
-------
permit-issuing authority that they are not using these

biocides. PSES must be attained on or before July 1, 1984:

Subpart I :
(Facilities where fine or tissue paper is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES ;
Maximum for any 1 day
Milligrams /liter
mg/1)
(0.032) (24.4)/y
(0.082) (24.4)/y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0084 .

y = wastewater discharged in kgal per ton of product ;
* The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass equivalent
limitations.
Subpart I
(Facilities where newsprint is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES
Maximum for any 1 day
Milligram's /liter
mg/1)
(0.032) (24. 4) /y
(0.010) (24.4)/y
. Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0010 '
y f wastewater discharged in kgal Iper ton of product
• The following equivalent mas limitations are provided as guidance in
cases when POTWs find it necessary'to impose mass equivalent.
limitations.
§ 430.97 Pretreatment standards for new sources (PSNS).

(a) Except as provided :in 40 CFR 403.7, any new source

subject to this subpart that 'introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards:for
972
-------
new sources (PSNS) if it uses chlorophenolic-containing

biocides. Permittees not using chlorophenolic-containing

biocides must .certify to the permit-issuing authority that

they are not using these biocides:

Subpart I
(Facilities where fine paper is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/liter
mg/1)
(0.049) (15. 9) /y
(0.126) (15.9)/y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0084
y = wastewater discharged in kgal per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass equivalent
limitations.

Subpart I
(Facilities where tissue paper is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day •
Milligrams /liter
mg/1)
(0.040) (19.5)/y
(0.103) (19.5)/y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0 .
0033
0084
y = wastewater discharged in kgal per ton of product
The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass equivalent
limitations.
973
-------
Subpart I
(Facilities where newsprint is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/ liter
mg/1)
(0.048) (16.2)/y
(0.015) (!6.2)/y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0010
y = wastewater discharged in kgal per ton of product
* The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary! to impose mass equivalent
limitations. [

Subpart J-Secondary Fiber Non^-Deink

§ 430.100 Applicability; description of the secondary fiber

non-deink subcategory.

The provisions of this subpart are applicable to

discharges resulting from the production of: paperboard from

wastepaper; tissue paper from wastepaper without deinking at

secondary fiber mills; molded products from wastepaper

without deinking at secondary fiber mills; and builders'

paper and roofing felt from wastepaper. '

§ 430.101 Specialized definitions.

For the purpose of this subpart:

(a) Except as provided'below, the general definitions,

abbreviations, and methods of analysis set forth in 4|0 CFR

part 401 and § 430.01 of this part shall apply to this

subpart.
'. !
(b) Noncorrugating medium furnish subdivision mills
974
-------
are mills where recycled corrugating medium is not used in

the production of paperboard.

mills where only recycled corrugating medium is used in the

production of paperboard.

§ 430.102 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

(a) Except as provided in 40 CFR 125.30 through

125.32, any existing point source subject to this subpart

must achieve the following effluent limitations representing

the degree of effluent reduction attainable by the

application of the best practicable control technology

currently available (BPT):

Subpart J
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
secondary fiber non-deink facilities where paperboard from
.wastepaper is produced- -noncorrugating medium finish
subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Maximum for any 1 day
3 . 0
5.0
C1)
Average of daily values for
30 consecutive days
1.5
2.5
D
^•Within the range of 6.0 to 9.0 at all times.
975
-------
Subpart J
Pollutant
or
pollutant
property
BODS
1SS
PH
BPT effluent limitations for '
secondary fiber non-deink facilities where paperboaird from
wastepaper is produced- -corrugating medium finish
subdivision i
Kg/kkg (or pounds per 1,000 Ib) of product
i
Maximum for any 1 day
5.7
9.2
H
Average of daily values for
30 consecutive days
2.8
4.6
D !
Within the range of 6.0 to 9.0 at all times.

Subpart J
Pollutant
or
pollutant
property
BODS
TSS
pH
Setteable
Solids
BPT effluent limitations for
secondary fiber non-deink facilities where
and roofing felt from wastepaper are
Kg/kkg (or pounds per 1,000 Ib) of
Maximum for any 1 day
5.0 '
5.0 1
-------
dischargers shall not be subject to the maximum day and

average of 30 consecutive days limitations but shall be

subject to annual average effluent limitations:
•f
Subpart J
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
secondary fiber non-deink facilities where tissue from
wastepaper is produced without deinking
Kg/kkg (or pounds per 1,000 lb) of product
Continuous dischargers
Maximum for any 1
day
13.7
17.05
H
Average of daily
values for 30
consecutive days
7.1
9.2
H
Non-continuous
dischargers
(Annual Average)
4.0
5.1
(l)
Within the range of 5.0 to-9.0'at all times.

Subpart J
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
secondary fiber non-deink facilities where molded products
from wastepaper are produced without deinking
Kg/kkg (or pounds per 1,000 lb) of product
Continuous dischargers
Maximum for any 1
day ^
4.4
10.8
P)
Average of daily
values for 30
consecutive days
2.3
5.8
(x)
Non- continuous
dischargers
(Annual Average)
1.3
3.2
(l)
1Within the range of 5.0 to 9.0 at all times.

§ 430.103 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT)
977
-------
(a) Except as provided Jin 40 CFR 125.30 through

125.32, any existing point so'urce subject to this subpart

shall achieve the following effluent limitations

representing the degree of effluent reduction attainable by

the application of the best conventional pollutant control

technology (BCT): The limitations shall be the same as those

specified for conventional pollutants (which are defined in

40 CFR 401.16) in §430.102 of this subpart for the best

practicable control technology currently available (BPT).

(b) For secondary fiber non-deink facilities where

paperboard from wastepaper is produced, non-continuous
1 f

dischargers shall not be subject to the maximum day and

average-of-30-consecutive-days limitations, but shall be

subject to annual average effluent limitations determined by

dividing the average-of-30-consecutive-days limitations for

BODS and TSS by 1.77 and 2.18!.

builders'" paper and roofing felt from wastepaper are

produced, non-continuous dischargers shall not be subject to

the maximum day and average-of-30-consecutive-days

limitations, but shall be subject to annual average effluent

limitations determined by dividing the average-of-30-

consecutive-days limitations for BODS and TSS by 1.90 and

1.90. I

§ 430.104 Effluent limitations representing the degree of
978
-------
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00087
0.00030
Milligrams /liter
(0.029) (7.2)/y
(0.010) (7.2)/y
y = wastewater discharged in kgal per ton of product
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Tr i chl oropheno 1
BAT effluent -limitations for
secondary fiber non-deink facilities where
builders ' paper and roofing felt from wastepaper
are produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0017
0.00060
Milligrams /liter
(0.029) (14.4) /y
(0.010) (14.4)/y
y = wastewater discharged in kgal per ton of product
980
-------
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Tri chlorophenol
BAT effluent limitations for !
secondary fiber non-deink facilities where tissue
from wastepaper is produced without deinking
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 lt>) of
product
0.0030
0.0011
Milligrams/ liter
(0.029) (25. 2) /Y
(0.010) (25. 2) /Y
y e wastewater discharged in kgal per ton of product ,
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
secondary fiber non-deink facilities where molded
products from wastepaper are produced without:
deinking
Maximum for any 1 day \
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0026
0.00088
Milligrams/ liter
(0.029) (21.1)/y
(0.010) (21.1)/y
y s wastewater discharged in kgal per ton of product
§ 430.105 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the

following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BODS and TSS, but shall be subject to annual

average effluent limitations. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply,

981
-------
where provided. Concentration limitations will only apply

to non-continuous dischargers. Only facilities where

chlorophenblic-containing biocides are used shall be subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are not

using these biocides:

Subpart J
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced- -
noncorrugating medium furnish subdivision ^
Kg/kkg (or pounds- per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
2.6
3.5
(x )
Average of
daily
values for
30
consecutive
days
1.4
1.8
i1 )
Non-continuous
Dischargers
(Annual Average )
0.73
0.95
(a ). • •
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00087
0.00030
Milligrams/ liter
(0.065) (3.2)/y
(0.023) (3.2)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
982
-------
Subpart J
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
KTSPS for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced--
corrugating medium finish subdivision)
Kg/kkg (or pounds per 1,000 lb) of product
Continuous Dischargers
Maximum for any 1
day
3.9
4.4
(l )
Average of
daily
values for
30
consecutive
days
2.1
2.3
(x )
Non- continuous
Dischargers
(Annual Average)
1.1
1.2
(* ).
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 lb) of
product
0.00087
0.00030
Milligrams /liter
(0.065) (3.2/y
(0.023) (3.2)/y
y = wastewater discharged in kgal per ton at all times
xWithin the range of 5.0 to 9.0 at all times.
983
-------
Subpart J
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
secondary fiber non-deink facilities where
builders ' paper and roofing felt from wastepaper
are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
1.7
2.7
(l )
Average of
daily
values for
30
consecutive
days
0.94
1.40
P )
Non - cont inuous
Dischargers
(Annual Average)
0.49
0.74
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
• product
0.0017
0.00060
Milligrams /liter
(0.155) (2.7) /y
(0.053) (2.7) /y
y = wastewater discharged in kgal per ton at all times
1Within the range of 5.0 to 9.0 at all times.
984
-------
Subpart J
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
secondary fiber non-deink facilities where tissue
from wastepaper is produced without delinking
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
4.6 ;
10.2
(l )
Average of
daily
values for
30
consecutive
days
2 .5
5.3
t1 )
Non- continuous
Dischargers
(Annual Average)
1.3
2.8
(M
1 Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0011
Milligrams/ liter
(O.Q45) (16.3)/y
(0.015) (16.3)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
985
-------
Subpart J
Pollutant or
pollutant property
BODS
TSS
PH

Pentachlorophenol
Trichlorophenol
NSPS for
secondary fiber non-deink facilities where molded
products from wastepaper are produced without
de inking
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
2.1
4.4
C1 )
Average of
daily
values for
30
consecutive
days
1.1
2.3
C1 )
Non-continuous
Dischargers
(Annual Average)
0.58
1.21
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0026
0.00088
Milligrams/ liter
(0.107) (5.7) /y
(0.037) (5.7)/y
y = wastewater discharged in kgal per ton at all times
the range of 5.0 to 9.0 at all times.

§ 430.106 Pretreatment standards for existing sources

(PSES).

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides. Permittees not
986
-------
using chlorophenolic-containing biocides must certify to the

permit-issuing authority that they are not using these

biocides. PSES must be attained on or before July 1, 1984:

Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for :
secondary fiber non-deink facilities where
paperboard from wastepaper is produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (7.2) /y
(0.010) (7.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.00096
0.00030
y = wastewater discharged in kgal ,per ton of product
* The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary 'to impose mass effluent limitations.
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Tri chloropheno 1
PSES for
secondary! fiber non-deink facilities where
builders ' paper and roofing felt from wastepaper
are produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (14.4)y
(0.010) Cl4.4)y
Kg/kkg (or pounds per
1,000 Ib) of product61
0.0019
0.00060
y = wastewater discharged in kgal per ton of product
* The following equivalent mass limitations are provided as guidance .in
cases when POTWs find it necessary to impose mass effluent limitations.
987
-------
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
secondary fiber non-deink facilities where tissue
from wastepaper is produced without deinking
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (25.2)y
(0.010) (25.2/y
Kg/kkg (or pounds per
1,000 Ib) of product a
0.0034
0.0011
y = wastewater discharged in kgal per ton of product
me roiiowing equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
secondary fiber non-deink facilities where molded
products from wastepaper are produced without
deinking
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (21.1)y
(0.010) (21.1)y
Kg/kkg (or pounds per
1,000 Ib) of product3
0. 0028
0.00088
y = wastewater discharged in kgal per ton of product
cases when POTWs find it necessary to impose mass effluent limitations.

§ 430.107 Pretreatment standards for new sources (PSNS).

Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources (PSNS) if it uses chlorophenolic-containing

biocides. Permittees not using chlorophenolic-containing
988
-------
biocides must certify to theipermit-issuing authority that

they are not using these biocides:

Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Tri chloropheno 1
PSNS for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced
Maximum for any 1 day •
Milligrams/liter (mg/1)
• (0.072) (3. 2)/y
(0.023) *3.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.00096
0 .00030
y = wastewater discharged in kgal; per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
secondary fiber non-deink facilities where
builders' paper and roofing felt from wastepaper
; are produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.171) '(2.7) /y
(0.053) :(2.7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0019
0.00060
y 3 wastewater discharged in kgal per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
989
-------
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
secondary fiber non-deink facilities where tissue
from wastepaper is produced without deinking
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.049) (16.3)/y
(0.015) (16. 3) /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0034
0. 0011
y = wastewater discharged in kgal per ton of product
The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
secondary fiber non-deink facilities where molded
products from wastepaper are produced without
deinking
Maximum for any 1 day
Milligrams /liter (mg/1)
(0.118) (5.7)/y
(0.037) (5.7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0028 •
0. 00088
y = wastewater discharged in kgal per ton of product
cases when POTWs find it necessary to impose mass effluent limitations.

Subpart K-Pine and Lightweight Papers from Purchased Pulp

§ 430.110 Applicability; description of the fine and

lightweight papers from purchased pulp subcategory.

The provisions of this subpart are applicable, to

discharges resulting from the production of: fine paper at

nonintegrated mills; and lightweight paper at nonintegrated
990
-------
mills. ;

•
§ 430.111 Specialized definitions. ,

For the purpose of this subpart: ;

(a) Except as provided in paragraphs (b) and (c) of

this section, the general definitions, abbreviations, :and

methods of analysis set forth, in 40 CFR part 401 and

§ 430.01 of this part shall apply to this subpart. <

(b) Cotton fiber furnish subdivision mills are those;

mills where significant quantities of cotton fibers (equal

to or greater than 4 percent of the total product) are used

in the production of fine papers.

mills where cotton fibers are not used in the production of

fine papers. ;

§ 430.112 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best practicable control technology currently available

(BPT), except that non-continuous dischargers shall not be

subject to the maximum day and average of 30 consecutive

days limitations but shall be subject to annual average

991
-------
effluent limitations:
Subpart K
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills
where fine paper Is produced from purchased pulp- -wood
fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
8.2
11.0
t1)
Average of daily
values for 30
consecutive days
, 4.25
5.9
(l)
Non-continuous
dischargers
(Annual Average)
2 .4
3.2
P)
Within the range of 5.0 to 9.0 at all times.
Subpart K
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for non- integrated mills
where fine paper is produced from purchased pulp --cotton
fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
,17.4
24.3
C1)
Average of daily
values for 30
consecutive days
9.1
13.1
t1)
Non-continuous
dischargers
(Annual Average)
5.1
7.2
(x)
•'•Within the range of 5.0 to 9.0 at all times.
992
-------
Subpart K
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills
where lightweight papers are produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
24.1
21.6
C1)
Average of daily
values for 30
consecutive days
13 .2
10.6
(l)
Non- continuous
dischargers
(Annual Average)
7.37
6.0
(i)-
Within the range of 5..0 to 9.0 at all times.
Subpart K
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills where
lightweight papers are produced from purchased pulp--
electrical ' grade papers subdivision
Kg/kkg (or pounds per 1,000 Ib) of product :
Continuous dischargers
Maximum for any 1
day
38.0
34.2
P)
Average of daily
values for 30
consecutive days
20.9
16.7
(*)
Non - cont inuous
dischargers
(Annual Average)
11.7
9.5
(*):
Within the range of 5.0 to 9.0 at all times.

§ 430.113 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

Except as provided in 40: CFR 125.30 through 125.32, any

existing point source subject, to this subpart shall achieve
993
-------
the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT): The

limitations shall be the same as those specified for

conventional pollutants (which are defined in 40 CFR 401.16)

in § 430.102 of this subpart for the best practicable

control technology currently available (BPT).

§ 430.114 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart where

chlorophenolic-containing biocides are used must achieve the

following effluent limitations representing the degree of

effluent reduction attainable- by the application of the best

available technology economically achievable (BAT). Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg (lb/1000 Ib) but shall be

subject to concentration limitations. Concentration

limitations are only applicable to non-continuous

dischargers. Permittees not using chlorophenolic-containing
r

biocides must certify to the permit-issuing authority that

they are not using these biocides:
994
-------
Subp'art K
Pollutant or
pollutant property
Pentachlorophenol
Tr i chl oropheno 1
BAT effluent limitations for non- integrated mills
where fine paper is produced from purchased
pulp- -wood fiber furnish subdivision
Maximum for any 1 day ;
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0018
0.00064
y = wastewater discharged in kgal per ton of
Milligrams /liter
(0.029) (15 .2) /y ;
(0.010) (15.2)/y
product :
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Tr i chl or opheno 1
BAT effluent limitations for non- integrated mills
where fine paper is produced from purchased
pulp- -cotton fiber furnish subdivision
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ibj of
product
0.0051 >
0.0018
Milligrams /liter
(0.029) (42.3)/y ,
(0.010) (42.3)/y
y a wastewater discharged in kgal per ton of product
995
-------
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for non- integrated mills
where lightweight papers are produced from
purchased pulp
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0059
0.0020
Milligrams /liter
(0.029) (48.7)/y
(0.010) (48.7)/y
y = wastewater discharged in kgal per ton of product
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for non- integrated mills
where lightweight papers are produced from
purchased pulp- -electrical grade papers
subdivision
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0093
0.0032
Milligrams/ liter
(0.029) (76.9)/y
(0.010) (76.9)/y
y = wastewater discharged in kgal per ton of product
§ 430.115 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the

following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BODS and TSS, but shall be subject to annual

average effluent limitations. Also, for non-continuous

dischargers, concentration limitations (mg/1) shall apply,
996
-------
where provided. Concentration limitations will only apply

to non-continuous dischargers. Only facilities where>

chlorophenolic-containing biocides are used shall be subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are' not

using these biocides:
997
-------
Subpart K
Pollutant or
pollutant property
BODS
TSS
PH

Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills
where fine paper is produced from purchased
pulp--wood fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.5
4.4
(I )
Average of
daily
values for
30
consecutive
days
1.9
2.3
(1 )
Non- continuous
Dischargers
(Annual Average)
1.0
1.2
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0018
0.00064
Milligrams /liter
(0.047) (9.4)/y
(0.016) (9.4)/y
y = wastewater discharged in kgal per ton at all times
•'•Within the range of 5.0 to 9.0 at all times.
998
-------
Subpart K
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills
where fine paper is produced from purchased
pulp- -cotton fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
; 7-8
9.5
(l )
Average of
daily
values for
30
consecutive
days
4.2
4.9
(l )
Non- continuous
Dischargers
(Annual Average)
2.2
2.6
! t1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product ;
0.0051
0.0018
Milligrams/ liter
(0.039) (31.1)/y
(0.014) (31.1)/y:
y =s wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
999
-------
Subpart K
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Tr i chl orophenol
NSPS for non- integrated mills
where lightweight papers are produced from
purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product •
Continuous Dischargers
Maximum for any 1
day
13.7
12.0
t1 )
Average of
daily
values for
30
consecutive
days
6.7
5.2
(x )
Non- continuous
Dischargers
(Annual Average)
.4.5
3.2
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0059
0.0020
Milligrams /liter
(0.037) (38.2)/y
(0.013). (38. 2)/y
y = wastewater discharged in kgal per ton at all times
1Within the range of 5.0 to 9.0 at all times.
1000
-------
Subpart K
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills where lightweight
papers are produced from purchased pulp--
electrical grade papers subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day ;
24.1 ;
21.1 ;
1
(1 ) !
Average of
daily
values for
30
consecutive
days
11.7
9.2
(l )
Non - c ont inuous
Dischargers
(Annual Average)
7.9
5.6
(1 )
Maximum for -any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product ;
0.0093 '
0.0032 ;
Milligrams /liter
(0.033) (6S.8)/y
(0.012) (66.8) /y,
y - wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.

§ 430.116 Pretreatment standards for existing sources

(PSES).

Except as provided in 40; CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides. Permittees not

using chlorophenolic-containihg biocides must certify to the

1001
-------
permit-issuing authority that they are not using these

biocides. PSES must be attained on or before July 1, 1984:

Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills
'where fine paper is produced from purchased
pulp- -wood fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (15.2)/y
(0.010) (15.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0020
0.00064
y = wastewater discharged in kgal per ton of product
The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills
where fine paper is produced from purchased
pulp --cotton fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (42.3)/y
(0.010) (42. 3) /y-
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0056
0.0018
y = wastewater discharged in legal per ton of product
The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
1002
-------
Subpart K
' Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills
where lightweight papers are produced ;from
purchased pulp
Maximum for any 1 day
Milligrams /liter (mg/1)
(0.032) ('48. 7) /y
(0.010) (48. 7) /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0065 ;
0.0032
y s wastewater discharged in kgal; per ton of product
8 The following equivalent mass limitations are provided as guidance in
cases when POTWs find it . necessary, to impose mass effluent limitations.
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills where lightweight
papers are produced from purchased pulp--
electrical grade papers subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (76.9) /y
(0.010) (76.9)/y
Kg/kkg (or pounds per
1,000 Ib) of product*
0.010
0.0032
y s wastewater discharged in kgal^per ton of product
•The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
§ 430.117 Pretreatment standards for new sources (PSNS).

Except as provided in 40 CFR 403.7, any new source

subject to this subpart that:introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards- for
1003
-------
new sources (PSNS) if it uses chlorophenolic-containing

biocides. Permittees n6t using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using'these biocides:

Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non- integrated mills
where fine paper is produced from purchased
pulp--wood fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.052) (9.4)/y
(0.016) (9.4)/y
Kg/kkg (or pounds per
1,000 Ib) of product21
0.0020
0.00064
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non- integrated mills
where fine paper is produced from purchased
pulp- -cotton fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.044) (31.1)/y
(0.014) (31.1)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0056
0.0018
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
1004
-------
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non- integrated mills
where lightweight papers are produced from
purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.041) (38.2) /y
(0.013) (38.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0065
0.0020
y = wastewater discharged in kgal per ton of product
The following equivalent mass
cases when POTWs find it necessary
limitations
are provided as guidance in
to impose mass effluent limitations.
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Tri chloropheno 1
PSNS for non- integrated mills where lightweight
papers are produced from purchased pulp--
electrical grade papers subdivision
Maximum for any 1 day ;
Milligrams/liter (mg/1)
(0.037) (66. 8) /y
(0.012) (66.8) /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.010
0.0032
y * wastewater discharged in kgal per ton of product
* The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
1005
-------
Subpart L-Tissue, Filter, Non-woven/ and Paperboard from

Purchased Pulp

§ 430.120 Applicability; description of the tissue, filter,

non-woven, and paperboard from purchased pulp subcategory.

The provisions of this subpart are applicable to

discharges resulting from the production of: tissue papers

at nonintegrated mills; filter and non-woven papers at

nonintegrated mills'; and paperboard at nonintegrated mills.

The production of electrical grades of board and matrix

board is not included in this subpart.

§ 430.121 Specialized definitions.

For the purpose of this subpart, the general

definitions, abbreviations, and methods of analysis set

forth in 40 CFR part 401 and § 430.01 of this part shall

apply to this subpart. .

§ 430.122 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

practicable control technology currently available (BPT).

Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best practicable control technology currently available

(BPT), except that non-continuous dischargers shall not be
1006
-------
subject to the maximum day and average of 30 consecutive
days limitations but shall be subject to annual average
effluent limitations: ;
• j • ;
Subpart L
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
non- integrated mills where tissue papers are produced from
purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product :
Continuous dischargers
Maximum for any 1
day
11.4 .
10.25
(*)
Average of daily
values for 30
consecutive days
6.25
5.0
H
Non- continuous
dischargers
(Annual Average)
3 . 49
2 . 8!4
(l).
'•Within the range of 5.0 to 9.0 at all times.
Subpart L
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills where
filter and non-woven papers are produced from purchased
pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
29.5
26.6
t1)
Average of daily
values for 30
consecutive days
16.3
13.0
(l)
Non-continuous
dischargers
(Annual Average)
9.1
7.4
(1)'
Within the range of 5.0 to 9.0 at all times.
1007
-------
Subpart L
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for non- integrated mills where
paperboard is produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
6.5
5.8
t1')
Average of daily
values for 30
consecutive days
3.6
2.8
(*)

Non -continuous
dischargers
(Annual Average)
2.0
1.6
(l)

§ 430.123 Effluent limitations guidelines representing the

degree of effluent reduction attainable by the application

of the best conventional pollutant control technology (BCT).

Except as provided in 40 CFR 125.30 through 125.32, any

/ existing point source subject to this subpart shall achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology (BCT): The

limitations shall be the same as those specified for

conventional pollutants (which are defined in 40 CFR 401.16)

in §430.122 of this subpart for the best practicable control

technology currently available (BPT).

§ 430.124 Effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT).
1008
-------
Except as provided in 40' CFR 125.30 through 125.32, any

existing point source subject to this subpart where

chlorophenolic-containing biocides are used must achieve the

following effluent limitation's representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT). Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg (lb/1000 Ib) but shall;be

subject to concentration limitations. Concentration .

limitations are only applicable to non-continuous

dischargers. Permittees not |using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for -.
non- integrated mills where tissue papers are
produced from purchased pulp
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0028
0.00096;
Milligrams/ liter
(0.029) (22.9)/y
(0.010) (22.9) /y
y = wastewater discharged in kgal per ton of product
1009
-------
Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
non- integrated mills where filter and non-woven
papers are produced from purchased pulp
.Maximum for any 1 day
Kg/kkg (or pounds
per 1;000 Ib) of
product
0.0072
0.0025
Milligrams/liter
(0.029) (59. 9) /y
(0.010) (59. 9) /y
y = wastewater discharged in kgal per ton of product
Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
non- integrated mills where paperboard is produced
from purchased pulp
Maximum for any 1 day
Kg/kkg (or pounds
per 1, 000 Ib) of
product
0.0016
0.00054
Milligrams/liter
(0.029) (12. 9) /y
(0.010) (12. 9) /y
y = wastewater discharged in kgal per ton of product
§ 430.125 New source performance standards (NSPS).

Any new source subject to this subpart must achieve the

following new source performance standards (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BODS and TSS, but shall be subject to annual

average effluent limitations. Also, for non-continuous
1010
-------
dischargers, concentration limitations (mg/1) shall apply,

where provided. Concentration limitations will only apply

to non-continuous dischargers. Only facilities where

chlorophenolic-containing biocides are used shall be subject

to pentachlorophenol and trichlorophenol limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they are not

using these biocides:
1011
-------
Subpart L
Pollutant or . .
pollutant property
i
BODS
TSS
PH

"
Pentachlorophenol
Tr i chl or ophenol
NSPS for non- integrated mills where tissue papers
are produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
7.0
6.0
<* )
Average of
daily
values for
30
consecutive
days
3.4
2.6
(l )
Non-continuous
Dischargers
(Annual Average)
2.3
1.6
(x )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0.028
0.00096
Milligrams/liter
(0.035) (19.1)/y
(0.0.12) (19.1)/y
y = wastewater discharged in kgal per ton at all times
1012
-------
Subpart L
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for
non- integrated mills where filter and non-woven
papers are produced from purchased pulp
, Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
17.1
15.0 ;
'(' ) :
Average of
daily
values for
30
consecutive
days
8.3
6.6
(l )
Non-continuous
Dischargers
(Annual Average)
5.6
4.0
(J )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0072
0.0025
Milligrams /liter
(0.037) (47.5)/y!
(0.013) (47.5)/y
y = wastewater discharged in kgal per ton at all times
aWithin the range of 5.0 to 9.0 at all times.
1013
-------
Subpart L
Pollutant or
pollutant property
BODS
TSS
pH

Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills where paperboard is
produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
4. 0
3.5
(l )
Average of
daily
values for
30
consecutive
days
1.9
1.5
• ' t1 •)
Non - continuous
Dischargers
(Annual Average)
1.3
0.9
C1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0016
0.00054
Milligrams/ liter
(0.033) (11.2}/y
(0.012) (11.2)/y
y = wastewater discharged in kgal per ton at all times
'•Within the range of 5.0 to 9.0 at all.times.

§ 430.126 Pretreatment standards for existing sources

(PSES). '

Except as provided in 40 CFR 403.7 and 403.13, any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides. Permittees not

using chlorophenolic-containing biocides must certify to the
1014
-------
permit-issuing authority that they are not using these

biocides. PSES must be attained on or before July 1, 1984:

Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
non- integrated mills where tissue papers are
produced from purchased pulp ;
Maximum for any 1 day
Milligrams/liter (mg/1)
i
(0.032) (22.9) /y
(0.010) (22.9)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0031
0.00096
y m wastewater discharged in kgal per ton of product
* The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary'to impose mass effluent limitations.
Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
non-integrated mills where filter and non-woven
papers are produced from purchased pulp
Maximum for any 1 day ,
Milligrams/liter (mg/1)
(0.032) (59.9)/y
(0.010) (59. 9} /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0080
0.0025 I
y = wastewater discharged in kgal !per ton of product
* The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary!to impose mass effluent limitations
1015
-------
Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills where paperboard is
produced from purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (12. 9) /y
(0.010) (12.9)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0017
0.00054
y = wastewater discharged in kgal per ton of product
The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
§ 430.127 Pretreatment standards for new sources (PSNS).

Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources (PSNS) if it uses chlorophenolic-containing

biocides. Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that'

they are not using these biocides:
1016
-------
Subpart L
Pollutant or
pollutant property
Pentach.loropb.enol
Trichlorophenol
PSNS for non- integrated mills where tissue papers
are produced from purchased pulp
Maximum for any 1 day
Milligrams/liter (tng/1)
(0.038) (19.1) /y
(0.012) (19.1) /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0031 :
0.00096
y = wastewater discharged in kgal per ton of product
* The following equivalent mass limitations are provided as guidance in
cas.es when POTWs find it necessary to impose mass effluent limitations.
SubpartL
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non -integrated mills where filter and
non-woven papers are produced from purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.040) (47.5)/y
(0.013) (47.5)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0080 •
0.0025
y = wastewater discharged in kgal per ton of product
• The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
1017
-------
Subpart L
Pollutant or
pollutant property
Pent achloropheno 1
Tri chl orophenol
PSNS for
non- integrated mills where paperboard is produced
from purchased pulp
Maximum for any 1 day
"Milligrams/liter (mg/1)
(0.037) (11.2)/y
(0.012) (11.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0017
0.00054
y = wastewater discharged in kgal per ton of product
The tpllowing equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Appendix A to Part 430--Methods 1650 and 1653

Method 1650

Adsorbable Organic Halides

by Adsorption and Coulometric Titration

1.0 Scope and Application

1. 1 This method is for determination of adsorbable organic

halides (AOX) associated with the Clean Water Act; the

Resource Conservation and Recovery Act; the Comprehensive

Environmental Response, Compensation, and Liability Act; and

other organic halides amenable to combustion and coulometric

titration.. The method is designed to meet the survey and

monitoring requirements of the Environmental Protection

Agency (EPA).

1.2 The method is applicable to the determination of AOX in

water and wastewater. This method is a combination of
1018
-------
several existing methods for organic halide measurements ^Bk

1 : ' V
(References 1 through 7).

1.3 The method can be used to measure organically-bound

halides (chlorine, bromine, iodine) present in dissolved or

suspended form. Results are reported as organic chloride

(Cl~). The detection limit of the method is usually .
I

dependent on interferences rather than instrumental

limitations. A method detection limit (MDL; Reference 8) of

6.6 /ig/L, and a minimum level (ML; Section 18) of 20 />tg/L,

can be achieved with no interferences present.

1.4 This method is for use by or under the supervision of

analysts experienced in the use of a combustion/micro-

coulometer. Each laboratory 'that uses this method must

demonstrate the ability to generate acceptable results using

the procedures described in Section 9.2.

1.5 Any modification of the :method beyond those expressly

permitted (Section 9.1.2) is subject to application and

approval of an alternate test procedure under 40 CFJR 136.4

and 136.5. ;

2.0 Summary of Method

2.1 Sample preservation: Residual chlorine that may be

present is removed by the addition of sodium thiosulfate.

Samples are adjusted to a pH < 2 and maintained at 0 to 4°C

until analysis. '

2.2 Sample analysis: Organic halide in water is determined

by adsorption onto granular activated carbon (GAG), washing

1019
-------
the adsorbed sample and GAG to remove inorganic halide,

combustion of the sample and GAG to form the hydrogen

halide, and titration of the hydrogen halide with a micro-

coulometer, as shown in Figure 1.

2.3 Micro-coulometer .

2.3.1 This detector operates by maintaining a constant

silver-ion concentration in a titration cell . An electric

potential is applied to a solid silver electrode to produce

silver ions in the cell . As hydrogen halide produced from

the combustion of organic halide enters the cell, it is

partitioned into an acetic acid electrolyte where it

precipitates as silver halide. The current produced is

integrated over the combustion period. The electric charge

is proportional to the number of moles of halogen captured

in the cell (Reference 6) .

2.3.2 The mass concentration of organic halides is reported

as an equivalent concentration of organically bound chloride
3.0 Definitions

3.1 Adsorbable organic halides is defined as the analyte

measured by this method. The nature of the organo- halides

and the presence of semi-extractable material will influence

the amount measured and interpretation of results .

3.2 Definitions for terms used in this method are given in

the glossary at the end of the method (Section 18) .

4.0 Interferences

1020
-------
4.1 Solvents, reagents, glassware, and other sample

processing hardware may yielcl elevated readings from the

micro-coulometer. All materials used in the analysis shall

be demonstrated to be free from interferences under the

conditions of analysis by running method blanks initially

and with each sample batch (samples started through the

adsorption process in a -given eight-hour shift, to a maximum

of 20 samples). Specific selection of reagents and

purification of solvents may be required.

4.2 Glassware is cleaned by'detergent washing in hot water,

rinsing with tap water and distilled water, capping with

aluminum foil, and baking at;450°C for at least one hour.

For some glassware, immersion in a chromate cleaning

solution prior to detergent washing may be required. If

blanks from glassware without cleaning or with fewer

cleaning steps show no detectable organic halide, the

cleaning steps that do not eliminate organic halide may be

omitted.

4.3 Most often, contamination results from methylene

chloride vapors in laboratories that perform organic

extractions. Heating, ventilating, and air conditioning

systems that are shared between the extraction laboratory

and the laboratory in which organic halide measurements are

performed transfer the methyiene chloride vapors to the air
i

in the organic halide laboratory. Exposure of the activated

carbon used in the analysis results in contamination.

1021
-------
Separate air handling systems, charcoal filters, and glove

boxes can be used to minimize this exposure.

4.4 Activated carbon.

4.4.1 The purity of each lot of activated carbon must be

verified before each use by measuring the adsorption

capacity and the background level of halogen (Section 9.5).

The stock of activated carbon should be stored in its

granular form in a glass container that is capped tightly.

Protect carbon at all times from sources of halogen vapors.

4.4.2 Inorganic substances such as chloride, chlorite,

bromide, and iodide will adsorb on activated carbon to an

extent dependent on their original concentration in the

aqueous solution and the volume of sample adsorbed.

Treating the activated carbon with a solution of nitrate

causes competitive desorption of inorganic halide species.

However, if the inorganic halide concentration is greater

than 2,000 times the organic halide concentration,

artificially high results may be obtained.

4.4.3 Halogenated organic compounds that are weakly adsorbed

on activated carbon are only partially recovered from the

sample. These include certain alcohols and acids such as

chloroethanol and chloroacetic acid that can be removed from

activated carbon by the nitrate wash.

4.5 Polyethylene gloves should be worn when handling

equipment surfaces in contact with the sample to prevent

transfer of contaminants that may be present on the hands.

1022
-------
5.0 Safety

5.1 The toxicity or carcinogenicity of each reagent used in

this method has not been precisely determined; however, each

chemical substance should be treated as a potential health

hazard. Exposure to these substances should be reduced to

the lowest possible level. The laboratory is responsible

for maintaining a current awareness file of OSHA regulations

regarding the safe handling of the chemicals specified in

this method. A reference file of material safety data

sheets (MSDSs) should be made1 available to all personnel

involved in the chemical analysis. Additional information

on laboratory safety can be found in References 9 through

11. ;

5.2 This method employs strong acids. Appropriate

clothing, gloves, and eye protection should be worn when

handling these substances.

5.3 Field samples may contain high concentrations of toxic

volatile compounds. Sample containers should be opened in a

hood and handled with gloves that will prevent exposure.

6 . 0 Equipment and Supplies

Note: Brand names, suppliers, and part numbers are for

illustrative purposes only. No endorsement is implied.

Equivalent performance may be- achieved using apparatus and

materials other than those specified here, but demonstration

of equivalent performance that meets the requirements of

1023 "
-------
this method is the responsibility of the laboratory.

6.1 Sampling equipment.

6.1.1 Bottles: 100- to 4000-mL, amber glass, sufficient for

all testing (Section 8.2). Detergent water wash, chromic

acid rinse, rinse with tap and distilled water, cover with

aluminum foil, and heat to 450°C for at least one hour

before use.

6.1.2 PTFE liner: Cleaned as above and baked at 100 to

200°C for at least one hour.

6.1.3 Bottles and liners must be lot certified to be free

of organic halide by running blanks according to this

method.

6.2 Scoop for granular activated carbon (GAC): Capable of

precisely measuring 40 mg (±5 mg) GAC (Dbhrmann Measuring

Cup 521-021, or equivalent).

6.3 Batch adsorption and filtration system.

6.3.1 Adsorption system: Rotary shaker, wrist action

shaker, ultrasonic system, or other system for assuring

thorough contact of sample with activated carbon. Systems

different from"the one described below must be demonstrated

to meet the performance requirements in Section 9 of this

method.

6.3.1.1 Erlenmeyer flasks: 250- to 1500-mL with ground-

glass stopper, for use with rotary shaker.

6.3.1.2 Shake table: Sybron Thermolyne Model LE "Big Bill"

rotator/shaker, or equivalent.

1024
-------
6.3.1.3 Rack attached to shake table to permit agitation of

16 to 25 samples simultaneously.

6.3.2 Filtration system (Figure 2).

6.3.2.1 Vacuum filter holder: Glass, with fritted-glass

support (Fisher Model 09-753E, or equivalent).
I

6.3.2.2 Polycarbonate filter: 0.40 to 0.45 micron, 25-mm

diameter (Micro Separations Inc, Model K04CP02500, or

equivalent) • '

6.3.2.3 Filter forceps: Fisher Model 09-753-50, or

equivalent, for handling filters. Two forceps may better

aid in handling filters. Clean by washing with detergent

and water, rinsing with tap and deionized water, and air

drying on aluminum foil.

6.3.2.4 Vacuum flask: 500- to 1500-mL (Fisher 10-180,0, or

equivalent).

6.3.2.5 Vacuum Source: A pressure/vacuum pump, rotary

vacuum pump, or other vacuum:source capable of providing at

least 610 mm (24 in.) Hg vacuum at 30 L/min free air

displacement.

6.3.2.6 Stopper and tubing to mate the filter holder to the

flask and the flask to the pump.

6.3.2.7 Polyethylene gloves: (Fisher 11-394-110-B, or

equivalent).

6.4 Column adsorption system.

6.4.1 Adsorption module: Dohrmann AD-2, Mitsubishi TXA-2,

or equivalent with pressurized sample and nitrate-wash

[

1025
-------
reservoirs, adsorption columns, column housings, gas and gas

pressure regulators, and receiving vessels. For each sample

reservoir, there are two adsorption columns connected in

series. A small steel funnel for filling the columns and a

rod for pushing out the carbon are also required. A ^

schematic of the column adsorption system is shown in Figure

6.4.2 Adsorption columns: Pyrex, 5 ± 0.2 cm long x 2 mm ID,

to hold 40 mg, of granular activated carbon (GAG).

6.4.3 Cerafelt: Johns-Manville, or equivalent, formed into

plugs using stainless steel borer (2 mm ID) with ejection

rod (available from Dohrmann or Mitsubishi) to hold 40 mg of

granular activated carbon (GAG). Caution: Handle Cerafelt

with gloves.

6.,4.4 Column holders: To support adsorption columns.

6.5 Combustion/micro-coulometer system:.Commercially

available as a single unit or assembled from parts. At the.

time of the writing'of this method, organic halide units

were commercially available from the Dohrmann Division of

Rosemount Analytical, Santa Glara, California; Euroglas BV,

Delft, the Netherlands; and Mitsubishi Chemical Industries,

Ltd., Tokyo,'Japan. .

6.5.1 Combustion system: Older systems may not have all of

the features shown in Figure 4. These older systems may. be

used provided the performance requirements (Section 9) of

this method are met.

1026
-------
6.5.1.1 Combustion tube: Quartz, capable of being heated to

800 to 1000°C and accommodating a boat sampler. The tube

must contain an air lock for introduction of a combustion

boat, connections for purge and combustion gas, and

connection to the micro-coulpmeter cell.
•
6.5.1.2 Tube furnace capable of controlling combustion tube

in the range of 800 to 1000°C.

6.5.1.3 Boat sampler: Capable of holding 35 to 45 mg of

activated carbon and a polycarbonate filter, and fitting

into the combustion tube (Section 6.5.1.1). Some

manufacturers offer an enlarged boat and combustion tube for

this purpose. Under a time-Controlled sequence, the boat is

first moved into an evaporation zone where water and other

volatiles are evaporated, and then into the combustion zone

where the carbon and all other organic material in the boat

are burned in a flowing oxygen stream. The evolved gases

are transported by a non-reactive carrier gas to the micro-

coulometer cell.

6.5.1.4 Motor driven boat sampler: Capable of advancing the

combustion boat into the furnace in a reproducible time

sequence. A suggested time sequence is as follows:

A. Establish initial gas flow rates: 160 mL/min CO2;

40 mL/min O2.

B. Sequence start '

C. Hold boat in hatch for five seconds to allow

integration for baseline subtraction.

1027
-------
D. Advance boat into vaporization zone.

E. Hold boat in vaporization zone for 110 seconds.

F. Establish gas flow rates for combustion: 200 mL/min

O2; 0 mL/min CO2; advance boat into pyrolysis zone

(800°C).

G. Hold boat in pyrolysis zone for six minutes.

H. Return gas flow rates to initial values; retract

boat into hatch to cool and to allow remaining HX to be

swept into detector (approximately two minutes).

I. Stop integration at 10 minutes after sequence

start.

Note: If the signal from the detector does not return to

baseline, it may be necessary to extend the pyrolysis

time.The sequence above may need to be optimized for each

instrument.

6.5.1.5 Absorber: Containing sulfuric acid to dry the gas

stream after combustion to prevent backflush of electrolyte

is highly recommended.

6.5.2 Micro-coulometer system: Capable of detecting the

equivalent of 0.2 //g of Cl". at a signal-to-noise ratio of 2 ;

capable of detecting the equivalent of 1 /zg of Cl" with a

relative standard deviation less than 10%, and capable of

'accumulating a minimum of the equivalent of 500 /xg of Cl"

before a change of electrolyte is required.

6.5.2.1 Micro-coulometer cell: The three cell designs
1028
-------
presently in use are shown in Figure 1. Cell operation is
i
described in Section 2.

6.5.2.2 Cell controller: Electronics capable of measuring

the small currents generated ;in the cell and accumulating

and displaying the charge produced by hydrogen halides

entering the cell. A strip-dhart recorder is desirable for

display of accumulated charge.
6.6 Miscellaneous glassware:
below; other sizes may be used, as necessary.
6.6.1 Volumetric flasks: 5-,
nominal sizes are specified
10-, 25-, 50-, 100-, and 1000-
mL. •

6.6.2 Beakers: 100-, 500-, and 1000-mL.

6.6.3 Volumetric pipets: 1- ;and 10-mL with pipet bulbs.

6.6.4 Volumetric micro-pipets: 10-, 20-, 50-, 100-, 200-,

and 500-^L with pipet control (Hamilton 0010, o±-

equivalent) . !

6.6.5 Graduated cylinders: 10-, 100-, and 1000-mL.

6.7 Micro-syringes: 10-, 50--, and 100-/iL.
• • t
6.8 Balances.

6.8.1 Top-loading, capable of weighing 0.1 g.

6.8.2 Analytical, capable of weighing 0.1 mg.

6.9 pH meter. ',

6.10 Wash bottles: 500- to 1000-mL, PTFE or polyethylene.

6.11 Strip-chart recorder: suggested but not required--

useful for determining end of integration (Section 11.4.2).

7.0 Reagents and Standards
]>

1029
-------
7.1 Granular activated carbon (GAG): 75 to 150 ^m (100 to

200 mesh); (Dohrmann, Mitsubishi, Carbon Plus, or

equivalent) , with chlorine content less than 1 /zg Cl" per

scoop (< 25 /zg Cl" per gram) , adsorption capacity greater

than 1000 jzg Cl" (as 2,4,6-trichlorophenol) per scoop

(>25,000 Atg/g) , inorganic halide retention of less than 1 /zg

Cl" per scoop in the presence of 10 mg of inorganic halide

(< 20 //g Cl" per gram in the presence of 2500 mg of

inorganic halide), and that meets the other test criteria in

this method.

7.2 Reagent water: Water in which organic halide is not

detected by this method.

7.2.1 Preparation: Reagent water may be generated by:

7.2.1.1 Activated carbon: Pass tap water through a carbon

bed (Calgon Filtrasorb-300, or equivalent).

7.2.1.2 Water purifier: Pass tap water through a purifier

(Millipore Super Q, or equivalent).

7.2.2 pH adjustment: Adjust the pH of the reagent water to

< 2 with nitric acid for all reagent water used in this

method, except for the acetic acid solution (Section 7.13).

7.3 Nitric acid (HNO3) : Concentrated, analytical grade.

7.4 Sodium chloride (NaCl). solution (100 /ig/mL of Cl") :

Dissolve 0.165 g NaCl in 1000 mL reagent water. This

solution is used for cell testing and for the inorganic

halide rejection test.

7.5 Ammonium chloride (NH4C1) solution (100 /ig/mL of Cl") :

1030
-------
Dissolve 0.1509 g NH4C1 in 1000 mL reagent water.

7.6 Sulfuric acid: Reagent grade (specific gravity 1184) .

7.7 Oxygen: 99.9% purity. ;

7.8 Carbon Dioxide: 99.9% purity. '

7.9 Nitrate stock solution: 'In a 1000-mL volumetric flask,

dissolve 17 g of NaNO3 in approximately 100 mL of reagent

water, add 1.4 mL nitric acid (Section 7.3) and dilute to
i

the mark with reagent water. : ;

7.10 Nitrate wash solution: Dilute 50 mL of nitrate stock

solution (Section 7.9) to 100:0 mL with reagent water.

7.11 Sodium thiosulfate (Na2S2O3) solution (1 N) : Weigh 79

grams of Na2S2O3 in a 1-L volumetric flask and dilute to the

mark with reagent water. ;

7.12 Trichlorophenol solutions

Note: The calibration solutions in this section employ 100-

mL volumes. For determinatidns requiring a larger or

smaller volume, increase or decrease the size of the

volumetric flasks commensurately. For example, if a 1-L
f ' (

sample is to be analyzed, use 1000-mL 'flasks (Sections

7.12.3.1 and 7.12.4) and 10 times the volume of reagent

[

water (Sections 7.12.3.1 and \7.12.4). The volume of stock

solution added to the calibration solutions and precision

and recovery (PAR) test solution remain as specified

(Sections 7.12.3.2 and 7.12.4) so that the same amount of
1;031
-------
chloride is delivered to the coulometric cell regardless of

the volume of the calibration and PAR solutions.

7.12.1 Methanol: HPLC grade.

7.12.2 Trichlorophenol stock solution (1.0 mg/mL of Cl") :

Dissolve 0.186 g of 2,4,6-trichlorophenol in 100 mL of

halide-free methanol. .

7.12.3 Trichlorophenol calibration solutions.

7.12.3.1 Place approximately 90 mL of reagent water in each

of five 100-mL volumetric flasks.

7.12.3.2 Using a calibrated micro-syringe or micro-pipets,

add 2, 5, 10, 30, and 80 /iL of the trichlorophenol stock

solution (Section 7.12.2) to the volumetric flasks and

dilute each to the mark with reagent water to produce

calibration solutions of 2, 5, 10, 30, and 80 fj.g Cl" per 100

mL of solution (20, 50, 100, 300, and 800 /^g/L) .

7.12.3.3 Some instruments may have a calibration range that

does not extend to 800 /zg/L (80 fj,g of Cl") . For those

instruments, a narrower dynamic range may be used. However,

if the concentration of halide in ,a sample exceeds that

range, the sample must be diluted to bring the concentration

within the range calibrated.

7.12.4 Trichlorophenol precision and recovery (PAR) test

solution (10 //g/L of Cl") : Partially fill a 100-mL

volumetric flask, add 10 /*L of the stock solution (Section

7.12.2), and.dilute to the mark with reagent water.

7.. 13 Acetic acid solution: Containing 30 to 70% acetic acid

1032
-------
in deionized water, per the instrument manufacturer's '

instructions.

8.0 Sample Collection, Preservation, and Storage

8.1 Sample preservation. l-

8.1.1 Residual chlorine: If the sample is known or

suspected to contain free chlorine, the chlorine must :be

reduced to eliminate positive1 interference that may result

from continued chlorination reactions. A knowledge of the

process from which the samplej. is collected may be of value

in determining whether dechlorination is necessary. :

Immediately after sampling, test for residual chlorine using

the following method or an alternative EPA method (Reference

12) :

8.1.1.1 Dissolve a few crystals of potassium iodide in the

sample and add three to five drops of a 1% starch solution.

A blue color indicates the presence of residual chlorine.

8.1.1.2 If residual chlorine1 is found, add 1 rnL of sodium

thiosulfate solution (Section 7.11) for each 2.5 ppm of free

chlorine or until the blue color disappears. Do not add an

excess of sodium thiosulfate. Excess sodium thiosulfate may

cause decomposition of a small fraction of the OX.
!
8.1.2 Acidification: Adjust the pH of aqueous samples to <

2 with nitric acid. Acidification inhibits biological

activity and stabilizes chemibal degradation, including

possible dehalogenation reactions that may occur at high pH.

Acidification is necessary to facilitate thorough

1033
-------
adsorption.

8.1.3 Refrigeration: Maintain Samples at a temperature of 0

to 4°C from time of collection until analysis.

8.2 Collect the amount of sample necessary for analysis

(Section 11) and all QC tests (Section 9) in an amber glass

bottle of the appropriate size (Section 6.1.1).

8.3 Analyze samples no less than three days nor more than

six months after collection.

9.0 Quality Control

9.1 Each laboratory that uses this method is required to

operate a formal quality assurance program. The minimum

requirements of this program consist of an initial

demonstration of laboratory capability, an ongoing analysis

of standards and blanks as tests of continued performance,

and analysis of matrix spike and matrix spike duplicate

(MS/MSD) samples to assess accuracy and precision.

Laboratory performance is compared to established

performance criteria to determine if the results of analyses

meet the performance characteristics of the method.

9.1.1 The laboratory shall make an initial demonstration of

the ability to produce acceptable results with this method.

This ability is demonstrated as described in Section 9.2.

9.1.2 The laboratory is permitted to modify this method to

improve separations or lower the costs of measurements,

provided that all performance specifications are met. Each

time a modification is made to the method, the laboratory is

1034
-------
required to repeat the procedures in Sections 9.2.2 and 10

to demonstrate continued method performance. If the

detection limit of the method will be affected by the

modification, the laboratory[should demonstrate that the MDL

(40 CFR 136, Appendix B) is less than or equal to the MDL in

this method or one-third the regulatory compliance level,

whichever is higher.

9.1.3 The laboratory shall spike 10% of the samples with

known concentrations of 2,4,6-trichlorophenol to monitor

method performance and matrix interferences (interferences

caused by the sample matrix). This test is described in

Section 9.3. When results of these spikes indicate atypical

method performance for samples, the samples are diluted to

bring method performance within acceptable limits.

9.1.4 Analyses of blanks are required to demonstrate

freedom from contamination. The procedures and criteria for

analysis of blanks are described in Section 9.4.

9.1.5 The laboratory shall,Jon an ongoing basis,

demonstrate through the analysis of the precision and

recovery (PAR) standard that;the analysis system is in

control. These procedures are described in Section 9.10.

9.1.6 The laboratory shall perform quality control tests on

the granular activated carboii. These procedures are

described in Section 9.5.,

9.1.7 Samples are analyzed in duplicate to demonstrate

precision. These procedures are described in Section 9.6.
i

' , 1035
-------
9.2 Initial demonstration of laboratory capability.

9.2.1 Method Detection Limit (MDL): To establish the

ability to detect AOX, the laboratory should determine the

MDL per the procedure in 40 CFR 136, Appendix B using the

apparatus, reagents, and standards that will be used in the

practice of this method. An MDL less than or equal to the

MDL in Section 1.3 should be achieved prior to the practice

of this method.

9.2.2 Initial precision and recovery (IPR): To establish

the ability to generate acceptable precision and recovery,

the laboratory shall perform the following operations:

9.2.2.1 Analyze four aliquots of the PAR standard (Section

7.12.4) and a method blank according to the procedures in

Sections 9.4 and 11. . .

9.2.2.2 Using the blank-subtracted results of the set of

four analyses, compute the average percent recovery (X) and

the standard deviation of the percent recovery (s) for the

results.

9.2.2.3 The average percent recovery shall be in the range

of 81 to 114 /ig/L and the standard deviation shall be less

than 8 /zg/L. If X and s meet these acceptance criteria,

system performance is acceptable and analysis of blanks and

samples may begin. If, however, s exceeds the precision

limit or X falls outside the range for recovery, system

performance is unacceptable. In this case, correct the

problem and repeat the test.

1036
-------
them to determine the concentration after spiking.

9.3.2.1 Compute the percent [recovery of each analyte in

each aliquot: ;

„. _ 100 (Found - Background)
% Recovery - - -
I T
where'. \
T is the true value of the spike

9.3.2.2 Compute the relative' percent difference (RPD)

between the two results (not between the two recoveries) as

described in Section 12.4.

9.3.2.3 If the RPD is less than 20%, and the recoveries for

the MS and MSD are within the range of 78 to 116%, the

results are acceptable. ,

9.3.2.4 If the RPD is greater than 20%, analyze two

alicjuots of the precision and recovery standard (PAR) . MB

9.3.2.4.1 If the RPD for the two aliquots of the PAR is

greater than 20%, the analytical system is out of control.

In this case, repair the problem and repeat the analysis of

the sample batch, including the MS/MSD.

9.3.2.4.2 If, however, the RPD for the two aliquots of the

PAR is less than 20%, dilute [the sample chosen for the

MS/MSD by a factor of 2 - 10 [(to remain within the working

range of the analytical system) and repeat the MS/MSD test.

If the RPD is still greater than 20%, the result may not be

reported for regulatory compliance purposes. In this case,

choose another sample for the MS/MSD and repeat analysis of •
|;
the sample batch.

1038
-------
"preparation (Section 11.1). If using the micro-column

procedure, adsorb the method blank using two columns, as

described in Section 11. Combust the GAG from each column

separately, as described in Section 11.

9.4.1.3 If the result from the blank from the batch method

or the sum of the results from two columns is more than 20

//g/L, analysis of samples is halted until the source of

contamination is eliminated and a blank shows no evidence of

contamination at this level.

9.4.2 Nitrate-washed GAG blanks: Analyzed daily to

demonstrate that the GAG is free from contamination.

9.4.2.1 Nitrate-washed GAG blank for the batch procedure:

Analyze a batch nitrate-washed GAG blank by adding a scoop

of dry GAG to the assembled filter apparatus containing the

polycarbonate membrane and washing the GAG with the nitrate

wash solution (Section 7.10) using the procedure in Section

11.2.6.

9.4,2.2 Nitrate-washed GAG blank for the column procedure:

Analyze a column nitrate-washed GAG blank by assembling two

carbon columns in series and washing the columns with the

nitrate wash solution (Section 7.10) using the procedure in

Section 11.3.4.2. Analyze the GAG in each column

separately. The results of the second analysis must be

within ±0.2 /zg Cl~ of the first. A difference greater than

0.2 fj,g Cl" indicates a lack of homogeneity in the GAG that

could introduce unacceptable variability. If the difference

1040
-------
exceeds this amount, the GAG;should be replaced.

9.4.3 The result for the reagent water blank (Section

9.4.1) shall not exceed the result for the nitrate wash

blank (Section 9.4.2.1 or 9.4.2.2) by more than 0.5 /zg Cl".

9.5 Granular activated carbon (GAG) batch testing: Each lot

number or batch of activated carbon received from a supplier

is tested once before use to:ensure adequate quality. Use

only GAG that meets the test •• criteria below.

9.5.1 Contamination test: Analyze a scoop of GAG. Rej ect

carbon if the amount of OX exceeds 1 /ig (25 /zg Cl"/g) .

9.5.2 Inorganic chloride adsorption test: Attempt to adsorb

NaCl from 100 mL of a solution containing 100 mg/L in

reagent water. Wash with nitrate solution and analyze. The

amount of halide should be less than 1 pg Cl" larger than

the blank. A larger amount indicates significant uptake of

inorganic chloride by the carbon. Reject carbon if the 1 /zg

level is exceeded. 1

9.6 Samples that are being used for regulatory compliance
I

purposes shall be analyzed in duplicate.

9.6.1 The procedure for preparing duplicate sample aliquots
f

is described in .Section 11.5.

9.6.2 Calculate the RPD by following the same procedure

described in Section 12.4. :

9.6.3 If the RPD is greater than 20%, the analyses must be

repeated. .

9.6.4 If the RPD remains greater than 20%, the result may

'1041
-------
not be reported for regulatory compliance purposes.

9.7 The specifications in this method can be met if the

apparatus used is calibrated properly and maintained in a

calibrated state. The standards used for calibration

(Section 10), calibration verification (Section 9.9), and

for initial (Section 9.2.2) and ongoing (Section 9.10)

precision and recovery should be identical, so that the most

precise results will be obtained.

9.8 Depending on specific program requirements, field

duplicates may be collected to determine the precision of

the sampling technique.

9.9 At the beginning and end of each eight-hour shift

during which analyses are performed, system performance and

calibration are verified. Verification of system

performance and calibration may be performed more

frequently, if desired.

9.9.1 If performance and calibration are verified at the

beginning and end of each shift (or more frequently),

samples analyzed during that period are considered valid.

9.9.2 If performance and calibration are not verified at--

both the beginning and end of a shift (or more frequently),

samples analyzed during that period must be reanalyzed.

9.9.3 If calibration is verified at the beginning of a

shift, recalibration using the five standards, described in

Section 10.6 is not necessary; otherwise, the instrument

must be recalibrated prior to analyzing samples (Section

1042
-------
10) .

9.9.4 Cell maintenance and other changes to the analytical

system that can affect system performance may not be .

performed during the eight-hour (or shorter) shift.

9.10 Calibration verification and ongoing precision and

recovery: Calibration and system performance are verified by

the analysis of the 100 pig/Li PAR standard.
r
9.10.1 Analyze a blank (Section 9.4) and analyze the PAR

standard (Section 7.12.4) immediately thereafter at the

beginning and end of each shift. Compute the concentration

of organic halide in the blank and in the PAR standard using

the procedures in Section 12. The blank shall be less than

2 n<3 Cl" (20 ^g/L equivalent) .

9.10.2 Subtract the result for the blank from the result of

the PAR standard using the procedures in Section 12, and

compute the percent recovery; of the blank-subtracted PAR

standard. The percent recovery shall be in the range of 78

to 116%. =

9.10.3 If the recovery is within this range, the analytical

process is in control and analysis of blanks and samples may

proceed. If, however, the recovery is not within the

acceptable range, the analytical process is not in control.

In this event, correct the problem and repeat the ongoing
I
precision and recovery test .(Section 9.10), or recalibrate

(Sections 10.5 through 10.6):.

9.10.4 If the recovery is riot within the acceptable range

i
1043
-------
for the PAR standard analyzed at the end.of the eight-hour

shift, correct the problem, repeat the ongoing precision and

recovery test (Section 9.10), or recalibrate (Sections 10.5

through 10.6), and reanalyze the sample batch that was

analyzed during the eight-hour shift.

9.10.5 If the recovery is within the"acceptable range at

the end of the shift, and samples are to be analyzed during

the next eight-hour shift, the end of shift verification may

be used as the beginning of shift verification for the

subsequent shift, provided the next eight-hour shift begins

as the first shift ends.

9.11 It is suggested but not required that the laboratory

develop a statement of data quality for AOX and develop>QC

charts to form a graphic demonstration of method

performance. Add results that pass the specification in

Section 9.10.2 to initial and previous ongoing data.

Develop a statement of data quality by calculating the

average percent recovery (R) and the standard deviation of

percent recovery (sr) . Express the accuracy as a recovery

interval from R - 2sr to.R + 2sr. For example, if R = 95%

and sr = 5%, the accuracy is 85 to 105%.

10.0 Calibration and Standardization

10.1 Assemble the OX system and establish the operating

conditions necessary for analysis. Differences between

various makes and models of instruments will require

different operating procedures. Laboratories should follow

1044
-------
the operating instructions provided by the manufacturer of

their particular instrument. Sensitivity, instrument

detection limit, precision, linear range, and interference
i

effects must be investigated £nd established for each

particular instrument. Calibration is performed when the

instrument is first set up and when calibration cannot be

verified (Section 9.9). |

10.2 Cell performance test: Inject 100 pJL of the sodium
t

chloride solution (10 /zg Cl"; Section 7.4) directly into the

titration cell electrolyte. Adjust the instrument to

produce a reading of 10 /ig Cl".

10.3 Combustion system test: This test can be used to

assure that the combustion/micro-coulometer systems are

performing properly without introduction of carbon. This

test should be used during initial instrument setup and when

instrument performance indicates a problem with the

combustion system. i

10.3.1 Designate a quartz boat for use with the ammonium

chloride (NH4C1) solution only.

10.3.2 Inject 100 /iL of the JsrH4Cl solution (Section 7.5)

into this boat and proceed with the analysis.

10.3.3 The result shall be between 9.5 and 1.0.5 /ig Cl". If

the recovery is not between these limits, the combustion or

micro-coulometer systems are hot performing properly. Check

the temperature of the combustion system, verify that there

are no leaks in the combustion system, confirm that the cell

1045
-------
is performing properly (Section 10.2), and then repeat the

test.

10.4 Trichlorophenol combustion test: This test can be used

to assure that the combustion/micro-coulometer systems are

performing properly when carbon is introduced. It should be

used during instrument -setup and when it is necessary to

.isolate the adsorption and combustion steps.

10.4.1 Inject 10 \iL of the 1 mg/mL trichlorophenol stock

solution (Section 7.12.2) onto one level scoop of GAG in a

quartz boat.

10.4.2 Immediately proceed with the analysis to prevent loss

of trichlorophenol and to prevent contamination of the

carbon.

10.4.3 The result shall be between 9.0 and 11.0 fj.g Cl". If

the recovery is not between these limits, the

combustion/micro-coulometer system shall be adjusted and the

test repeated until the result falls within these limits.

10.5 Background level of Cl": Determine the average

background level of Cl" for the entire analytical system, as

follows:

10.5.1 Using the procedure in Section 11 (batch or column)

that will be used for the analysis of sampl.es, determine the

background level of Cl" in each of- three portions of reagent

water. The volume of reagent water used shall be the same

as the volume used for analysis of samples.

10.5.2 Calculate the average (mean) concentration of Cl"

1046
-------
and the standard deviation of the concentration.

10.5.3 The sum of the average concentration plus two times

the standard deviation of the concentration shall be less

than 20 /Kj/L. If not, the water or carbon shall be

replaced, or the adsorption system moved to an area free of

organic halide vapors, and the test (Section 10.5) shall be

repeated. Only after this test is passed may calibration
•
i
proceed. i
I

10.6 Calibration by external standard: A calibration line

[

encompassing the calibration!range is developed using
i

solutions of 2,4,6-trichlorophenol.

10.6.1 Analyze each of the five calibration solutions

(Section 7.12.3) using the procedure in Section 11 (batch or

column) that will be used for the analysis of samples, and

the same procedure that was used for determination of the
f

system background (Section 10.5). Analyze these solutions

beginning with the lowest concentration and proceeding to

the highest. Record the response of the micro-coulometer to
I .

each calibration solution. !

10.6.2 Prepare a method blank as described in Section 9.4.

Subtract the value of the blank from each of the five

calibration results, as described in Section 12.

10.6.3 Calibration factor (ratio of response to

concentration) Using the blank subtracted results, compute

the calibration factor at each calibration point, and

compute the average calibration factor and the relative

1047 ^^
-------
standard deviation (coefficient of variation; Cv) of the

calibration factor over the calibration range.

10.6.4 Linearity: The Cv of the calibration factor shall be

less than 20%; otherwise, the calibration shall be repeated

after adjustment of the combustion/micro-coulometer system

and/or preparation of fresh calibration standards.

10.6.5 Using the average calibration factor, compute the

percent recovery at each calibration point. The recovery at

each calibration point shall be within the range of 80 to

111%. If any point is not within this range, a fresh

calibration standard shall be prepared for that point, this

standard shall be analyzed, and the calibration factor

(Section 10.6.3) and calibration linearity (Section 10.6.4)

shall be computed using the new calibration point. All

points used in the calibration must meet the 80 to 111%

recovery specification.

11.0 Procedure

11.1 Sample dilution: Many samples will contain high

concentrations of halide. If analyzed without dilution, the

micro-coulometer can be overloaded, resulting in frequent

cell cleaning and downtime. The following guidance is

provided to assist in estimating dilution levels.

11.1.1 Paper and pulp mills that employ chlorine bleaching:

Samples from pulp mills that use a chlorine bleaching

process may overload the micro-coulometer. To prevent

system overload, the maximum volume suggested for paper •

1048
-------
industry samples that employ halide in the bleaching process

is 100 mL. An adsorption volume as small as 25 mL may be

used, provided the concentration of AOX in the sample can be

measured reliably, as defined: by the requirements in Section

9.11. To minimize volumetric error, an adsorption volume

less than 25 mL may not be used. If AOX cannot be measured

reliably in a 100-mL sample volume, a sample volume to a

maximum of 1000 mL must be used. The sample and adsorption
\
volumes are suggested for paper industry samples employing

chlorine compounds in the bleaching process:
Paper or pulp mill stream
Evaporator condensate j
Process water
Pulp mill effluent
Paper mill effluent ;
Combined mill effluent
Combined bleach effluent
Z-stage filtrate
E-stage filtrate
Sample
volume
(mL) *
100
100
30
10
5
1
0.5
0.5
Adsorp-
tion
volume
(mL)
100
100
50
25
25
25
25
25
* Assumes dilution to final volume of 100 mL.
All sample aliquots (replicates, diluted
samples) must be analyzeii using the same fixed
final volume (sample volume plus reagent water,
as needed) .
11.1.2 Sample dilution procedure.

11.1.2.1 Partially fill a precleaned volumetric flask with

pH < 2 reagent water, allowing for the volume of sample to

be added.

1049
-------
11.1.2.2 Mix sample thoroughly by tumbling or shaking

vigorously.

11.1.2.3 Immediately withdraw the required sample aliquot

using a pipet or micro-syringe.

Note: Because it will be necessary to rinse the pipet or

micro-syringe (Section 11.1.2.5) , it may be necessary to

pre-calibrate the pipet or micro-syringe to assure that the

exact volume desired will be delivered.

11.1.2.4 Dispense or inject the aliquot into the volumetric

flask.

11.1.2.5 Rinse the pipet or syringe with small portions of

reagent water and add to the' flask.

11.1.2.6 Dilute to the mark with pH < 2 reagent water.

11.1.3 All samples to be reported for regulatory compliance

monitoring purposes must be analyzed in duplicate, as

described in Section 11.5.

11.1.4 Pulp and Paper in-process samples: The concentration

of organic halide in in-process samples has been shown to be

20 to 30% greater using the micro-column adsorption

technique than using the.batch adsorption technique. For

this reason, the micro-column technique shall be used for

monitoring in-process samples. Examples of in-process

samples include: combined bleach plant effluent, C-stage

filtrate, and E-stage filtrate.

11.2 Batch adsorption and filtration.
1050
-------
11.2.1 Place the appropriate^ volume of sample (diluted if

necessary), preserved as described in Section 8, into an

Erlenmeyer flask.

11.2.2 Add 5 mL of nitrate stock solution to the sample
I,
aliquot.

11.2.3 Add one level scoop of activated carbon that has

passed the quality control tests in Section 9.

11.2.4 Shake the suspension if or at least one hour in a

mechanical shaker. ;

11.2.5 Filter the suspension through a polycarbonate

membrane filter. Filter by suction until the liquid level

reaches the top of the carbon.
i
11.2.6 Wash the inside surface of the filter funnel with 25

mL (±5 mL) of nitrate wash solution in several portions.

After the level of the final wash reaches the top of the

GAG, filter by suction until [the cake is barely dry. The

time required for drying should be minimized to prevent

exposure of the GAG to halogen vapors in the air, but should

be sufficient to permit drying of the cake so that excess
I
water is not introduced into [the combustion apparatus. A

drying time of approximately 10 seconds under vacuum has

been shown to be effective for this operation.

11.2.7 Carefully remove the top of the filter holder,

making sure that no carbon is lost. This operation is most

successfully performed by removing the clamp, tilting the

top of the filter holder (the funnel portion) to one 'side,

1051
-------
and lifting upward.

11.2.8 Using a squeeze bottle or micro-syringe, rapidly

rinse the carbon from the inside of the filter holder onto

the filter cake using small portions of wash solution.

Allow the cake to dry under vacuum for no more than 10

seconds after the final rinse. Immediately turn the vacuum

off.

11.2.9 Using tweezers, carefully fold the polycarbonate

filter in half, then in fourths, making sure that no carbon

is lost.

11.3 Column adsorption.

11.3.1 Column preparation: Prepare a sufficient number of

columns for one day's operation as follows:

11.3.1.1 In a .glove box or area free from halide vapors,

place a plug of Cerafelt into the end of a clean glass

column.

11.3..1.2 Fill the glass column with one level scoop

(approximately 40 mg) of granular activated carbon that has

passed the quality control tests in Section 9l

11.3.1.3 Insert a Cerafelt plug into the open end of the

column to hold the carbon in place.

11.3.1.4 Store the columns in a glass jar with PTFE lined

screw-cap to prevent infiltration of halide vapors from the

air.

11.3.2 Column setup.

11.3.2.1 Install two columns in series in the adsorption

1052
-------
module. i

11.3.2.2 If the sample is known or expected to contain

particulates that could prevent free flow of sample through

the micro-columns, a Cerafelt plug is placed in the tubing

ahead of the columns. If a measurement of the OX content of

the particulates. is desired,; the Cerafelt plug can be washed

with nitrate solution; placed in a combustion boat, and

processed as a separate sample.

11.3.3 Adjusting sample flow rate: Because the flow rate

used to load the sample onto; the columns can affect the

ability of'the GAG to adsorb; organic halides, the flow rate

of the method blank is measured, and the gas pressure used
i1
to process samples is adjusted accordingly. The flow rate

of the blank, which is composed of acidified reagent water

and contains no particulate matter, should be greater than

the flow rate of any sample pontaining even small amounts of

particulate matter.

11.3.3.1 Fill the sample reservoir with the volume of

reagent water chosen for the1 analysis (Section 9.4.1.2) that

has been preserved and acidified as described in Section 8.
j
Cap the reservoir.

11.3.3.2 Adjust the gas pressure per the manufacturer's

instructions. Record the time required for the entire

volume of reagent water to pass through both columns. The

flow rate must not exceed 3 mL/min over the duration of the
I"
time required to adsorb the volume. If this flow rate is

,1053
-------
exceeded, adjust gas pressure, prepare another blank, and

repeat the adsorption.

11.3.3.3 Once the flow rate for the blank has been

established, the same adsorption conditions must be applied

to all subsequent samples during that eight-hour shift, or

until another method blank is processed, whichever comes

first. To aid in overcoming breakthrough problems, a lower

gas pressure (and, therefore, flow rate) may be used for

processing of samples, if desired. If the sample adsorption

unit is. disassembled or cleaned, the flow rate must be

checked before processing additional samples.

11.3.3.4 Elute the pair of columns with 2 mL of nitrate

wash solution. The flow rate of nitrate wash solution must

not exceed 3 mL/min.

11.3.3.5 Separate the columns and mark for subsequent

analysis.

11.3.4 The adsorption of sample volumes is performed in a

similar fashion. Fill the sample reservoir with the sample

volume chosen for the analysis (Section 11.1), that has been

preserved as described in Section 8. All analyses must be

performed with this volume (sample volume.plus reagent

water, as needed) in order to maintain a flow rate no

greater than that determined for the blank (see Section

11.3-.3) . .

11.3.4.1 Use the same gas pressure for sample adsorption as

is used for the blank.

1054
-------
11.3.4.2 Elute the columns with 2 mL of the nitrate wash

solution.

11.3.4.3 Separate the columns and mark for subsequent

analysis. >

11.3.5 If it is desirable to; make measurements at levels

lower than can be achieved with the sample volume chosen, or

if the instrument response of1 an undiluted sample is less

than three times the instrument response of the blank

(Section 12.6.3), a larger sample volume must be used.

11.4 Combustion and titration.

11.4.1 Polycarbonate filter and GAG from batch adsorption.

11.4.1.1 Place the folded polycarbonate filter containing

the GAG in a quartz combustion boat, close the airlock, and

proceed with the automated sequence.

11.4.1.2 Record the signal from the micro-coulometer for a

minimum integration time of 10 minutes and determine the

concentration of Cl" from calibration data, per Section 12.

11.4.2 Columns from column adsorption.

11.4.2.1 Using the push rod, ! push the carbon and the

Cerafelt plug(s) from the first column into a combustion

boat. Proceed with the automated sequence.

11.4.2.2 Record the signal from the micro-coulometer for a

minimum integration time of 10 minutes and determine the

concentration of Cl" for the first column from calibration

data, per Section 12. ; ,

11.4.2.3 Repeat the automated sequence with the second

1055
-------
column.

11.4.2.4 Determine the extent of breakthrough of organic

halides from the first column to the second column, as

described in Section 12.

11.4.3 The two columns that are used for the method blank

must be combusted separately, as is done for samples.

11.5 Duplicate sample analysis: All samples to be reported

for regulatory compriance purposes must be analyzed in

duplicate. This requirement applies-to both the batch and

column adsorption procedures. In addition, if it is

necessary to dilute the sample for the purposes of reducing

breakthrough or maintaining the concentration within the

calibration range, a more or less dilute sample must be

analyzed. The adsorption volumes used for analysis of

undiluted samples, diluted samples, and all replicates must

be the same as the volume used for QC tests and calibration

(Sections 9 and 10).

11.5.1 Using results from analysis of one sample volume

(Section 11.4) and the procedure in Section 11.1.2-,

determine if the dilution used was within the calibration

range of the instrument and/or if breakthrough exceeded the

specification in Section 12.3.1. If the breakthrough

criterion was exceeded or the sample was not within the

calibration range, adjust the dilution volume as needed. If

the breakthrough criterion was not exceeded.and the sample

dilution was within the calibration range, a second volume

1056
-------
at the same dilution level may be used. ^^-

w
11,5.2 Adsorb the sample using the same technique (batch or "^^

column) used for the first sample volume. Combust the GAG

from the second volume as described in Section 11.4, and

calculate the results as described in Section 12. Compare

the results of the two analyses as described in Section

12.4.

11.5.3 Duplicate analyses are not required for method

blanks, as different dilution levels are not possible.

11.5.4 Duplicate analyses of the PAR standard used for
i

calibration verification (Section 9.10) are not required.

12.0 Data Analysis and Calculations

12.1 Batch Adsorption Method: Calculate the blank-

subtracted concentration of adsorbable organic halide

detected in each sample (in micrograms of chloride per

liter) using the following equation:

AOX (^/£) - (C " jS)

•where: I

C = \ig Cl~ from micro-coulometer for the sample

B = pg Cl' from micro-coulometer for the reagent water blank (Section 9.4.1)

V = volume of sample in liters ;

This calculation is performed for each of the two dilution

levels analyzed for each sample.

12.2 Column Adsorption Method: Calculate'the blank-

subtracted concentration of adsorbable organic halide

detected in each sample (in micrograms of chloride per

liter) using the following equation:
1057
-------
•where:
C1 = p-g Cl' from micro-coulometer for first column from the sample
C2 = ]ig C!' from micro-coulometer for second column from the sample
Bi = V-g from micro-coulometer for first column from the reagent -water blank (Section 9.4.1)
&2 = t1^ ^ from micro-coulometer for second column from the reagent water blank (Section 9.4.1)
V = volume of sample in liters
12.3 Percent breakthrough: For each sample analyzed by the
column method, calculate the percent breakthrough of halide
from the first column to the second column, using the
following equation:
% Breakthrough =
(C2 -
[(C, ~
12.3.1 For samples' to be reported for regulatory compliance
purposes, the percent breakthrough must be less than or
equal to 25% for both of the two analyses performed on each
sample (see Section 11.5).
12.3.2 If the breakthrough exceeds 25%, dilute the affected
sample further, maintaining the amount of halide at least
three times higher than the level of blank, and reanalyze
the sample. Ensure that the sample is also analyzed at a
second level of dilution that is at least a factor of 2
different (and still higher than three times the blank).
12 .-4 Relative percent difference (RPD) : Calculate the
relative percent difference between the results of the two
analyses of each sample, using the following equation:
1058
-------
2001 (A OX. - AOX.)\
RPD = < —
[(AOX1 + AOXJ]
12.5 High concentrations of AOX: If the amount of halide
from either analysis exceeds the calibration range, dilute
the sample and reanalyze, maintaining at•least a factor of 2
difference in the dilution levels of the two portions of the

sample used. |.
12.6 Low concentrations of AOX: The blank-subtracted final
result from the batch procedure or the sum of the blank-
subtracted results from the two carbon columns should be
significantly above the level of the blank.
12.6.1 If the instrument response for a sample exceeds the
instrument response for the blank by a factor of at least 3, |H|
the result is acceptable. | '
12.6.2 If the instrument response for a sample is less than
I
three times the instrument response for the blank, and the
sample has been diluted, analyze a less dilute aliquot of

sample. ;
12.6.3 If the instrument response of an undiluted sample
containing AOX above the minimum level is less than three
times the instrument response; for the blank, the result is
suspect and may not be used for regulatory compliance
purposes. In this case, find the cause of contamination,
correct the problem, and reanalyze the sample under the
! '!
corrected conditions. -

1059
-------
12.7 Report results that meet all of the specifications in

this method as the mean of the blank-subtracted values from

Section 12.1 or 12.2 for the two analyses at different

dilution levels, in /ug/L of Cl" (not as 2,4,6-

t-richlorophenol) , to three significant figures. Report the

RPD of the two analyses. For samples analyzed by the column

procedure, also report the percent breakthrough.

13.0 Method Performance

The specifications contained in this method are based on

data from a single laboratory and from a large-scale study

of the pulp and paper industry.

14.0 Pollution Prevention

14.1 The solvents used in this .method pose little threat to

the environment when recycled and managed properly.

14.2 Standards should be prepared in volumes consistent

with laboratory use to minimize the volume of expired

standards to be disposed.

15.0 Waste Management

15.1 It is the laboratory's responsibility to .comply with

all federal, state, and local regulations governing waste

management, particularly the hazardous waste identification

rules and land disposal restrictions, and to protect the

air, water, and land by minimizing and controlling all

releases from fume hoods and bench operations. Compliance

with all sewage discharge permits and regulations is also
1060
-------
required.

15.2 Samples preserved with
HC1 or H2SO4 to pH < 2 are
hazardous and must be neutralized before being disposed, or

must be handled as hazardous waste. Acetic acid and silver

I:
acetate solutions resulting from cell flushing must be

disposed of in accordance with all applicable federal,

state, and local regulations.
l

15.3 For further information on waste management, consult

"The Waste Management Manual ;for Laboratory Personnel," and

"Less is Better: Laboratory Chemical Management for Waste

Reduction," both available from the.American Chemical

Society's Department of Government Relations and Science

Policy, 1155 16th Street N.W., Washington, D.C. 20036.
1061
-------
16.0 References

16.1 "Total Organic Halide, Methods 450.1--Interim,"

Prepared by Stephen Billets and James J. Lichtenberg, USEPA,

Office of Research and Development, Physical and Chemical

Methods Branch, EMSL-Cincinnati, Cincinnati, OH 45268, EPA

60,0/4-81-056 (1981) .

16.2 Method 9020, USEPA Office of Solid Waste, "Test

Methods for Evaluating Solid Waste, SW-846," Third Edition,

1987.

16.3 "Determination of Adsorbable Organic Halogens (AOX),"

"German Standard Methods for the Analysis of Water, Waste

Water and Sludge--General Parameters of Effects and

Substances," Deutsche Industrie Norm (DIN) Method 38 409,

Part 14, DIN German Standards Institute, Beuth Verlag,

Berlin, Germany (1987) .

16.4 "Water Quality: Determination of Adsorbable Organic

Halogens (AOX)," International Organization for

Standard/Draft International Standardization (ISO/DIS)

Method 9562 (1988).

16.5 "Organically Bound Chlorine by the AOX Method," SCAN-W

9:89, Secretariat, Scandinavian Pulp, Paper and Board

Testing Committee, Box 5604, S-11486, Stockholm, Sweden

(1989) .

16.6 Method 5320, "Dissolved Organic Halogen,;1 from

"Standard Methods for the Examination of Water and

Wastewater," 5320, American Public Health Association, 1015

1062
-------
15th St. NW, Washington, DC 2;0005 (1989) .

16.7 "Canadian Standard Methbd for the Determination of
f

Adsorbable Organic Halides (AOX) in Waters and Wastewaters,"

Environment Canada and The Canadian Pulp and Paper

Association (1990). ;

16.8 40 CFR Part 136, Appendix B.

16.9 "Working with Carcinogens," DHEW, PHS, CDC, NIOSH,

Publication 77-206, (Aug 1977;) .

16.10 "OSHA Safety and Health Standards, General Industry"

OSHA 2206, 29 CFR 1910 (Jan 1976).

16.11 "Safety in Academic Chemistry Laboratories," ACS

Committee on Chemical Safety s(1979) .

16.12 "Methods 330.4 and 330!. 5 for Total Residual
i

Chlorine," USEPA, EMSL-Cincinnati, Cincinnati, OH 45268, 4ftk

EPA-4-79-020 (March 1979). ;

16.13 "Validation of Method 1650: Determination of Organic

Halide," Analytical Technologies Inc., ERCE Contract 87-

3410,'November 15, 1990. Available from the EPA Sample

Control Center, DynCorp, 300 N. Lee St., Alexandria, VA

22314 (703-519-1140). !

17.0 Figures
1;0 6 3
-------
a. Mitsubishi
b. Dohrmann
c. Euroglas
Silver
Sensor
Electrode
Silver/Silver
Chloride
Reference
Electrode
Gases
In
Platinum
Electrode
Silver
Generator
Electrode
Gases
Out
Silver/Silver
Acetate
Reference
Electrode
Gases
r*Gases Silver
Silver
Sensor
Electrode
Generator JI
Electrode
Silver
Generator
Electrode

Platinum
Electrode
Platinum
Electrode
NoStirrer
Silver
Sensor
Electrode
Silvei/Silver
Chloride
Reference
Electrode
Figure 1. Microcoulometric Titration Cells (from Reference 7)

1064
-------
Funnel
Glarnp
Slain fess-
SteeI Support

PTFE Gasket
Base
No. 5
Stopper.
Figure 2. Filter Apparatus
1065
-------
Sample
Reservoir
(1of4)
GAG Column 1
<3AC Column 2
I
Nit rate Wash
Reservoir
Figures. Schematic of the Column Adsorption System

1066
-------
1235
1. Stripping Device
2. Sample inlet forAOX
3. AOXSampte
4. Furnace
5. Combustion Tube
6. Absorberfilledwilh HSSO4
7. Trtrsftioncell
8. Working electrodes
9. Measuring electrodes
10. Su'ner
11. Titraition mfcro-processor
12. Gas flow and temperature control device
8 • §
10
Figure 4. Schematic of an AOX Apparatus

1067
-------
18.0 Glossary of Definitions and Purposes

These definitions and purposes are specific to this

method but have been conformed to common usage as much

as possible.

18.1 Units of weight and measure and their abbreviations.

18.1.1 Symbols.

°C degrees Celsius

/ug microgram

AtL microliter

< less than

> greater than

% percent " .

18.1.2 Alphabetical characters.

cm centimeter

g gram •

h hour

ID inside diameter

in inch

L liter

m meter .

mg milligram

min minute

mL milliliter . •

mm millimeter

N normal; gram molecular weight of solute

divided by hydrogen equivalent of solute,

1068
-------
per liter of solution

OD outside diameter

ppb part-per-billion

ppm part-per-mi11ion
|i !
ppt part-per-trillion

psig pounds-per-square inch gauge

v/v volume per unit volume
P
w/v weight per unit volume
*
18.2 Definitions and acronyms (in alphabetical order,) . •

Analyte: AbX tested for by this method.

Calibration standard (CAL): A solution

prepared from a secondary standard and/or stock

solution which isiused to calibrate the response

of the instrument: with respect to analyte «B»

concentration.
I
Calibration verification standard (VER):

The mid-point calibration standard (CSS) that is

used to verify calibration.

Field blank: An aliquot of reagent water

or other reference matrix that is placed in a

sample container in the laboratory or the field,

and treated as a sample in all respects,

including exposure to sampling site conditions,

storage, preservation, and all analytical

procedures. The purpose of the field blank is

to determine if the field or sample transporting

1069
-------
procedures and environments have contaminated

the sample.

IPR: Initial precision and recovery; four

aliquots of the diluted PAR standard analyzed to

establish the ability to generate acceptable

. precision and accuracy. An IPR is performed

prior to the first time this method is used and

any time the method or instrumentation is

modified.

Laboratory blank: See Method blank.

Laboratory control sample (LCS): See

Ongoing precision and recovery sample (OPR).

Laboratory reagent blank: See Method

blank..

May: This action, activity, or procedural

step is neither required nor prohibited.

May not: This action, activity, or

procedural step is prohibited.

Method blank: An aliquot of reagent water

that is treated exactly as a sample including

exposure to all glassware, equipment, solvents,

reagents, internal standards, and surrogates

that are used with samples. The method blank is

used to determine if analytes or interferences

are present in the laboratory environment, the

reagents, or the apparatus.

1070
-------
Minimum level (ML): The level at which
j

the entire analytical system must give a

recognizable signal and acceptable calibration

point for the anaiyte. It is equivalent to the

concentration of the lowest calibration
l

standard, assuming that all method-specified

sample weights, volumes, and cleanup procedures

have been employed.

Must: Thisjaction, activity, or

procedural step is required.

OPR: Ongoing precision and recovery

standard; a laboratory blank spiked with a known

quantity of analyte. The OPR is analyzed exactly

like a sample. Its-purpose is to assure that the

results produced by the laboratory remain within

the limits specified in this method for

precision and recovery.

PAR: Precision and recovery standard;

secondary standard that is diluted and spiked to

form the IPR and OPR.

Preparation;blank: See Method blank.

Primary dilution standard: A solution

containing the specified analytes that is

purchased or prepared from stock solutions and

diluted as needed:to prepare calibration

solutions and other solutions.

1071 ^^
-------
Quality control check sample (QCS): A

sample containing all or a subset of the

analytes at known concentrations. The QCS is

obtained from a source external to the

laboratory or is prepared from a source of

standards different from the source of

calibration standards. It is used to check

laboratory performance with test materials

prepared external to. the normal preparation

process.

Reagent water: Water demonstrated to be

free from the analyte of interest and

potentially interfering substances at the method

detection limit for the analyte.

Relative standard deviation (RSD): The

standard deviation multiplied by 100, divided by

the mean.

RSD: See Relative standard deviation.

Should: .This action, activity, or

procedural step is suggested but not required.

Stock solution: A solution containing an

analyte that, is prepared using a reference

material traceable to EPA, the National

Institute of Science and Technology (MIST), or a

source that will attest to the purity and

authenticity of the reference material.

1072
-------
VER: See Calibration verification

standard. ;
1073
-------
Method 1653

Chlorinated Phenolics in Wastewater

by In Situ Acetylation and GCMS
r
1.0 Scope and Application

1.1 This method is for determination of chlorinated

phenolics (chlorinated phenols, guaiacols, catechols,

vanillins, syringaldehydes) and other compounds associated

with the Clean Water Act; the Resource Conservation and

Recovery Act; and the Comprehensive Environmental Response,

Compensation, and Liability Act; and that are amenable to in

situ acetylation, extraction, and analysis by capillary

column gas chromatography/mass spectrometry (GCMS). This

method is based on existing methods for determination of

chlorophenolics in pulp and paper industry wastewaters

(References 1 and 2) .

1.2 The chemical compounds listed in Table 1 may be

determined in waters and, specifically, in in-process

streams and wastewaters associated with the pulp and paper

industry. The method is designed to meet the survey and

monitoring requirements of the Environmental Protection

Agency (EPA).

1.3 The detection limit of this method is usually dependent

on the level of interferences rather than instrumental

limitations. The method detection limits (MDLs) in Table 2
1074
-------
typify the minimum quantity that can be detected with no

interferences present ' .

1.4 The GCMS portions of this method are for use only by

persons experienced with GCMS! or under the close supervision

of such qualified persons. Laboratories unfamiliar with

analyses of environmental samples by GCMS should run the

performance tests in Reference 3 before beginning.

1.5 Any modification of the method beyond those expressly

permitted is subject to the application and approval of

alternative test procedures under 40 CFR Parts 136.4 and

136.5. ;

2.0 Summary of Method

2.1 A 1000-mL aliquot of water is spiked with stable

isotopically labeled analogs 'of the compounds of interest

and an internal standard. The solution is adjusted to

neutral pH, potassium carbonate buffer is added, and the pH

is raised to 9 - 11.5. The chlorophenolics are converted in

situ to acetates by the addition of acetic anhydride. After
j;
acetylation, the solution is extracted with hexane. The

hexane is concentrated to a final volume of 0.5 mL, an

instrument internal standard ;is added, and an aliquot of the
I1
concentrated extract is injected into the gas chromatograph

(GC) . The compounds are separated by GC and detected by a

mass spectrometer (MS). The ;labeled compounds and internal
f
standard serve to correct the variability of the analytical
1075
-------
technique.

2.2 Identification of a pollutant (qualitative analysis) is

performed by comparing the relative retention time and mass

spectrum to that of an authentic standard. A compound is

identified when its relative retention time and mass

spectrum agree.

2.3 Quantitative analysis is performed in one of two ways

by GCMS using extracted ion-current profile (EICP) areas:

(1) For those compounds listed in Table 1 for which

standards and labeled analogs are available, the GCMS system

is calibrated and the compound concentration is determined

using an isotope dilution technique; (2) for those compounds

listed in Table 1 for which authentic standards but no. .

labeled compounds are available, the GCMS system is

calibrated and the compound concentration is determined

using an internal standard technique.

2.4 Quality is assured through reproducible calibration and

testing of the extraction and GCMS systems.

3.0 Definitions

3.1 Chlorinated phenolics are the chlorinated phenols,

guaiacols, catechols, vanillins, syringaldehydes and other

compounds amenable to in situ acetylation, extraction, and

determination by GCMS using this method.

3.2 Definitions for other terms used in this method are

given in the glossary at the end of the method (Section

20.0) .

1076
-------
4.0 Interferences

4.1 Solvents, reagents, glassware, and other sample

•processing hardware may yield artifacts and/or elevated

baselines, causing misinterpretation of chromatograms and

spectra. All materials used an the analysis shall be

demonstrated to be free from interferences under the

conditions of analysis by running method blanks initially

and with each sample batch (samples started through the

extraction process on a given1 eight-hour shift, to a maximum

of 20). Specific selection of reagents and purification of

solvents by distillation in all-glass systems may be

required. Glassware and, where possible, reagents are

cleaned by using solvent rinse and baking at 450°C for a

minimum of one hour. ;
t

4.2 Interferences co-extracted from samples will vary

considerably from source to source, depending on the

!'
diversity of the site being sampled. Industry experience

suggests that high levels of non-chlorinated phenols may

cause poor recovery of the compounds of interest,

particularly in samples collected in the vicinity of a

source of creosote, such as a wood-preserving plant

(Reference 1). |

4.3 The internal standard, 3|, 4,5-trichlorophenol, has been

reported to be an anaerobic degradation product of
i

2,3,4,5-tetrachlorophenol and/or pentachlorophenol

(Reference 1). When an interference with this or another

1077
-------
compound occurs, labeled pentachlorophenol or another

labeled compound may be used as an alternative internal

standard; otherwise, the internal standards and reference

compounds must be used as specified in this method.

4.4 Blank contamination by pentachlorophenol has been

reported (Reference 1) to be traceable to potassium

carbonate; it has also been reported that this contamination

may be removed by baking overnight at 400 to 500°C.

4.5 Catechols are susceptible to degradation by active

sites on injection port liners and columns, and are subject

to oxidation to the corresponding chloro-o-benzoquinones

(Reference 2). A small amount of ascorbic acid may be added

to samples to prevent auto-oxidation (Reference 2; also see

Section 11.1.6). For pulp and paper industry samples,

ascorbic acid may be added to treated effluent samples only.

5.0 Safety

5.1 The toxicity or carcinogenicity of each compound or

reagent used in this method has not been precisely

determined; however, each chemical compound should be

treated as a potential health hazard. Exposure to these

compounds should be reduced to the lowest possible level.

The laboratory is responsible for maintaining a current

awareness file of OSHA regulations regarding the safe

handling of the chemicals specified in this method. A

reference file of materials safety data sheets (MSDSs)

should be made available to all personnel involved in these

1078
-------
analyses. Additional information on laboratory safety can

be found in References 4 through 6.

5.2 Samples may contain high concentrations of toxic

compounds, and should be handled with gloves and a hood

opened to prevent exposure.

6.0 Equipment and Supplies

Note: Brand names, suppliers, and part numbers are for

illustrative purposes only. \No endorsement is implied.
f
Equivalent performance may be achieved using apparatus and

materials other than those specified here, but demonstration
|:

of equivalent performance that meets the requirements of

this method is the responsibility of the laboratory.

6.1 Sampling equipment for discrete or composite sampling.

6.1.1 Sample bottles and caps.

6.1.1.1 Sample bottle: Amber glass, 1000-mL minimum, with

screw-cap. If amber bottles are not available, samples

shall be protected from light.

6.1.1.2 Bottle caps: Threaded to fit sample bottles.. Caps

shall be lined with PTFE. •• •

6.1.1.3 Cleaning bottles: Detergent water wash, cap with

aluminum foil, and bake at 450°C for a minimum of one hour

before use. \

6.1.1.4 Cleaning liners: Detergent water wash, reagent
i
water (Section 7.4) and solvent rinse, and bake at

approximately 200°C for a minimum of 1 hour prior to use.

1079
-------
6.1.1.5 Bottles and liners must be lot-certified to be free

of chlorophenolics by running blanks according to this

method. If blanks from bottles and/or liners without

cleaning or with fewer cleaning steps show no detectable

chlorophenolics, the bottle and liner cleaning steps that do

not eliminate chlorophenolics may be omitted.

6.1.2 Compositing equipment: Automatic or manual

compositing system incorporating glass containers cleaned

per bottle cleaning procedure above. Sample containers are

kept at 0 to 4°C during sampling. Glass or PTFE tubing only

shall be used. If the sampler uses a peristaltic pump, a

minimum length of compressible silicone rubber tubing may be

used in the pump only. Before use, the tubing shall be

thoroughly rinsed with methanol, followed by repeated

rinsing with reagent water (Section 7.4) to minimize sample

contamination. An integrating flow meter is used to collect

proportional composite samples.

6.2 Extraction apparatus.

6.2.1 Bottle or beaker: 1500- to 2000-mL capacity.

6.2.2 Separatory funnel: 500- to 2000-mL, glass, with PTFE

stopcock.

6.2.3 Magnetic stirrer: Corning Model 320, or equivalent,

with stirring bar.

6.3 Polyethylene gloves: For handling samples and

extraction equipment (Fisher 11-394-110-B,.or equivalent).

6.4 Graduated cylinders: 1000-mL, lOO.-mL, and 10-mL

1080
-------
nominal. [
i
i
6.5 Centrifuge: Capable of accepting 50-mL centrifuge tubes
i
and achieving 3000 RPM. ;

6.5.1 Centrifuge tubes.

6.5.1.1 35-mL nominal, with ;PTFE-lined screw-cap.

6.5.1.2 15-mL nominal, conical graduated, with ground-glass

stopper. • !

6.6 Concentration apparatus.

6.6.1 Kuderna-Danish (K-D) concentrator tube: 10-mL,

graduated (Kontes K-570050-1025, or equivalent) with

calibration verified. Grounql-glass stopper (size 19/22

joint) is used to prevent evaporation of extracts.

6.6.2 Kuderna-Danish (K-D) evaporation flask: 1000-mL

(Kontes K-570001-1000, or equivalent), attached to

concentrator tube with springs (Kontes K-662750-0012).

6.6.3 Snyder column: Three-ball macro (Kontes

K-503000-0232, or equivalent)| .

6.6.4 Snyder column: Two-ball micro (Kontes K-469002-0219,

or equivalent).

6.6.5 Boiling chips: Approximately 10/40 mesh, extracted

with methylene chloride and baked at 450°C for a minimum of

one hour. ,

6.6.6 Nitrogen evaporation apparatus: Equipped with a water

bath controlled at 35 to 40°C (N-Evap, Organomation

Associates, Inc., South Berlin, MA, or equivalent),

installed in a fume hood. This device may be used in place

1081
-------
of the micro-Snyder column concentrator in Section 6.6.4
above. •
6.7 Water bath: Heated, with concentric ring cover, capable
of temperature control (± 2°C), installed in a fume hood.
6.8 Sample vials: Amber glass, 1- to 3-mL, with PTFE-lined
screw-cap.
6.9 Balances.
6.9.1 Analytical: Capable of weighing 0.1 mg.
6.9.2 Top loading: Capable of weighing 10 mg.
6.10 pH meter.
6.11 Gas chromatograph: Shall have.splitless or on-column
injection port for capillary column, temperature program
-with 50°C hold, and shall meet all of. the performance
specifications in Section 9.
.6.12 Gas chromatographic column: 30 m (±5 m) x 0.25 mm
(±0.02 mm) I.D. x 0.25 micron, 5% phenyl, 94% methyl, 1%
vinyl silicone bonded-phase fused-silica capillary column (J
& W DB-5, or equivalent) ..
6.13 Mass spectrometer: 70 eV electron impact ionization,
shall repetitively scan from 42 to' 450 amu in 0.95 to 1.00
second, and shall produce a unit resolution (valleys between
m/z 441 - 442 less than 10% of the height of the 441 peak),
background-corrected mass spectrum from 50 ng
decafluprotriphenylphosphine (DFTPP) introduced through the
GC inlet. The spectrum shall meet the mass-intensity
criteria in Table 3 (Reference - 7) . The mass spectrometer

1082
-------
shall be interfaced to the GC such that the end of the

capillary column terminates within 1 cm of the ion source,

but does not intercept the electron or ion beams. All

portions of the column which connect the GC to the ion
!
source shall remain at or above the column temperature

during analysis to preclude condensation of less volatile

compounds. '

6.14 Data system: Shall collect and record MS data, store

mass-intensity data in spectral libraries, process GCMS

data, generate reports, and compute and record response

factors.

6.14.1 Data acquisition: Mass spectra shall be collected.

continuously throughout the analysis and stored on a mass

storage device.

6.14.2 Mass spectral libraries: User-created libraries.

containing mass spectra obtained from analysis of authentic

standards shall be employed to reverse search GCMS runs for

the compounds of interest (Section 10.2).

6.14.3 Data processing: The data system shall be used to

search, locate, identify, and quantify the compounds of

interest in each GCMS analysis. Software routines shall be

employed to compute retention times, and to compute peak

areas at the m/z's specified; (Table 4). Displays of

spectra, mass chromatograms, and library comparisons are

required to verify results. ;

6.14.4 Response factors and; multi-point calibrations: The

i!083
-------
data system shall be used to record and maintain lists of

response factors (response ratios for isotope dilution) and

multi-point calibration curves (Section 10). Computations

of relative standard deviation (coefficient of variation)

are used for testing calibration linearity. Statistics on

initial (Section 9.3.2) and ongoing (Section 9.6)

performance shall be computed and maintained.

7.0 Reagents and Standards

7.1 Reagents for adjusting sample pH.

7.1.1 Sodium hydroxide: Reagent grade, 6 N in reagent

water.

7.1.2 Sulfuric acid: Reagent grade, 6 N in reagent water.

7.2 Reagents for sample preservation.

7.2.1 Sodium thiosulfate (Na2S2O3) solution (1 N) : Weigh 79

g Na2S2O3 in a 1-L volumetric flask and dilute to the mark

with reagent water.

7.2.2 Ascorbic acid solution: Prepare a solution of

ascorbic acid in reagent water at a concentration of 0.1

g/mL. This solution must be prepared fresh on each day when

derivatizations will be performed. Therefore, do not

prepare more than will be used that day. (A 50-mL volume is

sufficient for ten analyses).

7.3 Solvents: Hexane, acetone, and methanol. Distilled in

glass (Burdick and Jackson, or equivalent).

7.4 Reagent water: Water in which the compounds of interest

and interfering compounds are not detected by this method.

1084
-------
7.5 Reagents for derivatization.

7.5.1 Potassium carbonate (KjCOs) .

7.5.1.1 Purification: Spread1 in a shallow baking .dish, heat

overnight at 400 to 500°C.

7.5.1.2 Solution: Dissolve 150 g purified K2CO3 in 250 mL

reagent water.

7.5.2 Acetic anhydride: Redistilled reagent grade.

7.6 Analytical standards.

7.6.1 Derivatization: Because the chlorinated phenolics are

determined as their acetate derivatives after in situ
\

acetylation, the method requires that the calibration

standards be prepared by spiking the underivatized materials

into reagent water and carrying the spiked reagent water

aliquot through the entire derivatization and extraction
i

procedure that is applied to the field samples.

7.6.2 Standard solutions: Purchased as solutions or

mixtures with certification to their purity, concentration,

and authenticity, or prepared from materials of known purity

and composition. If chemical purity of a compound is 98% or

greater, the weight may be used without correction to

compute the concentration of 'the standard. When not being

used, standards are stored in the dark at -20 to -10°C in

screw-capped vials with PTFE-lined lids. A mark is placed

on the vial at the level of the solution so that solvent

evaporation loss can be detected. The vials are brought to

room temperature prior to use.

1085
-------
7.6.3 If the chemical purity of any standard does not meet

the 98% requirement above, the laboratory must correct all

calculations, calibrations, etc., for the difference in

purity.

7.7 Preparation of stock solutions: Prepare chlorovanillins

and chlorosyringaldehydes in acetone, as these compounds are

subject to degradation in .methanol. Prepare the remaining

chlorophenolics in methanol. Prepare all standards per the

steps below. Observe the safety precautions in Section 5.

7.7.1 Dissolve an appropriate amount of assayed reference

material in a suitable solvent. For example, weigh 50 mg

(±0.1 mg) of pentachlorophenol in a 10-mL ground-glass-

stoppered volumetric flask and fill to the mark with

methanol. After the pentachlorophenol is completely

dissolved, transfer the solution to a 15-mL vial with

PTFE-lined cap.

7.7.2 Stock solutions should be checked for signs of

degradation prior to the preparation of calibration or

performance test standards and shall be replaced after six

months, or sooner if comparison with quality control check

standards indicates a change in concentration.

7.8 Labeled compound spiking solution: From stock solutions

prepared as above, or from mixtures, prepare one spiking

solution to contain the labeled chlorovanillin in acetone

and a second spiking solution to contain the remaining

chlorophenolics, including the 3,4,5-trichlorophenol sample

1086
-------
matrix internal standard (SMIS), in methanol. The labeled

compounds and SMIS are each at a concentration of 12.5
7.9 Secondary standards for^calibration: Using stock

solutions (Section 7.7), prepare one secondary standard

containing the chlorovanilliris and chlorsyringaldehydes

listed in Table 1 in acetone and a second secondary standard

•
containing the remaining chlqrophenolics in methanol. The

monochlorinated phenol, guaiacol, and catechol are included

at a concentration of 25 /Kj/niL; the trichlorinated

catechols, tetrachlorinated g'uaiacol and catechol,

pentachlorophenol, 5,6-dichldrovanillin, and

2,6-dichlorosyringaldehyde are included at a concentration

of 100 /ig/mL; and the remaining compounds are included at a

concentration of 50 pig/mL, each in their respective

I;
solutions.

7.10 Instrument internal standard (IIS): Prepare a solution

of 2 , 2 '-dif luorobiphenyl (DFB) at a concentration of. 2 .5

mg/mL in hexane.

7.11 DFTPP solution: Prepare a solution of DFTPP at 50

/zg/mL in acetone. ;

7.12 Solutions for obtaining authentic mass spectra

(Section 10.2) : Prepare mixtures of compounds at

concentrations which will assure authentic spectra are

obtained for storage in libraries.

7.13 Preparation of calibration solutions.

1087
-------
7.13.1 Into five 1000-mL aliquots of reagent water, spike

50, 100, 200, 500 and 1000 /zL of each of the two solutions

in Section 7.9. Spike 1.00 mL of each of the two labeled

compound spiking solutions (Section 7.8) into each of the

five aliquots. - • '

7.13.2 Using the procedure 'in Section 11, derivatize and

extract each solution, and concentrate the extract to a

final volume of 0.50 mL. This will produce calibration

solutions of nominal 5, 10, 20, 50, and 100 ptg/mL of the

native chlorophenolics and a constant concentration of 25

yUg/mL of each labeled compound and the SMIS (assuming 100%

derivatization and recovery). As noted in Section 11.1.6,

ascorbic acid is added to all samples of final effluents to

stabilize chlorocatechols, but is not added to samples of

pulp and paper in-process wastewaters. Therefore, it is

necessary to prepare separate sets of five initial

calibration standards with and without the addition of

ascorbic acid. Also, in the event that the laboratory is

extracting final effluent samples by both the stir-bar and

separatory funnel procedures (see Section 11.3), initial

calibration standards should be prepared by both methods.

7.13.3 These solutions permit the relative response

(labeled to unlabeled) and the response factor to be

measured as a function of concentration (Sections 10.4 and

10.5) .

7.13.4 The nominal 50 ^ig/mL standard may also be used as a

1088
-------
calibration verification standard (see Section 9.6).

7.14 Ongoing precision and recovery (OPR) standard: Used

for determination of initial (Section 9.3.2) and ongoing

(Section 9.6) precision and recovery. This solution is

prepared by spiking 500 /iL of each the two solutions of* the

secondary calibration standards (Section 7.9) and 1 mL of

each of the two labeled compound spiking solutions (Section

7.8) into 1000 mL of reagent water.

7.15 Stability of solutions:' All standard solutions

(Sections 7.7 through 7.14) shall be analyzed within 48

hours of preparation and on a1 monthly basis thereafter for

signs of degradation. Standards will remain acceptable if

the peak area at the quantitation m/z relative to the DFB

internal standard remains within ±15% of the area obtained

in the initial analysis of the standard.

8.0 Sample Collection, Preservation, and Storage

8.1 Collect'samples in glass, containers (Section 6.1)

following conventional sampling practices (Reference 9) .

Aqueous samples are collected, in refrigerated bottles using

automatic sampling equipment.1

8.2 Sample preservation.

8.2.1 Residual chlorine: If the sample contains residual

chlorine, the chlorine must be reduced to eliminate positive

interference resulting from continued chlorination

reactions. Immediately after sampling, test for residual

chlorine using the following method or an alternative EPA

1089
-------
method (Reference 10).

8.2.1.1 Dissolve a few crystals of potassium iodide in the

sample and add three to five drops of a 1% starch solution.

A blue color indicates the presence of residual chlorine.

8.2.1.2 If residual chlorine is found, add 1 mL of sodium

thiosulfate solution (Section 7.2.1) for each 2.5 ppm of

free chlorine or until the blue color disappears.

8.2.2 Acidification: Adjust pH of all aqueous samples to <2

with sulfuric acid (Section 7.1.2). Failure to acidify

samples may result in positive interferences from continued

chlorination reactions.

8.2.3 Refrigeration: Maintain sample temperature at 0 to

4°C from time of collection until extraction, and maintain

extracts at a temperature of 0 to 4°C from time of

extraction.until analysis.

8.3 Collect a minimum of 2000 mL of sample. This will

provide a sufficient amount for all testing. Smaller

amounts may be collected if the stream is known to contain

high levels of chlorophenolics.

8.4 All samples must be acetylated and extracted within 30

days of collection, and must be analyzed within 30 days of

acetylation. If labeled compound recoveries for a sample do

not meet the acceptance criteria in Table 5 and the 30-day

holding time is not met, a new sample must be collected.

9.0 Quality Control
1090
-------
9.1 Each laboratory that uses this method is required to
i
operate a formal quality assurance program (Reference 8).

The minimum requirements of this program consist of an

initial demonstration of labpratory capability, analysis of

samples spiked with labeled compounds to evaluate and

document data quality, and analysis of standards and blanks
i
as tests of continued performance. Laboratory performance

is compared to established performance criteria to determine

if the results of analyses meet the performance

characteristics of the method.

9.1.1 DFTPP spectrum validity shall be checked at the

beginning of each eight-hour; shift during which analyses are

performed. This test is despribed in Section 9.2.

9.1.2 The laboratory shall make an initial demonstration of

the ability to generate acceptable results with this method.

This ability is established as described in Section 9.3.
j
9.1.3 The laboratory is permitted to modify this method to

improve separations or lower the costs of measurements,

provided all performance specifications are met. Each time

a modification is made to the method, the laboratory is
(
required to repeat the procedures in Sections 10.3 and 9.3.2

to demonstrate method performance. If the detection limits--

for the analytes in this method will be affected by the

modification, the laboratory should demonstrate that each

MDL (40 CFR 136, Appendix B); is less than or equal to the
I,
MDL in this method or one-ttiird the regulatory compliance

f
;1091
-------
level, whichever is higher.

9.1.4 The laboratory shall spike all samples with labeled

compounds and the sample matrix internal standard (SMIS) to

monitor method performance. This test is described in

Section 9.4. When results of these spikes indicate atypical

method performance for samples, the samples are diluted to

bring method performance within acceptable limits (Section

13).

9.1.5 Analyses of blanks are required to demonstrate

freedom from contamination. The procedures and criteria for

analysis of a blank are described in Section 9.5.

9.1.6 The laboratory shall, on an ongoing basis,

demonstrate through analysis of the ongoing precision and

recovery standard (Section 7.14) that the analysis system is

in control. These procedures are described in Section 9.6.

9.1.7 The laboratory shall maintain records to define the

quality of data that is generated. Development of accuracy

statements is'described in Section 9.4.4 and 9.6.3.

9.2 DFTPP spectrum validity: Inject 1 /^L of the DFTPP

solution (Section 7.11) either separately or within a few

seconds of injection of the OPR standard (Section 9.6.)

analyzed at the beginning of each shift. The criteria in

Table 3 shall be met. .

9.3 Initial demonstration of laboratory capability.

9.3.1 Method Detection Limit(MDL): To establish the ability

to detect the analytes in this method, the laboratory should

1092
-------
determine the MDL per the procedure in 40 CFR 136, Appendix

B using the apparatus, reagents, and standards that will be

used in the practice of this method. MDLs less than or

equal to the MDLs in Table 2 should be achieved prior to the

practice of this method. |

9.3.2 Initial precision and recovery (IPR): To establish

the ability to demonstrate control over the analysis system

and to generate acceptable precision and accuracy, the

laboratory shall perform the following operations:

9.3.2.1 Derivatize, extract,; concentrate, and analyze four

1000-mL aliquots of the ongoing precision and recovery
i

standard (OPR; Section 7.14), according to the procedure in

Section 11. Separate sets of IPR aliquots must be prepared

with the addition of ascorbic acid and without. BB

9.3.2.2 Using results of the: four analyses, compute the

average percent recovery (X) and the relative standard

deviation of the recovery (s) for each compound, by isotope

dilution for pollutants with !a labeled analog, and by

internal standard for pollutants with no labeled analog and

for the labeled compounds and the SMIS.

9.3.2.3 For each compound, compare s and X with the

corresponding limits for initial precision and recovery in

Table 5. If s and X for all ^compounds meet the acceptance

criteria, system performance ;is acceptable and analysis of

blanks and samples may begin.- If, however, any individual s

exceeds the precision limit or any individual X falls
1093
-------
outside the range for recovery, system performance is

unacceptable for that compound. In this event, correct the

problem and repeat the test (Section 9.3.2) .

9.4 Labeled compound recovery: The laboratory shall spike

all samples with labeled compounds and the sample matrix

internal standard (SMIS) to assess method performance on the

sample matrix.

9.4.1 Analyze each sample according to the method beginning

in Section 11. •• • .

9.4.2 Compute the percent recovery (P) of the labeled

compounds and the SMIS using the internal standard method

(Section 14.3) with 2,2'-difluorobiphenyl as the reference

compound.

9.4.3 Compare the labeled compound and SMIS recovery for

each compound with the corresponding limits in Table 5. If

the recovery of any compound falls outside its warning

limit, method performance i.s unacceptable for that compound

in that sample. Therefore, the sample is complex. The

sample is diluted and reanalyzed per Section 13.

9.4.4 As part of the QA program for the laboratory, it is

suggested, but not required, that method accuracy for

samples be assessed and records maintained. After the

analysis of five samples for which the labeled compounds

pass the tests in Section 9.4.3, compute the average percent

recovery (P) and the standard deviation of the percent

recovery (sp) for the labeled compounds only. Express the

1094
-------
accuracy assessment as a percent recovery interval from P -

2sp to P + 2sp for each matrix. For example, if P = 90% and

sp = 10%, the accuracy interval is expressed as 70 to 110%.

Update the accuracy assessment for each compound on a

regular basis (e.g., after each 20 to 30 new accuracy

measurements).

9.5 Blanks: Reagent water blanks are analyzed to

demonstrate freedom from contamination.

9.5.1 Extract and concentrat'e a 1000-mL reagent water blank

with each sample batch (samples started through the

extraction process on the same eight-hour shift, to a

maximum of 20 samples). Blanks associated with samples to

which ascorbic acid is added must be prepared with ascorbic

acid, and blanks associated with samples to which ascorbic

acid is not added must be prepared without ascorbic acid.

Analyze the blank immediately, after analysis of the OPR

(Section 7.14) to demonstrate freedom from contamination.

9.5.2 If any of the compounds of interest (Table 1) or any

potentially interfering compound is found in an aqueous

blank at greater than 5 /Kj/L (assuming a response factor of

one relative to the sample matrix internal standard for

compounds not listed in Tables 1), analysis of samples is

halted until the source of contamination is eliminated and a

blank shows no evidence of contamination at this level.

9.6 Calibration verification! and ongoing precision and

recovery: At the beginning of, each eight-hour shift during

1095
-------
which analyses are performed, analytical system performance

is verified for all compounds. Analysis of DFTPP (Section

9.2) and the nominal 50 /xg/mL OPR (Section 11.1.5) is used

to verify all performance criteria. Adjustment and/or

recalibration, per Section 10, shall be performed until all

performance criteria are met. Only after all performance

criteria are met may samples and blanks be analyzed.

9.6.1 Analyze the extract of the OPR (Section 11.1.5) at

the beginning of each eight-hour shift arid prior to analysis

of samples from the same batch. Alternatively, a separate

calibration verification may be performed using an aliquot

of the midpoint calibration standard from Section 7.13 (with

a nominal concentration of 50 //g/mL) . This alternative may

be used to check instrument performance on failure of an

OPR, or when samples extracted with an OPR aliquot are not

analyzed within the same eight-hour analysis shift.

9.6.1.1 Retention times: The absolute retention time of

2,2'-difluorobiphenyl shall be within the range of 765 to

885 seconds, and the relative retention times of all

pollutants and labeled compounds shall fall within the

limits given in Table 2.

9.6.1.2 GC resolution: The valley height between

4, 6-dichloroguaiacol and 3,4-dichloroguaiacol at m/z 192

shall not exceed 10% of the height of the taller of the two

peaks..
1096
-------
9.6.1.3 Multiple peaks: Each compound injected shall give a ^
w
single, distinct GC peak.
9.6.2 Compute the percent recovery of each pollutant (Table
1) by isotope dilution (Section 10.4) for those compounds
that have labeled analogs. Compute the percent recovery of
each pollutant that has no labeled analog by the internal
standard method (Section 10.5), using the
3,4,5-trichlorophenol (SMIS) 'as the internal standard.
Compute the percent recovery of the labeled compounds and
the SMIS by the internal standard method, using the
2,2'-difluorobiphenyl as the internal standard.
9.6.2.1 For each compound, compare the recovery with the
limits for ongoing precision and recovery in Table 5. If
all compounds meet the acceptance criteria, system
performance is acceptable and analysis of blanks and samples
may proceed. If, however, any individual recovery falls
outside of the range given, system performance is
unacceptable for that compound. In this event, there may be
a problem with the GCMS or with the
derivatization/extraction/coricentration systems.
9.6.2.2 GCMS system: To determine if the failure of the OPR
test (Section 9.6.2.1) is due to instrument drift, analyze
i .
the current calibration verification extract (Section
7.13.4), calculate the percent recoveries of all compounds,
and compare with the OPR recovery limits in Table 5. If all
compounds meet these criteria, GCMS performance/stability is

1097
-------
verified, and the failure of the OPR analysis is attributed

to problems in the derivat.ization/extraction/concentration

of the OPR. In this case, analysis of the sample extracts

may proceed. However, failure of any of the recovery

criteria in the analysis of a sample extract requires

rederivatization of that sample (Sections 13.3.1 and

13.3.2). If, however, the performance/stability of the GCMS

is not verified by analysis of the calibration verification

extract, the GCMS requires recalibration and all extracts

associated with the failed OPR must be reanalyzed.

9.6.3 Add results that' pass the specifications in Section

9.6.2.1 to initial and previous ongoing data for each

compound. Update QC charts to form a graphic representation

of continued laboratory performance. Develop a statement of

laboratory accuracy for each pollutant and labeled.compound

in each matrix type (reagent water, C-stage filtrate,

E-stage filtrate, final effluent, etc.) by calculating the

average percent recovery (R) and the standard deviation of

percent recovery (sr) . Express the accuracy as a recovery

interval from R - 2sr to R + 2sr. For example, if R = 95%

and sr = 5%, the accuracy is 85 to 105%.

9.7 The specifications contained in this method can be met

if the apparatus used is calibrated properly, then

maintained in a calibrated state. The standards used for

calibration (Section 10) and for initial (Section 9.3.2) and

ongoing ' (Section 9.6) precision and recovery should be

1098
-------
identical, so that the most precise results will be

obtained. The GCMS instrument in particular will provide

the most reproducible results' if dedicated to the settings

and conditions required for the analyses of chlorophenolics

by thip method.

9.8 Depending on specific prpgram requirements, field

replicates may be collected to determine the precision of

the sampling technique, and spiked samples may be required

to determine the accuracy of the analysis when the internal

standard method is used. J

10.0 Calibration and Standardization

10.1 Assemble the GCMS and establish the operating

conditions in Section 12. Analyze standards per the

procedure in Section 12 to demonstrate that the analytical

system meets the minimum levels in Table 2, and the

mass-intensity criteria in Table 3 for 50 ng DFTPP.

10.2 Mass-spectral libraries!: Detection and identification

of compounds of interest are dependent upon spectra stored

in user-created'libraries.

10.2.1 Obtain a mass spectrum of the acetyl derivative of

each chlorophenolic compound Kpollutant, labeled compound,

and the sample matrix internal standard) by derivatizing and

analyzing an authentic standard either singly or as part of

a mixture in which there is no interference between closely

eluting components. That only a single compound is present

is determined by examination of the spectrum. Fragments not

1099
-------
attributable to the compound under study indicate the

presence of an interfering compound.

10.2.2 Adjust the analytical conditions and scan rate (for

this test only) to produce an undistorted spectrum at the GC

peak maximum. An undistorted spectrum will usually be

obtained if five complete spectra are collected across the

upper half of the GC peak. Software algorithms designed to

"enhance" the spectrum may eliminate distortion, but may

also eliminate authentic m/z's or introduce other

distortion.

10.2.3 The authentic reference spectrum is obtained under

DFTPP tuning conditions (Section 10.1 and Table 3) to

normalize it to spectra from other instruments.

10.2.4 The spectrum is edited by removing all peaks in the

m/z 42 to 45 range, and saving the five most intense mass-

spectral peaks and all other mass spectral peaks greater

than 10% of the base peak (excluding the peaks in the m/z 42

to 45 range). The spectrum may be further edited to remove

common interfering m/z's. The spectrum obtained is stored

for reverse search and for compound confirmation.

10.3 Minimum level: Demonstrate that the chlorophenolics

are detectable at the minimum level (per all criteria in

Section 14) . The nominal 5 /ig/mL calibration standard

(Section 7.13) can be used to demonstrate this performance.

10.4 Calibration with isotope dilution: Isotope dilution is

used when (1) labeled compounds are available, (2)

1100
-------
interferences do not preclude its use, and (3) the

quantitation m/z (Table 4) extracted ion-current profile

(EICP) area for the compound is in the calibration range.

Alternative labeled compounds and quantitation m/z's may be

used based on availability. 'If any of the above conditions

preclude isotope dilution, the internal standard calibration

method (Section 10.5) is used.

10.4.1 A calibration curve encompassing the concentration

range is prepared for each compound to be determined. The

relative response (pollutant jto labeled) vs. concentration

in standard solutions is plotted or computed using a linear
,
regression. The example in figure 1 shows a calibration

curve for phenol using phenol-d5 as the isotopic diluent.

Also shown are the ±10% error limits (dotted lines).

Relative response (RR) is determined according to the

procedures described below. 'A minimum of five data points

are employed for calibration.1

10.4.2 The relative response of a pollutant to its labeled

analog is determined from isotope ratio values computed from

acquired data. Three isotope ratios are used in this
i
process:

RX = the isotope ratio measured for the pure pollutant.
R = the isotope ratio measured for the labeled compound.
Rm = the isotope ratio of ah analytical mixture of pollutant
and labeled compounds.
1101
-------
The m/z's are selected such that Rx > Ry. If Rm is not

between 2Ry and 0.5RX, the method does not apply and the

sample is analyzed by the internal standard method.

10.4.3 Capillary columns sometimes separate the

pollutant-labeled pair when deuterium labeled compounds are

used, with the labeled compound eluted first (Figure 2).

For this case,
R =
X
area m Jz 1

, at the retention time of the pollutant (RT~).
R = -= ^, at the retention time of the labeled compound

y \area m
m
[•

larea at m.lz (at RTj]
R - I 1, as measured in the mixture of the pollutant and
larea at m2/z (at RTjl

labeled compounds (Figure 2), and RR = R .
10.4.4 When the pollutant-labeled pair is not separated (as

occurs with carbon-13-labeled compounds), or when another
*

labeled compound with interfering spectral masses overlaps

the pollutant (a case which can occur with isomeric

compounds), it is necessary to determine the contributions

of the pollutant and labeled compound to the respective EICP

areas.: If the peaks are separated well enough to permit the

data system or operator to remove the contributions of the
1102
-------
compounds to each other, the equations in Section 10.4.3
apply. This usually occurs when the height of the valley
between the two GC peaks at the same m/z is less than 70 to
90% of the height of the shorter of the two peaks. If
significant GC and spectral overlap occur, RR is computed
using the following equation:
** = ^
Where:
Rx is measured as shown in figure 3A,
R is measured as shown in figure 3B,
Rm is measured as shown in figure 3C.
For example, Rx = 46100/4780 = 9.644; Ry = 2650/43600 =
0.0608; R,,, = 49200/48300 = 1.1019; thus, RR = 1.114.
10.4.5 To calibrate the analytical system by isotope
dilution, analyze a I-/JL aliquot of each of the calibration
standards (Section 7.13) using the procedure in Section 12.
Compute the RR at each concentration.
10.4.6 Linearity: If the ratio of relative response to
concentration for any compound is constant (less than 20%
coefficient of variation) over the five-point calibration
range, an averaged relative response/concentration ratio may
be used for that compound; otherwise, the complete
calibration curve for that compound shall be used over the
five-point calibration range.!
10.5 Calibration by internal; standard: The method contains
two types of internal standards, the sample matrix internal

__
-------
standard (SMIS) and the instrument internal standard (IIS) ,

and they are used for different quantitative purposes. The

3, 4,5-trichlorophenol sample matrix internal standard (SMIS)
is used for measurement of .all pollutants with no labeled

analog and when the. criteria for isotope dilution (Section

10.4) cannot be met. The 2, 2 ' -dif luorobiphenyl instrument

internal standard (IIS) is used for determination of the

labeled compounds and the SMIS. The result's are used for
intralaboratory statistics (Sections 9.4.4 and 9.6.3).'
10.5.1 Response factors: Calibration requires the

determination of response factors (RF) for both the

pollutants with no labeled analog and for the labeled

compounds and the SMIS . The response factor is defined by
the following equation:
W,, * c.)
Where:
As = the area of the chracteristic mass for the compound in the daily standard.
Ajs = the area of the characteristic mass for the internal standard.
Cis = the concentration of the internal standard (iig/mL).
Cs = is the concentration of the compound in the calibration standard (\iglmL).

When this equation is used to determine the response factors
for pollutant compounds without labeled analogs, use the
area (Ais) and concentration (Cis) of 3 , 4, 5-trichlorophenol

(SMIS) as the internal standard. When this equation is used
to determine the response factors for the labeled analogs
1104
-------
and the SMIS, use the area (Ais) and concentration (Cis) of

2, 2'-difluorobiphenyl as the 'internal standard.

10.5.2 The response factor i's determined for at least five

concentrations appropriate to the response of each compound

(Section 7.13); nominally, 5,; 10, 20, 50, and 100 /zg/mL.

The amount of SMIS added to each solution is the same (25
j

^g/mL) so that Cis remains constant. Likewise, the

concentration of IIS is constant in each solution. The area

ratio (As/Ais) is plotted versus the concentration ratio

(Cs/Cis) for each compound in the standard to produce a

calibration curve.

10.5.3 Linearity: If the response factor (RF) for any

compound is constant (less than 35% coefficient of

variation) over the five-point calibration range, an

averaged response factor may be used for that compound;

otherwise, the complete calibration curve for that compound

shall be used over the five-point range.

10.6 Combined calibration: By using calibration solutions

(Section 7.13) containing the pollutants, labeled compounds,

and the internal standards, a single set of analyses can be

used to produce calibration qurves for the isotope dilution

and internal standard methods. These curves are verified

each shift (Section 9) by analyzing the OPR standard, or an

optional calibration verification (VER) standard.

Recalibration is required only if OPR criteria (Section 9.6

and Table 5) cannot be met.

1105
-------
11.0 Sample Derivatization, Extraction, and Concentration

The procedure described in this section uses a stir-bar in a

beaker for the derivatization. The extraction procedures

applied to samples depend on the type of sample being

analyzed. Extraction of samples from in-process wastewaters

is performed using a separatory funnel procedure. All

calibrations, IPR, OPR, and blank analyses associated with

in-process wastewater samples must be performed by the

separatory funnel procedure.

Extraction of samples of final effluents and raw water

may be performed using either the stir-bar procedure or the

separatory funnel procedure. However, all calibrations,

IPR, OPR, blank, and sample analyses must be performed using

the same procedure. Both procedures are described below.

11.1 Preparation of all sample types for stir-bar

derivatization.

11.1.1 Allow sample to warm to room temperature.

11.1.2 Immediately prior to measuring, shake sample

vigorously to insure homogeneity.

11.1.3 Measure 1000 mL (±10 mL) of sample 'into a clean

2000-mL beaker. Label the beaker with the sample number.

11.1.4 Dilute aliguot(s).

11.1.4.1 Complex samples: For samples that are expected to

be difficult to derivatize, concentrate, or are expected to

overload the GC column or mass spectrometer, measure an

additional 100 mL (±1 mL) into a clean 2000-mL beaker and

1106
-------
dilute to a final volume of 1000-mL (±50 mL) with reagent

water. Label with the sample number and as the dilute

aliquot. However, to ensurejadequate sensitivity, a 1000-mL

aliquot must always be prepared and analyzed.

11.1.4.2 Pulp and paper industry samples: For in-process

streams such as E-stage and C-stage filtrates and other

in-process wastewaters, it may be necessary to prepare an

aliquot at an additional level of dilution. In this case,

dilute 10 mL (±0.1 mL) of sample to 1000-mL (±50 mL).

11.1.5 QC aliquots: For a batch of samples of the same type

to be extracted at the same time (to a maximum of 20), place
|
two 1000-mL (±10 mL) aliquots of reagent water in clean
i
2000-mL beakers. Label one beaker as the blank and the

other as the ongoing precision and recovery (OPR) aliquot.

Because final effluent samples are treated with ascorbic
i

acid and in-process wastewater samples are not (see Section

lit 1.6), prepare an OPR aliquot and a blank for the final

effluent and a separate pair\for the in-process samples.

Treat these QC aliquots in the same fashion as the

associated samples, adding ascorbic acid to the pair

associated with the final effluents, and not adding ascorbic

acid to the pair associated with the in-process samples.

11.1.6 Ascorbic acid: Added to stabilize chlorocatechols.

However, for pulp and paper industry in-process streams and

other in-process wastewaters, the addition of ascorbic acid

may convert chloro-o-quinones to catechols if these quinones

1107
-------
are present. Separate calibration curves must be prepared

with and without the addition of ascorbic acid (Section

7.13.2) .

11.1.6.1 Spike 5 to 6 mL of the ascorbic acid solution

(Section 7.2.2) into each final effluent sample, and the

associated calibration standards, IPR and OPR aliquots, and

blank.

11.1.6.2 For pulp and paper industry C-stage filtrates,

E-stage filtrates, and untreated effluents,'omit the

ascorbic acid to prevent the conversion of chloro-o-quinones

to catechols. Prepare calibration standards, IPR and OPR

aliquots, and blanks associated with these samples without

ascorbic acid as well.

11.1.7 Spike 1000 /zL of the labeled compound spiking

solution (Sectipn 7.8) into the sample and QC aliquots.

11.1.8 Spike 500 /j.L> of the nominal 50 /ig/mL calibration

solution (Section 7.13.4) into the OPR aliquot.

11.1.9 Adjust the pH of the sample aliquots to between 7.0

and 7.1. For calibration standards, IPR and OPR aliquots,

and blanks, pH adjustment is not required.

11.1.10 Equilibrate all sample and QC solutions for

approximately 15 minutes, with occasional stirring.

11.2 Derivatization: Because derivatization must proceed

rapidly, particularly upon the addition of the K2CO3 buffer,

it is necessary to work with one sample at a time until the

derivatization step (Section 11.2.3) is complete.

1108
-------
11.2.1 Place a beaker containing a sample or QC aliquot on

the magnetic stirrer in a fume hood, drop a clean stirring

bar into the beaker, and increase the speed of the stirring

bar until the vortex is drawn to the bottom of the beaker.

11.2.2 Measure 25 to 26 mL of K2CO3 buffer into a graduated
i

cylinder or other container and 25 to 26 mL of acetic acid

into another.

11.2.3 Add the K2C03 buffer to the sample or QC aliquot,

immediately (within one to three seconds) add the acetic

anhydride, and stir for three to five minutes to complete

the derivatization.

11.3 Extraction: Two procedures are described below for the

extraction of derivatized samples. The choice of extraction

procedure will depend on the sample type. For final

effluent samples, either of two procedures may be utilized

for extraction of derivatized samples. For samples of

in-process wastewaters, the separatory funnel extraction

procedure must be used. •',

Note: Whichever procedure is employed, the same extraction

procedure must be used for calibration standards, IPR

aliquotSf OPR aliguots, blanks, and the associated field

samples.

11.3.1 Stir-bar extraction of final effluents.
1109
-------
11.3.1.1 Add 200 mL (±20 mL) of hexane to the beaker and

stir for three to five minutes, drawing the vortex to the

bottom of the beaker.

11.3.1.2 Stop the stirring and drain the hexane and a

portion of the water into a 500- to 1000-mL separatory

funnel. Allow the layers to separate.

11.3.1.3 Drain the aqueous layer back into the beaker.

11.3.1.4 The formation of emulsions can be expected in any

solvent extraction procedure. If an emulsion forms, the

laboratory must take steps to break the emulsion before

proceeding. Mechanical means of breaking the emulsion

include the use of a glass stirring.rod, filtration through

glass wool, and other techniques. For emulsions that resist

these techniques, centrifugation is nearly 100% effective.

If centrifugation is employed to break the emulsion,

drain the organic layer into a centrifuge tube, cap the

tube, and centrifuge for two to three minutes or until the

phases separate. If the emulsion cannot be completely

broken, collect as much of the organic phase as possible,

and measure and record the volume of the organic phase

collected.

If all efforts to break the emulsion fail, -including

centrifugation, and none of the organic phase can be

collected, proceed with the dilute aliquot (Section

11.1.4.2). However, use of the dilute aliquot will
1110
-------
sacrifice the sensitivity of the method, and may not be

appropriate in all cases. ;

11.3.1.5 Drain the organic layer into a Kuderna-Danish

(K-D) apparatus equipped with a 10-mL concentrator tube.

Label the K-D apparatus. Itmay be necessary to pour the

organic layer through a funnel containing anhydrous sodium

sulfate to remove any traces;of water from the extract.
I
11.3.1.6 Repeat the extraction (Section 11.3.1.1 through

11.3.1.5) two more times using another 200-mL of hexane for

each extraction, combining the extracts in the K-D

apparatus.

11.3.1.7 Proceed with concentration of the extract, as

described in Section 11.4.

11.3.2 Separatory funnel extraction of either final flB

effluents or in-process wastewaters.

11.3.2.1 Transfer the derivatize£ sample or QC aliquot to a

2-L separatory funnel.

11.3.2.2 Add 200 mL (±20 mL)' of hexane to the separatory

funnel. Cap the funnel and extract the sample by shaking

the funnel for two to three minutes with periodic venting.

11.3.2.3 Allow the organic layer to separate from the water

phase for a minimum of 10 minutes.

11.3.2.4 Drain the lower aqueous layer into the beaker used

for derivatization (Section 11.2), or into a second clean 2-

L separatory funnel. Transfer the solvent to a 1000-mL K-D

flask. It may be necessary to pour the organic layer
f

1111
-------
through a funnel containing anhydrous sodium sulfate to

remove any traces of water from the extract.

11.3.2.5 The formation of emulsions can be expected in any

solvent extraction procedure. If an emulsion forms, the

laboratory must take steps to break the emulsion before

proceeding. Mechanical means of breaking the emulsion

include the use of a glass stirring rod, filtration through

glass wool, and other techniques. For emulsions that resist

these techniques, centrifugation may be required.

If centrifugation is employed to break the emulsion,

drain the organic layer into a centrifuge tube, cap the

tube, and centrifuge for two to three minutes or until the

phases separate. If the emulsion cannot be completely

broken, collect as much of the organic phase as possible,

and measure and record the volume of the organic phase

collected. If all efforts to break the emulsion, including

centrifugation, fail and none of the organic phase can be

collected, proceed with the dilute aliquot (Section

11.1.4.2). However, use of the dilute aliquot will

sacrifice the sensitivity of the method, and may not be

appropriate in all cases.

11.3.2.6 . If drained into a beaker, transfer the aqueous

layer to the 2-L separatory funnel (Section 11.3.2.1).

Perform a second extraction using another 200 mL of fresh

solvent.
1112
-------
11.3.2.7 Transfer the extract to the 1000-mL K-D flask in

Section 11.3.2.4.

11.3.2.8 Perform a third extraction in the same fashion as

above.

11.3.2.9 Proceed with concentration of the extract, as

described in Section 11.4.

11.4 Macro concentration: Concentrate the extracts in
i '
I

separate 1000-mL K-D flasks equipped with 10-mL concentrator

tubes. Add one to two clean iboiling chips to the flask and

attach a three-ball macro-Snyder column. Prewet the column

by adding approximately 1 mL ,of hexane through the top.

Place the K-D apparatus in a ihot water bath so that the

entire lower rounded surface of the flask is bathed with

steam. Adjust the vertical position of the apparatus and
t

the water temperature as required to complete the

concentration in 15 to 20 minutes. At the proper rate of

distillation, the balls of the column will actively chatter
f

but the chambers will not flood. When the liquid has

reached an apparent volume of 1 mL, remove the K-D apparatus

from the bath and allow the solvent to drain and cool for at

least 10 minutes. Remove the Snyder column and rinse the

flask and its lower joint into the concentrator tube with 1

to 2 mL of hexane. A 5-mL' syringe is recommended for this

operation. <
1113
-------
11.5 Micro-concentration: Final concentration of the

extracts may be accomplished using either a micro-Snyder

column or nitrogen evaporation.

11.5.1 Micro-Snyder column: Add a clean boiling chip and

attach a two-ball micro-Snyder column to the concentrator

tube. Prewet the column by adding approximately 0.5 mL

hexane through the top. Place the apparatus in the hot

water bath. Adjust the vertical position and the water

temperature as required to complete the concentration in 5

to 10 minutes. At' the proper rate of distillation, the

balls of the column will actively chatter but the chambers

will not flood. When the liquid reaches an apparent volume

of approximately 0.2 mL, remove the apparatus from the water

bath and allow to drain and cool for at least 10 minutes.

Remove the micro-Snyder column and rinse its lower joint

into the concentrator tube with approximately 0.2 mL of

hexane. Adjust to a final volume of 0.5 mL.

11.5.2 Nitrogen evaporation: Transfer the concentrator tube

to a nitrogen evaporation device and direct a gentle stream

of clean dry nitrogen into the concentrator. Rinse the

sides of the concentrator tube with small volumes of hexane,

. and concentrate the extract to a final volume of 0.5 mL.

11.6 Spike each extract with 10' /zL of the

2,2'-difluorobiphenyl IIS (Section 7.10) and transfer the

concentrated extract to a clean screw-cap vial using hexane

to rinse the concentrator tube. Seal the vial with a

1114
-------
PTFE-lined lid, and mark the ilevel on the vial. Label with

the sample number and store in the dark at -20 to -10°C

until ready for analysis.

12.0 GCMS Analysis \

12.1 Establish the following operating conditions:

Carrier gas flow: j Helium at 30 cm/sec at 50°C

Injector temperature: 300°C

Initial temperature: ; 50°C

Temperature program: 8°c/min to 270°c

Final hold: Until after 2,6-

dichlorosyringaldehyde elutes

Adjust the GC conditions to meet the requirements in Section

9.6.1.1 and Table 2 for analyte separation and sensitivity.

Once optimized, the same GC conditions must be used for the WB
I u
analysis of all standards, blanks, IPR and OPR aliquots, and

samples.

12.2 Bring the concentrated.extract (Section 11.6) or

standard (Sections 7.13 and 7.14) to room temperature and

verify that any precipitate has redissolved. Verify the

level on the extract (Sections 7.13, 7.14, and 11.6) and

bring to the mark with solvent if required.

12.3 Inject a l-/iL volume of the standard solution or

extract using on-column or splitless injection. For 0.5 mL

extracts, this l-/iL injection volume will contain 50 ng of

the DFB internal standard. If an injection volume other

than 1 /zL is used, that volume must contain 50 ng of DFB.

1115
-------
12.4 Start the GC column temperature ramp upon injection.
Start MS data collection after the solvent peak elutes.
Stop data collection after the 2,6-dichlorosyringaldehyde
peak elutes. Return the column to the initial temperature
for analysis of the next sample.
13.0 Analysis of Complex Samples
Some samples may contain high levels (>1000 /ig/L) of the
compounds of interest, interfering compounds, and/or other
phenolic materials. Some samples will not concentrate to
0.5 mL (Section 11.5); others will overload the GC column
and/or mass spectrometer; others may contain amounts of
phenols that may 'exceed the capacity of the derivatizing
agent.
13.1 Analyze the dilute aliquot (Section 11.1.4) when the
sample will not concentrate to 0.5 mL. If a dilute aliquot
was not extracted, and the sample holding time (Section 8.4)
has not been exceeded, dilute an aliquot of sample with
reagent water, and derivatize and extract it (Section
11.1.4). Otherwise, dilute the extract (Section 14.7.3) and
quantitate it by the internal standard method (Section
14.3) .
13.2 Recovery of the 2,2'-difluorobiphenyl instrument
internal standard: The EICP area of the internal standard
should be within a factor of two of the area in the OPR or
VER standard (Section. 9.6). If the absolute areas of the
labeled compounds and the SMIS are within a factor of two of
1116
-------
the respective areas in the OPR or VER standard, and the DFB

internal standard area is less than one-half of its

respective area, then internal standard loss in the extract

has occurred. In this case,\analyze the extract from the
i

dilute aliquot (Section 11.1,4).

13.3 Recovery of labeled compounds and the sample matrix.

internal standard (SMIS): SMIS and labeled compound recovery

I
specifications have been developed for samples with and

without the addition of ascorbic acid. Compare the

recoveries to the appropriate limits in Table 5.

13.3.1 If SMIS or labeled compound recoveries are outside

the limits given in Table 5 and the associated OPR analysis

meets the recovery criteria, I the extract from the dilute

aliquot (Section 11.1.4) is analyzed as in Section 14.7.

13.3.2 If labeled compound or SMIS recovery is outside the

limits given in Table 5 and the associated OPR analysis did

not meet recovery criteria, a problem in the

derivatization/extraction/concentration of the sample is

indicated, and the sample must be rederivatized and

reanalyzed.
l

14.0 Data Analysis and Calculations

14.1 Qualitative determination: Identification is

accomplished by comparison of data from analysis of a sample

or blank with data stored in: the mass spectral libraries..
Identification of a compound

criteria are met:
is confirmed when the following
1117
-------
14.1.1 The signals for m/z 43 (to indicate the presence of

the acetyl derivative) and all characteristic m/z's stored

in the spectral library (Section 10.2.4) shall be present

and shall maximize within the same two consecutive scans.

14.1.2 Either (1) the background corrected EICP areas, or

(2) the corrected relative intensities of the mass spectral

peaks at the GC peak maximum shall agree within a factor of

two (0.5 to 2 times) for all m/z's stored in the library.

14.1.3 The relative retention time shall be within the

window specified in Table 2.

14.1.4 .The m/z's present in the mass spectrum from the

component in the sample that are not present in the

reference mass spectrum shall be accounted for by

contaminant or background ions. If the mass spectrum is

contaminated, an experienced spectrometrist (Section 1.4)

shall determine the presence or absence of the compound.

14.2 Quantitative determination by isotope dilution: By

adding a known amount of a labeled compound to every sample

prior to derivatization and extraction, correction for

recovery of the pollutant can be made because the pollutant

and its labeled analog exhibit the same effects upon

derivatization, extraction, concentration, and gas

chromatography. Relative response (RR) values for sample

mixtures are used in conjunction with calibration curves

described in Section 10.4 to determine concentrations

directly, so long as labeled compound spiking levels are

1118
-------
constant. For the phenol example given in Figure 1 (Section
10.4.1), RR would be equal to1 1.114. For this RR value, the
phenol calibration curve given in Figure 1 indicates a
concentration of 27 /ig/mL in the sample extract (Cex) .
14.2.1 Compute the concentration in the extract using the
response ratio determined from calibration data (Section
10.4) and the following equation:
L) = (An x C,) / (Al x RR)
Where: \
C a = concentration of the pollutant in the extract.
An- area of the characteristic m/z for the
pollutant.
Cl = concentration of the labeled compound in the extract.
Aj = area of the characteristic mlz for the labeled compound.
RR = response ratio from the initial calibration.
14.2.2 For the IPR (Section 9.3.2) and OPR (Section 9.6),
compute the percent recovery of each pollutant using the
equation in Section 14.6. The percent recovery is used for
the evaluation of method and laboratory performance, in the
form of IPR (Section 9.3.2) and OPR (Section 9.6).
14.3 Quantitative determination by internal standard:
Compute the concentration using the response factor
determined from calibration data (Section 10.5) and the
following equation:
1119
-------
Cex(ng/mL) = (A, x CJ / (Ais x

Where:
Cex = concentration of the pollutant in the extract.
As= area of the characteristic m/z for the pollutant.
Cjs = concentration of the internal standard in the extract
(see note below).
A.s = area of the characteristic m/z for the internal standard.
RF = response factor from the initial calibration.

Note: When this equation is used to compute the extract

concentrations of native compounds without labeled analogs,

use the area (Ais) and concentration (Cis) of

3,4,5-trichlorophenol (SMIS) as the internal standard.

For the IPR (Section 9.3.2) and OPR (Section 9.6),

compute the percent recovery using the equation in Section
14.6.

Note: Separate calibration curves will be required for

samples with and without the addition of ascorbic acid, and

also for both extraction procedures (stir-bar and separatory

funnel) where applicable.

14.4 Compute the concentration of the labeled compounds and
the SMIS using the equation in Section 14.3, but using the
area and concentration of the 2,2'-difluorobiphenyl as the
internal standard, and the area of the labeled compound or
SMIS as As.

14.5 Compute the concentration of each pollutant compound
in the sample using the following equation:
1120
-------
o
•where:
Cs = Concentration of the pollutant in the sample.
Ca = Concentration of the pollutant in the extract.
V^. = Volume of the concentrated extract (typically 0.5 mL).
V = Volume of the original sample in liters.

Primaryl4•6 Compute the recovery of each labeled compound
and the SMIS as the ratio of 'concentration (or amount) found

to the concentration (or amount) spiked, using the following

equation:

Concentration found ,„,.
Percent recovery = —— x 100
Concentration spiked

These percent recoveries are .used to assess method
performance according to Sections 9 and 13.
14.7 If the EICP area at the quantitation m/z for any
i.
compound exceeds the calibration range of the system, three
approaches are used to obtain results within the calibration

range.
14.7.1 If the recoveries of'all the labeled compounds in
the original sample aliquot meet the limits in Table 5, then
the extract of the sample may be diluted by a maximum of a
factor of 10, and the diluted extract reanalyzed.
14.7.2 If the recovery of aiiy labeled compound is outside
its limits in Table 5, or if a tenfold dilution of the
extract will not bring the pollutant- within the calibration
range, then extract and analyze a dilute aliquot of the

1121
-------
sample (Section 11) . Dilute 100 mL, 10 mL, or an

appropriate volume of sample to 1000 mL with reagent water

and extract per Section 11.

14.7.3 If the recoveries of all labeled compounds in the

original sample aliquot (Section 14.7.1) meet the limits in

Table 5, and if the sample holding time has been exceeded,

then the original sample extract is diluted by successive

factors of 10, the DFB internal standard is added to give a

concentration of 50 ^ug/mL in the diluted extract, and the

diluted extract is analyzed. Quantitation of all analytes

is performed using the DFB internal standard.

14.7.4 If the recoveries of all labeled compounds in the

original sample aliquot (Section 14.7.1) or in the dilute

aliquot (Section 14.7.2) (if a dilute aliquot was analyzed)

do not meet the limits in Table 5, and if the holding time

has been exceeded, re-sampling is required.

14.8 Results are reported for all pollutants, labeled

compounds, and the sample matrix internal standard in

standards, blanks, and samples, in units of /xg/L.

14.8.1 Results for samples which have been diluted are

reported at the least dilute level at which the area at the

quantitation m/z is within the calibration range (Section

14.7).

14.8.2 For compounds having a labeled analog, results are

reported at the least dilute level at which the area at the

quantitation m/z is within the calibration range (Section

1122
-------
14.7) and the labeled compound recovery is within the normal

range for the method (Section 13.3).

15.0 Method Performance
I

15.1 Single laboratory performance for this method is

detailed in References 1, 2, and 11. Acceptance criteria

were established from multiple laboratory use of the draft

method.
i
15.2 A chromatogram of the ongoing precision and recovery

standard (Section 7.14) is shown in Figure 4.

16.0 Pollution Prevention j

16.1 The solvents used in this method pose little threat to

the environment when'recycled and managed properly.

16.2 Standards should be prepared in volumes consistent

with laboratory use to minimize the volume of expired

standards to be disposed. I

17.0 Waste Management

17.1 It is the laboratory's responsibility to comply with

all federal, state, and local[ regulations governing waste

management, particularly the hazardous waste identification

rules and land disposal restrictions, and to protect the

air, water, and land by minimizing and controlling all

releases from fume hoods and bench operations. Compliance

with all sewage discharge permits and regulations is also

required.
1123
-------
17.2 Samples preserved with HC1 or H2SO4 to pH < 2 are

hazardous and must be neutralized before being disposed, or

must be handled as hazardous waste.

17.3 For further information on waste management, consult

"The Waste Management Manual for Laboratory Personnel", and

"Less is Better:- Laboratory Chemical Management for Waste

Reduction", both available from the American Chemical

Society's Department of Government Relations and Science

Policy, 1155 16th Street N.W., Washington, B.C. 20036.

18.0 References

18.1 "Chlorinated Phenolics in Water by In Situ

Acetylation/GC/MS Determination," Method CP-86.01, National

- Council of the Paper Industry for Air and Stream

Improvement, Inc., 260 Madison Avenue, New York, NY 10016

(July 1986).

18.2 "6240-Chlorinated Phenolics (Interim Standard)," Draft

Version, U. S. Environmental Protection Agency, Manchester

Laboratory, Manchester, Washington.

18.3 "Performance Tests for the Evaluation of Computerized

Gas Chromatography/Mass Spectrometry Equipment and

Laboratories," USEPA, EMSL Cincinnati, OH 45268,

EPA-600/4-80-025 (April 1980).

18.4 "Working with Carcinogens," DHEW, PHS, CDC, NIOSH,

Publication 77-206 (August 1977).

18.5 "OSHA Safety and Health Standards, General Industry,"

OSHA 2206, 29 CFR 1910 (January 1976).

1124
-------
18.6 "Safety in Academic Chemistry Laboratories," ACS

Committee on Chemical Safety (1979).

18.7 "Interlaboratory Validation of U. S. Environmental

Protection Agency Method 1625A, Addendum Report," SRI

International, Prepared for Analysis and Evaluation Division

(WH-557), USEPA, 401 M St. SW, Washington, DC 20460 (January

1985).

18.8 "Handbook of Analytical Quality Control in Water and

Wastewater Laboratories," USEPA, EMSL, Cincinnati, OH 45268,

EPA-600/4-79-019 (March 1979) .

18.9 "Standard Practice for ^Sampling Water," ASTM Annual

Book of Standards, ASTM, Philadelphia, PA, 76 (1980) .

18.10 "Methods 330.4 and 330.5 for Total Residual

Chlorine," USEPA, EMSL, Cincinnati, OH 45268, EPA

600/4-70-020 (March 1979).

18.11 "Determination of Chlorophenolics, Special Analytical

Services Contract 1047, Episode 1886," Analytical

Technologies, Inc., Prepared for W. A. Telliard, Industrial

Technology Division (WH-552), USEPA, 401 M St. SW,

Washington, DC 20460 (June 1990).

18.12 "Determination of Chlorophenolics by GCMS,

Development of Method 1653," 'Analytical Technologies, Inc.,

Prepared for W. A. Telliard, industrial Technology Division

(WH-552), USEPA, 401 M St. SW, Washington, DC 20460 (May

1991).
1125
-------
19.0 Tables and Figures
Table 1. Chlorophenolic Compounds Determined by GCMS using

Isotope Dilution and Internal Standard Techniques
Compound
1-chlorophenol
2 , 4 -dichlorophenol
2 , 6 -dichlorophenol
2 , 4 , 5-trichlorophenol
2,4, 6-trichlorophenol
2,3,4, 6-tetrachloroph-
snol
pentachlorophenol
1 - chloroguaiacol
3 , 4 -dichloroguaiacol
1 , 5 -dichloroguaiacol
1 , 6 -dichloroguaiacol
3,4, 5 -tri chloroguaia-
nol
3,4, 6-trichloroguaia-
rol
1,5, 6-trichloroguaia-
=01
tetrachloroguaiacol
4-chlorocatechol
3 , 4 -dichlorocatechol
3 , 6 -dichlorocatechol
1 , 5 -dichlorocatechol
3 , 4 , 5-trichlorocatec-
10!
3 , 4, 6-trichlorocatec-
aol
tetrachlorocatechol
5-chlorovanillin
S - chlorovani 1 1 in
5, 6 -di chlorovani 11 in
Pollutant
CAS Registry
106-48-9
120-83-2
87-65-0
95-95-4
88-06-2
58-90-2
87-86-5
16766-30-6
77102-94-4
2460-49-3
16766-31-7
57057-83-7
60712-44-9
2668-24-8
2539-17-5
2138-22-9
3978-67-4
3938-16-7
3428-24-8
56961-20-7
32139-72-3
1198-55-6
19463-48-0
18268-76-3
18268-69-4
EPA-EGD
1001
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013
1014
1015
1016
1017
1018
1019
1020
1021
1022
1023
1024
1025
Labeled Compound
Analog

<*3

13C6
13C6

13C6

13C6
13c6

CAS Registry

93951-74-7

85380-74-1
136955-39-0

136955-40-3
136955-41-4

.136955-42-5

136955-43-6
136955-44-7

EPA-
EGD

1102

1107
1108

1114
1115

1119

1122
1123

1126
-------
2-chlorosyringaldehyde 76341-69-0
2,6-
iichlorosyringaldehyde
trichlorosyringol
76330-06-8
2539-26-6
1026
1027
1028
Sample matrix internal standard (SMIS)
3,4,5-trichlorophenol
609-19-8
184
Instrument internal standard (IIS)',
2,2'-di£luorobiph.enyl | 388-82-9
164
1127
-------
m
o
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i — 1
0
a
o
SH
O
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43
U
rH
o
CQ
4J
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6
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(U
Q
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(0
SN
43
as Chromatograp
T-K
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is;

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Compound

rH
rH
H

in
CM
rH

rH
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VD
O
1
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in
VO
O

•*
co
rH

tH
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VD

4-chlorophenol

rH
O
O
rH

Ol
ro
rH

in
CM

Ol
p~
r-
o
i
r-
m
r-
o

•*
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VD
Ol

6 -dichlorophenol
«.
CM

co
o
o
tH

CO
Ol
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o
1
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CO
°]
0

•*
VO
rH

CO
rH
CO

- di chl or opheno 1 - d3
^
„.
CM

CM
O
H
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in
H
o

in
CM

VD
O
O
rH
1
r-
Ol
Ol
o

CM
o
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tH

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CO

4 -dichlorophenol
>•
CM

O
CM
rH

O
O
•
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^
VD
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in
CM
CO

1 -dif luorobiphenyl
(I.S.)
CM

VO
rH

ro
O
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1
r-.
[--
O
tH

^
VO
tH

O
O
cn

ihloroguaiacol - 13C6
u
i
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CO
o
rH
rH

cn
o
o

in
H

in
*

0
rH
O
tH

r-
in
o

in
CM

CO
in
0
rH
I
t-
ro
o,
tH

^,
CO
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CO
o
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-dichlorocatechol
VO
^
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CO
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0
tH

co
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in
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CO
f-
o
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1
o
in
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lorophenol
CM

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^
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r-
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VD
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hlorovanillin-13C6
u
i
in

ro
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in
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tH
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Ol
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-chlorovanillin
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l/>
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-chlorovanillin
VO

CM
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O
VD
O

in
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in
o
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ro
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-dichlorocatechol
*3*
„
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r-
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H
I

CO
ro
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rH

CO
in
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10
ichlorocatechol -13C
•d

in
•=»<

cn
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CO
cs
-------

*> ^?
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S Di

§M~
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c S §)
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s

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EH 0
pi *o
K £«
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ro
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in

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1
cn
o
M
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CO
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CO
r-
ro

, 6-dichlorosy-
ringaldehyde
CM

CM
0
H
d by the internal standard
0)
-H
t-t
-rl
JJ
S3
(d
3
tj1

jj
S3
(d
jj
3
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ft

0)
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43

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Ti

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pound quantified by the
E
o
u

T5
1
43
laboratory {reference 12) ,

0)
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OS
cs
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to -H IH

01 O1 U
OJ 0)
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-i H ft
r-H JJ
(d , rH
S-l rH (d

JJ S3 JJ
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43
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0) JJ nJ
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nS a)
ri u
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tn
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0) O rH
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£ (d (d cd
•H ta ^ - PL,
ri -H jj w
•H s ri JJ e!
s cn a> ^j fe
o o cn u
u rt -H

-------
Table 3. DFTPP Mass Intensity Specifications1
Reference 7
Mass
51
68
69
70
127
197
198
199
275
441
442
443
•Intensity Required
8 to 82% of m/z 198 •
less than 2% of m/z 69
11 to 91% of m/z 198
less than 2% of m/z 69
32 to 59% of m/z 198
less than 1% of m/z 198
base peak, 100% abundance
4 to 9% of m/z 198
11 to 30% of m/z 198
44 to 110% of m/z 443
30 to 86% of m/z 198
14 to 24% of m/z 442
1131
-------
Table 4. Characteristic m/z's of Chloropheholic Compounds
Compound
4 -chlorophenol
2 , 4-dichlorophenol
2 , 4-dichlorophenol-d3
2 , 6 -dichlorophenol
2 , 4 , 5-trichlorophenol
2,4, S-trichlorophenol
2,3,4, 6-tetrachlorophenol
pentacnioropnenoi
pentachlorophenol~i3C6
4 - chloroguaiacol
4 - chloroguaiacol - 13C6
3 , 4 -di chloroguaiacol
4 , 5 -di chloroguaiacol
4 , 6-dichloroguaiacol
3 ,4, 5 -tri chloroguaiacol
3,4, 6-trichloroguaiacol
4 , 5 , 6-trichloroguaiacol
4,5, 6-trichloroguaiacol-13C6
tetrachloroguaiacol
tetrachloroguaiacol -13C6
4 - chlorocatechol
3 , 4-dichlorocatechol
3 , 6-dichlorocatechol
4 , 5 -di chlorocatechol
4, 5-dichlorocatechol-13C6
3,4, 5-trichlorocatechol
3,4, 6-trichlorocatechol
tetrachlorocatechol
tetrachlorocatechol - 13C6
5 -chlorovanillin
5 - chlorovani 1 1 in~13C6
6 - chl orovani 1 1 in
5 , 6-dichlorovanillin
2 -chlorosyringaldehyde
2 , S-dichlorosyringaldehyde
tri chlorosyr ingo 1
Primary m/z
128
162
167
162
196
196
232
266
272 •
158
164
192
192
192
226
226
226
234
262
268
144
178
178
178
184
212
212
248
254
186
192
186
220
216
250
256
Sample Matrix Internal Standard (SMIS)
3,4, 5-trichlorophenol
196
Instrument Internal Standard (IIS)
2,2' -dif luorobiphenyl
190
1132
-------

In
cn
a)
o
nj

O
(U
a,

w
O

(d
•H
rl
(U
JJ
•H
M
U

(U
O
rrt
Table 5. Accepts

TJ •
C en .. u
is -y -H
• 0 rQ "O tJ7
-o o 2 t! -H *
(3 CD -H O O
3 CO ID •" U (d rv
O 3 W *
ts^ «tji cO
H rH
0)
U £> T3
TlJ U (u r*
rH U •"
S » s -a s *
II * 8 8 p,
^w S
»&»3
-H 2 ^ CO
OK O
21 8 6 il
S i
Otj
rl ^ ^.^ LJ
J»| ^ " "H
ft § 8 • s
rH -rl 0 °] H
5 w -> u cu
"ri , q) o.
JJ T3 rn *-? CQ
•H C W
c m
H

*>"•!
en y B

o
CN
H

r^
VO
H
1
c-
CN

H
1
co

in
i
rH
VO
cn
vo
1
co
in

r-l
CN

in
CN

=ntachlorophenol-13C6
ft
•r-
o
rH
H

O
CN
1
CO
CO
o
CN
1
03
03

0
CN

in
CN

4-chloroguaiacol

03
O
CN
rH

CO
VO
H
1
ro
^t1

rH
CN
rH
1
0\
in
CN
in
i
^
VD
CO
rH
i
00
VD

O
rH

in
CN

:-chloroguaiacol-13C6

00
2
*""!

VD
1
rn
i
CN
CO
VD
CN
1
0
00

CO
H

o
in

, 4-dichloroguaiacol4
ro
cn
o
o
H

co
CN
1
O
CO
rH
CN
1
CN
00

0
in

, 5-dichloroguaiacol
rf
O
H
O
rH

O
CN
1
VD
CO
VO
CN
rH
i
CN
03

vo
rH

O
in

, 6-dichloroguaiacol
•*
rH
rH
O
rH

ro
1
0
oo
o
ro
1
CO
^

vo
H

O
in

,4,5-trichloroguai-
acol
ro
CN
rH
O
rH

O
-------
en
ro
H
1
i-H
in
H
ro
H
1
00
<*
o
^
rH
1

VD
^ji
H
1
VD
VO

CO
in
OJ
4,5, 6-trichloroguai-
acol-13C6
•>#
rH

VD
CM
i-H
1
rH
CO

in
H
i-H
1
*^
CO

^
o
o
H
tetrachloroguaiacol
in
rH
CM
H
H
VD
H
1
r-
CM
o
O)
H
1
in
ro
i-H
VD
H
1
in
VD

ro
f^
i-H
1
r-
m

CM
CM
in
CM
tetrachloroguaiacol -
"C6
in
H
rH
rH

CN
rH
1
O
CO

O
^
rH
1
VD
f-

CO
in
CM
4-chlorocatechol
VD
rH
O
rH

ro
rH
1
CO
I-

•>#
in
rH
1
VD
VD

CN
O
in
3 , 4-dichlorocatechol
r-
i-H
O
rH

VO
CM
rH
1

VD
ro
rH
1
co
f-

VD
rH
O
in
3 , 6-dichlorocatechol
CO
rH
O
H

CM
CM
rH
1
VD
CO

00
rH
rH
1
T^
CO

CO
o
in
4, 5-dichlorocatechol
en
H
CM
H

CM
rH
1
to
ro
CM
«^1
rH
1
VO
VO

•*
^
i-H
1
CO
VD

CO
t-
in
CM
4 , 5-dichlorocatechol-
13C6
en
i-H
i-H
rH

CO
CM
rH
1
CM
r-

VD
VO
rH
1
O
VD

r-
i-H
o
0
H
3,4, 5-trichlorocate-
chol
O
CM
O
rH

en
^
rH
1

CO
ro
rH
1
**F
r-

rH
O
O
rH
3,4, 6-trichlorocate-
chol4
rH
CM
O
rH

CM
ro
•I-H
l
H
CO

•*
ro
CM
1
VD
^

cn
CM
o
o
rH
tetrachlorocatechol
CM
CM
CM
rH
i

CO
i-H
rH
1
*3*
rH
CM
in
rH
1
ro
VD

r-
OJ
Ol
1
CO
^

ro
in
O]
tetrachlorocatechol -
13C6
0)
OI
i-H
i-H

CO
rH
rH
1

CO
O
O)
1
*3*
cn

o
OJ
o
in
5 -chlorovani 11 in
ro
CM
CM
H

in
CM
I
CM
ro
VD
CM
i-H
I
rH
in

^
rH
1
O
t—

O
VD
rH
1
CO
VD

CO
in
CM
5 - chlorovani 11 in- 13C6
ro
CM
rH
rH

VD
CM
rH
1
O
CO

co
CM
rH
1
CM
CO

CM
CM
O
in
6-chlorovanillin

CM
O
i-H

O
•st1
rH
1
r-
r-

VD
*3*
rH
1
r-
vo

en
o
o
i-H
5, 6-dichlorovanillin
in
CM
0
rH

VD
in
i-H
I
CM
r-

o
ro
t-H
1
VD
r-

co
CM
o
in
2 -chlorosyringaldehyde
VD
CM
O
rH

ro
CO
rH
1
O
VD

cn
CM
H
1
CM
CO

rH
O
O
H
2 , 6-dichlorosyring-
aldehyde
r-
0]
0
H

r-
rH
1
VD
VD

VD
ro
rH
1
VD
f-

CO
H
o
in
trichlorosyringol
CO
CM
0
i-H

'C
JH
ns
•o
«
4J
to

.
ns

l\
(U
jj
C!
r-j
4J
§
-------
dicate a pollutant quantified by the internal standard
th 11 indicate a labeled compound quantified by the
mbers beginning with 12 indicate a pollutant quantified
mL.
G
•H

0
H

f*
JJ
•H
3

01
G
-H

•r)
01

•H
M
0)
•d
cJ
o
-H
JJ
trf
U
•H
•H
O
0)
a
w
co
-------
10 -
1.0 -
0.1 -
T-
10
—r—
20
—I—
50
—i r—
100 200
Concentration (pg/mL)
The dotted lines enclose a ±10% error window.
Figure 1. Relative Response Calibration Curve for Phenol
1136
-------
Area at
Area at
M-./Z

Area at
M/Z
Area at
Figure 2. Extracted Ion-Current Profiles for Chromatographically
Resolved Labeled (Ma/Z) and Unlabeld (fi/^/Z) Pairs
1137
-------
<3A)
Aiea= 46100
Aiea= 4780
(3BJ
Area= 2650
Area= 43600
Area = 49200
Aiea= 48300
Figure 3. Extracted Ion-Current Profiles for (3A) Unlabeled Compound, (3B) Labeled
Compound, and (3Q Equal Mixture of Unlabeled and Labeled Compounds
1138
-------
10:12 13:24
1638 SD:00

ReiBntion lime (Minutes)
• 23:12
Figure 4. Chromatogram of Chbropheroics
1139
-------
20.0 Glossary of Definitions and Purposes

These definitions and purposes are specific to this method

but have been conformed to common usage as much as possible.

20.1 Units of weight and measure and their abbreviations

20.1.1 Symbols.

°C degrees Celsius

ftL> microliter '

< less than

> greater than

% percent

20.1.2 Alphabetical characters.

cm centimeter

g gram

h hour

ID inside diameter

in. inch

L liter

M Molecular ion ,

m meter

mg milligram

min minute

mL milliliter

mm millimeter

m/z mass-to-charge ratio
1140
-------
N normal; gram molecular weight of

solute divided by hydrogen equivalent

of solute, per liter of solution

OD outside diameter

pg picogram

ppb part-per-billion

ppm part-per-million

ppt part-per-trillion

psig pounds-per-square inch gauge

v/v volume per unit volume

w/v weight per unit volume

20.2 Definitions and acronyms (in alphabetical order).

Analyte: A chlorophenolic tested for by this method.

The analytes are listed in Table 1.

Calibration standard (CAL): A solution prepared from a

secondary standard and/or stock solutions and used to

calibrate the response of the instrument with respect to

analyte concentration.

Calibration verification standard (VER): The mid-point

calibration standard (CSS) that is used to verify

calibration. See Table 4.

Chlorophenolics: collectively, the analytes listed in

Table 1. i

CS1, CS2, CSS, CS4, CS5 :• See Calibration standards and

Table 4.

1141
-------
Field blank: An aliquot of reagent water or other

reference matrix that is placed in a sample container in the

laboratory or the field, and treated as a sample in all

respects, including exposure to sampling site conditions,

storage, preservation, and all analytical procedures. The

purpose of the field blank is to determine if the field or

sample transporting procedures and environments have

contaminated the sample.

GC: Gas chromatograph or gas chromatography.

• HRGC: High resolution GC.

IPR: Initial precision and recovery; four aliguots of

the diluted PAR standard analyzed to establish the ability

to generate acceptable precision and accuracy. An IPR is

performed prior to the first time this method is used and

any time the method or instrumentation is modified.

K-D: Kuderna-Danish concentrator; a device used to

concentrate the analytes in a solvent.

Laboratory blank: See Method blank.

Laboratory control sample (LCS): See Ongoing precision

and recovery standard (OPR).

Laboratory reagent blank:. See Method blank.

May: This action, activity, or procedural step is

neither required nor prohibited.

May not: This action, activity, or procedural step is

prohibited.
1142
-------
Method blank: An aliquot of reagent water that is ^^
treated exactly as a sample including exposure to all
glassware, equipment, solvents, reagents, internal
standards, and surrogates that are used with samples. The
method blank is used to determine if analytes or
interferences are present in the laboratory environment, the
reagents, or the apparatus. :
Minimum level (ML): The level at which the entire
analytical system must give a recognizable signal and
acceptable calibration point for the analyte. It is
equivalent to the concentration of the lowest calibration
standard, assuming that all method-specified sample weights,
volumes, and cleanup procedures have been employed.
MS: Mass spectrometer pr mass spectrometry.
Must: This action, activity, or procedural step is
required. :
OPR: Ongoing precision and recovery standard (OPR); a
laboratory blank spiked with known quantities of analytes.
The OPR is analyzed exactly like a sample. Its purpose is
to assure that the results produced by the laboratory remain
within the limits specified in this method for precision and
recovery. ;
PAR: Precision and recovery standard; secondary
standard that is diluted and spiked to form the IPR and OPR.
Preparation blank: See1 Method blank.
1143
-------
Primary dilution standard': A solution containing the

specified ahalytes that is purchased or prepared from stock

solutions and diluted as needed to prepare calibration

solutions and other solutions.

Quality control check sample (QCS): A sample

containing all or a subset of the analytes at known

concentrations. The QCS is obtained from a source external

to the laboratory or is prepared from a source of standards

different from the source of calibration standards. It is

used to check laboratory performance with test materials

prepared external to the normal preparation process.

Reagent water: Water demonstrated to be free from the

analytes of interest and potentially interfering substances

at the method detection limit for the analyte.

Relative standard deviation (RSD): The standard

deviation times 100 divided by the mean.

RF: Response factor. See Section 10.5.1.

RR: Relative response. See Section 10.4.4.

RSD: See Relative standard deviation.

Should: This action', activity, or procedural step is

suggested but not required.

Stock solution: A solution containing an analyte that

is prepared using a reference material traceable to EPA, the

National Institute of Science and Technology (NIST), or a

source that will attest to the purity and authenticity of

the reference material.

1144
-------
VER: See Calibration verification standard.
1145
-------