For the reasons set out in the preamble, title 40,
Chapter I of the Code of Federal Regulations is amended as
follows:
PART 63--NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR
POLLUTANTS FOR SOURCE CATEGORIES
1. The authority citation for part 63 continues to
read as follows:
Authority: 42 U.S.C. 7401, et seq.
2. Part 63 is amended by adding subpart S to read as
follows:
Subpart S--National Emission Standards for Hazardous Air
Pollutants from the Pulp and Paper Industry
Sec.
63.440 Applicability.
63.441 Definitions.
63.442 [Reserved]
63.443 Standards for the pulping system at kraft, soda, and
semi-chemical processes.
63.444 Standards for the pulping system at sulfite
processes.
63.445 Standards for the bleaching system.
63.446 Standards for kraft pulping process condensates.
63.447 Clean condensate alternative.
63.448-449 [Reserved]
63.450 Standards for enclosures and closed-vent systems.
63.451-452 [Reserved]
63.453 Monitoring Requirements.
63.454 Recordkeeping Requirements.
63.455 Reporting Requirements.
63.456 [Reserved]
63.457 Test methods and procedures.
63.458 Delegation of authority.
63.459 [Reserved]
Table 1 to Subpart S. General Provisions Applicability to
Subpart S
Subpart S--National Emission Standards for Hazardous Air
Pollutants from the Pulp and Paper Industry
63.440 Applicability.
(a) The provisions of this subpart apply to the owner
or operator of processes that produce pulp, paper, or
paperboard; that are located at a plant site that is a major
source as defined in 63.2 of subpart A of this part; and
that use the following processes and materials:
(1) Kraft, soda, sulfite, or semi-chemical pulping
processes using wood; or
(2) Mechanical pulping processes using wood; or
(3) Any process using secondary or non-wood fibers.
(b) The affected source to which the existing source
provisions of this subpart apply is as follows:
(1) For the processes specified in paragraph (a)(1) of
this section, the affected source is the total of all HAP
emission points in the pulping and bleaching systems; or
(2) For the processes specified in paragraphs (a)(2)
or (a)(3) of this section, the affected source is the total
of all HAP emission points in the bleaching system.
(c) The new source provisions of this subpart apply to
the total of all HAP emission points at new or existing
sources as follows:
(1) Each affected source defined in paragraph (b)(1)
of this section that commences construction or
reconstruction after December 17, 1993;
(2) Each pulping system or bleaching system for the
processes specified in paragraph (a)(1) of this section that
commences construction or reconstruction after December 17,
1993;
(3) Each additional pulping or bleaching line at the
processes specified in paragraph (a)(1) of this section,
that commences construction after December 17, 1993;
(4) Each affected source defined in paragraph (b)(2)
of this section that commences construction or
reconstruction after March 8, 1996; or
(5) Each additional bleaching line at the processes
specified in paragraphs (a)(2) or (a)(3) of this section,
that commences construction after March 8, 1996.
(d) Each existing source shall achieve compliance no
later than [insert date 3 years after date published in the
FEDERAL REGISTER], except as provided in paragraphs (d)(1)
through (d)(3) of this section.
(1) Each kraft pulping system shall achieve compliance
with the pulping system provisions of 63.443 for the
equipment listed in 63.443(a)(1)(ii) through (a)(1)(v) as
expeditiously as practicable, but in no event later than
[insert date 8 years after date published in the FEDERAL
REGISTER] and the owners and operators shall establish
dates, update dates, and report the dates for the milestones
specified in 63.455(b).
(2) Each dissolving-grade bleaching system at either
kraft or sulfite pulping mills shall achieve compliance with
the bleach plant provisions of 63.445 of this subpart as
expeditiously as practicable, but in no event later than
3 years after the promulgation of the revised effluent
limitation guidelines and standards under 40 CFR 430.14
through 430.17 and 40 CFR 430.44 through 430.47.
(3) Each bleaching system complying with the Voluntary
Advanced Technology Incentives Program for Effluent
Limitation Guidelines in 40 CFR 430.24, shall comply with
the requirements specified in either paragraph (d)(3)(i) or
(d)(3)(ii) of this section for the effluent limitation
guidelines and standards in 40 CFR 430.24.
(i) Comply with the bleach plant provisions of
63.445 of this subpart as expeditiously as practicable,
but in no event later than [insert date 3 years after date
published in the FEDERAL REGISTER].
(ii) Comply with all of the following:
(A) The owner or operator of a bleaching system shall
comply with the bleach plant provisions of 63.445 of this
subpart as expeditiously as practicable, but in no event
later than [insert date 6 years after date published in the
FEDERAL REGISTER].
(B) The owner or operator of a bleaching system shall
not increase the application rate of chlorine or
hypochlorite in kg of bleaching agent per megagram of ODP,
in the bleaching system above the average daily rates used
over the three months prior to [insert date 60 days after
publication in the FEDERAL REGISTER] until the requirements
of paragraph (d)(3)(ii)(A) of this section are met and
record application rates as specified in 63.454(c).
(C) Owners and operators shall establish dates, update
dates, and report the dates for the milestones specified in
63.455(b).
(e) Each new source, specified as the total of all HAP
emission points for the sources specified in paragraph (c)
of this section, shall achieve compliance upon start-up or
[insert date 60 days after published in the FEDERAL
REGISTER], whichever is later, as provided in 63.6(b) of
subpart A of this part.
(f) Each owner or operator of an affected source with
affected process equipment shared by more than one type of
pulping process, shall comply with the applicable
requirement in this subpart that achieves the maximum degree
of reduction in HAP emissions.
(g) Each owner or operator of an affected source
specified in paragraphs (a) through (c) of this section must
comply with the requirements of subpart A - General
Provisions of this part, as indicated in table 1.
63.441 Definitions.
All terms used in this subpart shall have the meaning
given them in the CAA, in subpart A of this part, and in
this section as follows:
Acid condensate storage tank means any storage tank
containing cooking acid following the sulfur dioxide gas
fortification process.
Black liquor means spent cooking liquor that has been
separated from the pulp produced by the kraft, soda, or
semi-chemical pulping process.
Bleaching means brightening of pulp by the addition of
oxidizing chemicals or reducing chemicals.
Bleaching line means a group of bleaching stages
arranged in series such that bleaching of the pulp
progresses as the pulp moves from one stage to the next.
Bleaching stage means all process equipment associated
with a discrete step of chemical application and removal in
the bleaching process including chemical and steam mixers,
bleaching towers, washers, seal (filtrate) tanks, vacuum
pumps, and any other equipment serving the same function as
those previously listed.
Bleaching system means all process equipment after
high-density pulp storage prior to the first application of
oxidizing chemicals or reducing chemicals following the
pulping system, up to and including the final bleaching
stage.
Boiler means any enclosed combustion device that
extracts useful energy in the form of steam. A boiler is
not considered a thermal oxidizer.
Chip steamer means a vessel used for the purpose of
preheating or pretreating wood chips prior to the digester,
using flash steam from the digester or live steam.
Closed-vent system means a system that is not open to
the atmosphere and is composed of piping, ductwork,
connections, and, if necessary, flow-inducing devices that
transport gas or vapor from an emission point to a control
device.
Combustion device means an individual unit of
equipment, including but not limited to, a thermal oxidizer,
lime kiln, recovery furnace, process heater, or boiler, used
for the thermal oxidation of organic hazardous air pollutant
vapors.
Decker system means all equipment used to thicken the
pulp slurry or reduce its liquid content after the pulp
washing system and prior to high-density pulp storage. The
decker system includes decker vents, filtrate tanks,
associated vacuum pumps, and any other equipment serving the
same function as those previously listed.
Digester system means each continuous digester or each
batch digester used for the chemical treatment of wood or
non-wood fibers. The digester system equipment includes
associated flash tank(s), blow tank(s), chip steamer(s) not
using fresh steam, blow heat recovery accumulator(s), relief
gas condenser(s), prehydrolysis unit(s) preceding the pulp
washing system, and any other equipment serving the same
function as those previously listed. The digester system
includes any of the liquid streams or condensates associated
with batch or continuous digester relief, blow, or flash
steam processes.
Emission point means any part of a stationary source
that emits hazardous air pollutants regulated under this
subpart, including emissions from individual process vents,
stacks, open pieces of process equipment, equipment leaks,
wastewater and condensate collection and treatment system
units, and those emissions that could reasonably be conveyed
through a stack, chimney, or duct where such emissions first
reach the environment.
Evaporator system means all equipment associated with
increasing the solids content and/or concentrating spent
cooking liquor from the pulp washing system including pre-evaporators, multi-effect evaporators, concentrators, and
vacuum systems, as well as associated condensers, hotwells,
and condensate streams, and any other equipment serving the
same function as those previously listed.
Flow indicator means any device that indicates gas or
liquid flow in an enclosed system.
HAP means a hazardous air pollutant as defined in
63.2 of subpart A of this part.
High volume, low concentration or HVLC collection
system means the gas collection and transport system used to
convey gases from the HVLC system to a control device.
High volume, low concentration or HVLC system means the
collection of equipment including the pulp washing, knotter,
screen, decker, and oxygen delignification systems, weak
liquor storage tanks, and any other equipment serving the
same function as those previously listed.
Knotter system means equipment where knots, oversized
material, or pieces of uncooked wood are removed from the
pulp slurry after the digester system and prior to the pulp
washing system. The knotter system equipment includes the
knotter, knot drainer tanks, ancillary tanks, and any other
equipment serving the same function as those previously
listed.
Kraft pulping means a chemical pulping process that
uses a mixture of sodium hydroxide and sodium sulfide as the
cooking liquor.
Lime kiln means an enclosed combustion device used to
calcine lime mud, which consists primarily of calcium
carbonate, into calcium oxide.
Low volume, high concentration or LVHC collection
system means the gas collection and transport system used to
convey gases from the LVHC system to a control device.
Low volume, high concentration or LVHC system means the
collection of equipment including the digester, turpentine
recovery, evaporator, steam stripper systems, and any other
equipment serving the same function as those previously
listed.
Mechanical pulping means a pulping process that only
uses mechanical and thermo-mechanical processes to reduce
wood to a fibrous mass. The mechanical pulping processes
include, but are not limited to, stone groundwood,
pressurized groundwood, refiner mechanical, thermal refiner
mechanical, thermo-mechanical, and tandem thermo-mechanical.
Non-wood pulping means the production of pulp from
fiber sources other than trees. The non-wood fiber sources
include, but are not limited to, bagasse, cereal straw,
cotton, flax straw, hemp, jute, kenaf, and leaf fibers.
Oven-dried pulp or ODP means a pulp sample at zero
percent moisture content by weight. Pulp samples for
applicability or compliance determinations for both the
pulping and bleaching systems shall be unbleached pulp. For
purposes of complying with mass emission limits in this
subpart, megagram of ODP shall be measured to represent the
amount of pulp entering and processed by the equipment
system under the specified mass limit. For equipment that
does not process pulp, megagram of ODP shall be measured to
represent the amount of pulp that was processed to produce
the gas and liquid streams.
Oxygen delignification system means the equipment that
uses oxygen to remove lignin from pulp after high-density
stock storage and prior to the bleaching system. The oxygen
delignification system equipment includes the blow tank,
washers, filtrate tanks, any interstage pulp storage tanks,
and any other equipment serving the same function as those
previously listed.
Primary fuel means the fuel that provides the principal
heat input to the combustion device. To be considered
primary, the fuel must be able to sustain operation of the
combustion device without the addition of other fuels.
Process wastewater treatment system means a collection
of equipment, a process, or specific technique that removes
or destroys the HAP's in a process wastewater stream.
Examples include, but are not limited to, a steam stripping
unit, wastewater thermal oxidizer, or biological treatment
unit.
Pulp washing system means all equipment used to wash
pulp and separate spent cooking chemicals following the
digester system and prior to the bleaching system, oxygen
delignification system, or paper machine system (at
unbleached mills). The pulp washing system equipment
includes vacuum drum washers, diffusion washers, rotary
pressure washers, horizontal belt filters, intermediate
stock chests, and their associated vacuum pumps, filtrate
tanks, foam breakers or tanks, and any other equipment
serving the same function as those previously listed. The
pulp washing system does not include deckers, screens,
knotters, stock chests, or pulp storage tanks following the
last stage of pulp washing.
Pulping line means a group of equipment arranged in
series such that the wood chips are digested and the
resulting pulp progresses through a sequence of steps that
may include knotting, refining, washing, thickening,
blending, storing, oxygen delignification, and any other
equipment serving the same function as those previously
listed.
Pulping process condensates means any HAP-containing
liquid that results from contact of water with organic
compounds in the pulping process. Examples of process
condensates include digester system condensates, turpentine
recovery system condensates, evaporator system condensates,
LVHC system condensates, HVLC system condensates, and any
other condensates from equipment serving the same function
as those previously listed. Liquid streams that are
intended for byproduct recovery are not considered process
condensate streams.
Pulping system means all process equipment, beginning
with the digester system, and up to and including the last
piece of pulp conditioning equipment prior to the bleaching
system, including treatment with ozone, oxygen, or peroxide
before the first application of a chemical bleaching agent
intended to brighten pulp. The pulping system includes
pulping process condensates and can include multiple pulping
lines.
Recovery furnace means an enclosed combustion device
where concentrated spent liquor is burned to recover sodium
and sulfur, produce steam, and dispose of unwanted dissolved
wood components in the liquor.
Screen system means equipment in which oversized
particles are removed from the pulp slurry prior to the
bleaching or papermaking system washed stock storage.
Secondary fiber pulping means a pulping process that
converts a fibrous material, that has previously undergone a
manufacturing process, into pulp stock through the addition
of water and mechanical energy. The mill then uses that
pulp as the raw material in another manufactured product.
These mills may also utilize chemical, heat, and mechanical
processes to remove ink particles from the fiber stock.
Semi-chemical pulping means a pulping process that
combines both chemical and mechanical pulping processes.
The semi-chemical pulping process produces intermediate
yields ranging from 55 to 90 percent.
Soda pulping means a chemical pulping process that uses
sodium hydroxide as the active chemical in the cooking
liquor.
Spent liquor means process liquid generated from the
separation of cooking liquor from pulp by the pulp washing
system containing dissolved organic wood materials and
residual cooking compounds.
Steam stripper system means a column (including
associated stripper feed tanks, condensers, or heat
exchangers) used to remove compounds from wastewater or
condensates using steam. The steam stripper system also
contains all equipment associated with a methanol
rectification process including rectifiers, condensers,
decanters, storage tanks, and any other equipment serving
the same function as those previously listed.
Strong liquor storage tanks means all storage tanks
containing liquor that has been concentrated in preparation
for combustion or oxidation in the recovery process.
Sulfite pulping means a chemical pulping process that
uses a mixture of sulfurous acid and bisulfite ion as the
cooking liquor.
Temperature monitoring device means a piece of
equipment used to monitor temperature and having an accuracy
of ñ1.0 percent of the temperature being monitored expressed
in degrees Celsius or ñ0.5 degrees Celsius (oC), whichever
is greater.
Thermal oxidizer means an enclosed device that destroys
organic compounds by thermal oxidation.
Turpentine recovery system means all equipment
associated with recovering turpentine from digester system
gases including condensers, decanters, storage tanks, and
any other equipment serving the same function as those
previously listed. The turpentine recovery system includes
any liquid streams associated with the turpentine recovery
process such as turpentine decanter underflow. Liquid
streams that are intended for byproduct recovery are not
considered turpentine recovery system condensate streams.
Weak liquor storage tank means any storage tank except
washer filtrate tanks containing spent liquor recovered from
the pulping process and prior to the evaporator system.
63.442 [Reserved]
63.443 Standards for the pulping system at kraft, soda,
and semi-chemical processes.
(a) The owner or operator of each pulping system using
the kraft process subject to the requirements of this
subpart shall control the total HAP emissions from the
following equipment systems, as specified in paragraphs (c)
and (d) of this section.
(1) At existing affected sources, the total HAP
emissions from the following equipment systems shall be
controlled:
(i) Each LVHC system;
(ii) Each knotter or screen system with total HAP mass
emission rates greater than or equal to the rates specified
in paragraphs (a)(1)(ii)(A) or (ii)(B) or the combined rate
specified in paragraph (a)(1)(ii)(C) of this section.
(A) Each knotter system with emissions of
0.05 kilograms or more of total HAP per megagram of ODP
(0.1 pounds per ton).
(B) Each screen system with emissions of
0.10 kilograms or more of total HAP per megagram of ODP
(0.2 pounds per ton).
(C) Each knotter and screen system with emissions of
0.15 kilograms or more of total HAP per megagram of ODP
(0.3 pounds per ton).
(iii) Each pulp washing system;
(iv) Each decker system that:
(A) Uses any process water other than fresh water or
paper machine white water; or
(B) Uses any process water with a total HAP
concentration greater than 400 parts per million by weight;
and
(v) Each oxygen delignification system.
(2) At new affected sources, the total HAP emissions
from the equipment systems listed in paragraphs (a)(1)(i),
(a)(1)(iii), and (a)(1)(v) of this section and the following
equipment systems shall be controlled:
(i) Each knotter system;
(ii) Each screen system;
(iii) Each decker system; and
(iv) Each weak liquor storage tank.
(b) The owner or operator of each pulping system using
a semi-chemical or soda process subject to the requirements
of this subpart shall control the total HAP emissions from
the following equipment systems as specified in
paragraphs (c) and (d) of this section.
(1) At each existing affected sources, the total HAP
emissions from each LVHC system shall be controlled.
(2) At each new affected source, the total HAP
emissions from each LVHC system and each pulp washing system
shall be controlled.
(c) Equipment systems listed in paragraphs (a) and (b)
of this section shall be enclosed and vented into a closed-vent system and routed to a control device that meets the
requirements specified in paragraph (d) of this section.
The enclosures and closed-vent system shall meet the
requirements specified in 63.450.
(d) The control device used to reduce total HAP
emissions from each equipment system listed in
paragraphs (a) and (b) of this section shall:
(1) Reduce total HAP emissions by 98 percent or more
by weight; or
(2) Reduce the total HAP concentration at the outlet
of the thermal oxidizer to 20 parts per million or less by
volume, corrected to 10 percent oxygen on a dry basis; or
(3) Reduce total HAP emissions using a thermal
oxidizer designed and operated at a minimum temperature of
871 oC (1600 oF) and a minimum residence time of
0.75 seconds; or
(4) Reduce total HAP emissions using a boiler, lime
kiln, or recovery furnace by introducing the HAP emission
stream with the primary fuel or into the flame zone.
(e) Periods of excess emissions reported under
63.455 shall not be a violation of 63.443(c) and (d)
provided that the time of excess emissions (excluding
periods of startup, shutdown, or malfunction) divided by the
total process operating time in a semi-annual reporting
period does not exceed the following levels:
(1) One percent for control devices used to reduce the
total HAP emissions from the LVHC system; and
(2) Four percent for control devices used to reduce
the total HAP emissions from the HVLC system; and
(2) Four percent for control devices used to reduce
the total HAP emissions from both the LVHC and HVLC systems.
63.444 Standards for the pulping system at sulfite
processes.
(a) The owner or operator of each sulfite process
subject to the requirements of this subpart shall control
the total HAP emissions from the following equipment systems
as specified in paragraphs (b) and (c) of this section.
(1) At existing sulfite affected sources, the total
HAP emissions from the following equipment systems shall be
controlled:
(i) Each digester system vent;
(ii) Each evaporator system vent; and
(iii) Each pulp washing system.
(2) At new affected sources, the total HAP emissions
from the equipment systems listed in paragraph (a)(1) of
this section and the following equipment shall be
controlled:
(i) Each weak liquor storage tank;
(ii) Each strong liquor storage tank; and
(iii) Each acid condensate storage tank.
(b) Equipment listed in paragraph (a) of this section
shall be enclosed and vented into a closed-vent system and
routed to a control device that meets the requirements
specified in paragraph (c) of this section. The enclosures
and closed-vent system shall meet the requirements specified
in 63.450. Emissions from equipment listed in
paragraph (a) of this section that is not necessary to be
reduced to meet paragraph (c) of this section is not
required to be routed to a control device.
(c) The total HAP emissions from both the equipment
systems listed in paragraph (a) of this section and the
vents, wastewater, and condensate streams from the control
device used to reduce HAP emissions, shall be controlled as
follows.
(1) Each calcium-based or sodium-based sulfite pulping
process shall:
(i) Emit no more than 0.44 kilograms of total HAP or
methanol per megagram (0.89 pounds per ton) of ODP; or
(ii) Remove 92 percent or more by weight of the total
HAP or methanol.
(2) Each magnesium-based or ammonium-based sulfite
pulping process shall:
(i) Emit no more than 1.1 kilograms of total HAP or
methanol per megagram (2.2 pounds per ton) of ODP; or
(ii) Remove 87 percent or more by weight of the total
HAP or methanol.
63.445 Standards for the bleaching system.
(a) Each bleaching system that does not use any
chlorine or chlorinated compounds for bleaching is exempt
from the requirements of this section. Owners or operators
of the following bleaching systems shall meet all the
provisions of this section:
(1) Bleaching systems that use chlorine;
(2) Bleaching systems bleaching pulp from kraft,
sulfite, or soda pulping processes that uses any chlorinated
compounds; or
(3) Bleaching systems bleaching pulp from mechanical
pulping processes using wood or from any process using
secondary or non-wood fibers, that use chlorine dioxide.
(b) The equipment at each bleaching stage, of the
bleaching systems listed in paragraph (a) of this section,
where chlorinated compounds are introduced shall be enclosed
and vented into a closed-vent system and routed to a control
device that meets the requirements specified in
paragraph (c) of this section. The enclosures and closed-vent system shall meet the requirements specified in
63.450.
(c) The control device used to reduce chlorinated HAP
emissions (not including chloroform) from the equipment
specified in paragraph (b) of this section shall:
(1) Reduce the total chlorinated HAP mass in the vent
stream entering the control device by 99 percent or more by
weight;
(2) Achieve a treatment device outlet concentration of
10 parts per million or less by volume of total chlorinated
HAP; or
(3) Achieve a treatment device outlet mass emission
rate of 0.001 kg of total chlorinated HAP mass per megagram
(0.002 pounds per ton) of ODP.
(d) The owner or operator of each bleaching system
subject to paragraph (a)(2) of this section shall comply
with paragraph (d)(1) or (d)(2) of this section to reduce
chloroform air emissions to the atmosphere, except the owner
or operator of each bleaching system complying with extended
compliance under 63.440(d)(3)(ii) shall comply with
paragraph (d)(1) of this section.
(1) Comply with the following applicable effluent
limitation guidelines and standards specified in 40 CFR
part 430:
(i) Dissolving-grade kraft bleaching systems and lines
430.14 through 430.17;
(ii) Paper-grade kraft and soda bleaching systems and
lines, 430.24(a)(1) and (e), and 430.26 (a) and (c);
(iii) Dissolving-grade sulfite bleaching systems and
lines, 430.44 through 430.47; or
(iv) Paper-grade sulfite bleaching systems and lines,
430.54 (a) and (c), and 430.56 (a) and (c).
(2) Use no hypochlorite or chlorine for bleaching in
the bleaching system or line.
63.446 Standards for kraft pulping process condensates.
(a) The requirements of this section apply to owners
or operators of kraft processes subject to the requirements
of this subpart.
(b) The pulping process condensates from the following
equipment systems shall be treated to meet the requirements
specified in paragraphs (c), (d), and (e) of this section:
(1) Each digester system;
(2) Each turpentine recovery system;
(3) Each evaporator stage where weak liquor is
introduced (feed stages) in the evaporator system;
(4) Each HVLC collection system; and
(5) Each LVHC collection system.
(c) One of the following combinations of HAP-containing
pulping process condensates generated, produced, or
associated with the equipment systems listed in
paragraph (b) of this section shall be subject to the
requirements of paragraphs (d) and (e) of this section:
(1) All pulping process condensates from the equipment
systems specified in paragraphs (b)(1) through (b)(5) of
this section.
(2) The combined pulping process condensates from the
equipment systems specified in paragraphs (b)(4) and (b)(5)
of this section, plus pulping process condensate stream(s)
that in total contain at least 65 percent of the total HAP
mass from the pulping process condensates from equipment
systems listed in paragraphs (b)(1) through (b)(3) of this
section.
(3) The pulping process condensates from equipment
systems listed in paragraphs (b)(1) through (b)(5) of this
section that in total contain a total HAP mass of 3.6
kilograms or more of total HAP per megagram (7.2 pounds per
ton) of ODP for mills that do not perform bleaching or 5.5
kilograms or more of total HAP per megagram (11.1 pounds per
ton) of ODP for mills that perform bleaching.
(d) The pulping process condensates from the equipment
systems listed in paragraph (b) of this section shall be
conveyed in a closed collection system that is designed and
operated to meet the requirements specified in
paragraphs (d)(1) and (d)(2) of this section.
(1) Each closed collection system shall meet the
individual drain system requirements specified in 63.960,
63.961, and 63.962 of subpart RR of this part, except for
closed vent systems and control devices shall be designed
and operated in accordance with 63.443(d) and 63.450,
instead of in accordance with 63.693 as specified in
63.962 (a)(3)(ii), (b)(3)(ii)(A), and
(b)(3)(ii)(B)(5)(iii); and
(2) If a condensate tank is used in the closed
collection system, the tank shall meet the following
requirements:
(i) The fixed roof and all openings (e.g., access
hatches, sampling ports, gauge wells) shall be designed and
operated with no detectable leaks as indicated by an
instrument reading of less than 500 parts per million above
background, and vented into a closed-vent system that meets
the requirements in 63.450 and routed to a control device
that meets the requirements in 63.443(d); and
(ii) Each opening shall be maintained in a closed,
sealed position (e.g., covered by a lid that is gasketed and
latched) at all times that the tank contains pulping process
condensates or any HAP removed from a pulping process
condensate stream except when it is necessary to use the
opening for sampling, removal, or for equipment inspection,
maintenance, or repair.
(e) Each pulping process condensate from the equipment
systems listed in paragraph (b) of this section shall be
treated according to one of the following options:
(1) Recycle the pulping process condensate to an
equipment system specified in 63.443(a) meeting the
requirements specified in 63.443(c) and (d); or
(2) Discharge the pulping process condensate below the
liquid surface of a biological treatment system meeting the
requirement specified in paragraph (e)(3) of this section;
or
(3) Treat the pulping process condensates to reduce or
destroy the total HAP's by at least 92 percent or more by
weight; or
(4) At mills that do not perform bleaching, treat the
pulping process condensates to remove 3.3 kilograms or more
of total HAP per megagram (6.6 pounds per ton) of ODP, or
achieve a total HAP concentration of 210 parts per million
or less by weight at the outlet of the control device; or
(5) At mills that perform bleaching, treat the pulping
process condensates to remove 5.1 kilograms or more of total
HAP per megagram (10.2 pounds per ton) of ODP, or achieve a
total HAP concentration of 330 parts per million or less by
weight at the outlet of the control device.
(f) Each HAP removed from a pulping process condensate
stream during treatment and handling under paragraphs (d) or
(e) of this section, except for those treated according to
paragraph (e)(2) of this section, shall be controlled as
specified in 63.443(c) and (d).
(g) For each steam stripper system used to comply with
the requirements specified in paragraph (e)(3) of this
section, periods of excess emissions reported under 63.455
shall not be a violation paragraphs (d), (e), and (f) of
this section provided that the time of excess emissions
(including periods of startup, shutdown, or malfunction)
divided by the total process operating time in a semi-annual
reporting period does not exceed 10 percent.
(h) Each owner or operator of a new or existing
affected source subject to the requirements of this section
shall evaluate all new or modified pulping process
condensates or changes in the annual bleached or non-bleached ODP used to comply with paragraph (i) of this
section, to determine if they meet the applicable
requirements of this section.
(i) For the purposes of meeting the requirements in
paragraphs (c)(2), (e)(4), or (e)(5) of this section at
mills producing both bleached and unbleached pulp products,
owners and operators may meet a prorated mass standard that
is calculated by prorating the applicable mass standards
(kilograms of total HAP per megagram of ODP) for bleached
and unbleached specified in paragraphs (c)(2), (e)(4), or
(e)(5) of this section by the ratio of annual megagrams of
bleached and unbleached ODP.
63.447 Clean condensate alternative.
As an alternative to the requirements specified in
63.443(a)(1)(ii) through (a)(1)(v) for the control of HAP
emissions from pulping systems using the kraft process, an
owner or operator must demonstrate to the satisfaction of
the Administrator, by meeting all the requirements below,
that the total HAP emissions reductions achieved by this
clean condensate alternative technology are equal to or
greater than the total HAP emission reductions that would
have been achieved by compliance with 63.443(a)(1)(ii)
through (a)(1)(v).
(a) For the purposes of this section only the
following additional definitions apply.
(1) Clean condensate alternative affected source means
the total of all HAP emission points in the pulping,
bleaching, causticizing, and papermaking systems (exclusive
of HAP emissions attributable to additives to paper machines
and HAP emission points in the LVHC system).
(2) Causticizing system means all equipment associated
with converting sodium carbonate into active sodium
hydroxide. The equipment includes smelt dissolving tanks,
lime mud washers and storage tanks, white and mud liquor
clarifiers and storage tanks, slakers, slaker grit washers,
lime kilns, green liquor clarifiers and storage tanks, and
dreg washers ending with the white liquor storage tanks
prior to the digester system, and any other equipment
serving the same function as those previously listed.
(3) Papermaking system means all equipment used to
convert pulp into paper, paperboard, or market pulp,
including the stock storage and preparation systems, the
paper or paperboard machines, and the paper machine white
water system, broke recovery systems, and the systems
involved in calendering, drying, on-machine coating,
slitting, winding, and cutting.
(b) Each owner or operator shall install and operate a
clean condensate alternative technology with a continuous
monitoring system to reduce total HAP emissions by treating
and reducing HAP concentrations in the pulping process water
used within the clean condensate alternative affected
source.
(c) Each owner or operator shall calculate HAP
emissions on a kilogram per megagram of ODP basis and
measure HAP emissions according to the appropriate
procedures contained in 63.457.
(d) Each owner or operator shall determine the
baseline HAP emissions for each equipment system and the
total of all equipment systems in the clean condensate
alternative affected source based on the following:
(1) Process and air pollution control equipment
installed and operating on or after December 17, 1993, and
(2) Compliance with the following requirements that
affect the level of HAP emissions from the clean condensate
alternative affected source:
(i) The pulping process condensates requirements in
63.446;
(ii) The applicable effluent limitation guidelines and
standards in 40 CFR part 430, subparts A, B, D, and E; and
(iii) All other applicable requirements of local,
State, or Federal agencies or statutes.
(e) Each owner or operator shall determine the
following HAP emission reductions from the baseline HAP
emissions determined in paragraph (d) of this section for
each equipment system and the total of all equipment systems
in the clean condensate alternative affected source:
(1) The HAP emission reduction occurring by complying
with the requirements of 63.443(a)(1)(ii) through
(a)(1)(v), and
(2) The HAP emissions reduction that occurring by
complying with the clean condensate alternative technology.
(f) For the purposes of all requirements in this
section, each owner or operator may use as an alternative,
individual equipment systems (instead of total of all
equipment systems) within the clean condensate alternative
affected source to determine emissions and reductions to
demonstrate equal or greater than the reductions that would
have been achieved by compliance with 63.443(a)(1)(ii)
through (a)(1)(v).
(g) The initial and updates to the control strategy
report specified in 63.455(b) shall include to the extent
possible the following information:
(1) A detailed description of:
(i) The equipment systems and emission points that
comprise the clean condensate alternative affected source;
(ii) The air pollution control technologies that would
be used to meet the requirements of 63.443(a)(1)(ii)
through (a)(1)(v);
(iii) The clean condensate alternative technology to
be used.
(2) Estimates and basis for the estimates of total HAP
emissions and emissions reductions to fulfill the
requirements paragraphs (d), (e), and (f) of this section.
(h) Each owner or operator shall report to the
Administrator by the applicable compliance date specified in
63.440(d) or (e) the rationale, calculations, test
procedures, and data documentation used to demonstrate
compliance with all the requirements of this section.
63.448-449 [Reserved]
63.450 Standards for enclosures and closed-vent systems.
(a) Each enclosure and closed-vent system specified in
63.443(c), 63.444(b), and 63.445(b) for capturing and
transporting vent streams that contain HAP shall meet the
requirements specified in paragraphs (b) through (d) of this
section.
(b) Each enclosure shall maintain negative pressure at
each enclosure or hood opening as demonstrated by the
procedures specified 63.457(e). Each enclosure or hood
opening closed during the initial performance test specified
in 63.457(a) shall be maintained in the same closed and
sealed position as during the performance test at all times
except when necessary to use the opening for sampling,
inspection, maintenance, or repairs.
(c) Each component of the closed-vent system used to
comply with 63.443(c), 63.444(b), and 63.445(b) that
is operated at positive pressure and located prior to a
control device shall be designed for and operated with no
detectable leaks as indicated by an instrument reading of
less than 500 parts per million by volume above background,
as measured by the procedures specified in 63.457(d).
(d) Each bypass line in the closed-vent system that
could divert vent streams containing HAP to the atmosphere
without meeting the emission limitations in 63.443,
63.444, or 63.445 shall comply with either of the following
requirements:
(1) On each bypass line, the owner or operator shall
install, calibrate, maintain, and operate according to
manufacturer's specifications a flow indicator that provides
a record of the presence of gas stream flow in the bypass
line at least once every 15 minutes. The flow indicator
shall be installed in the bypass line in such a way as to
indicate flow in the bypass line; or
(2) For bypass line valves that are not computer
controlled, the owner or operator shall maintain the bypass
line valve in the closed position with a car seal or a seal
placed on the valve or closure mechanism in such a way that
valve or closure mechanism cannot be opened without breaking
the seal.
63.451-452 [Reserved]
63.453 Monitoring Requirements.
(a) Each owner or operator subject to the standards
specified in 63.443(c) and (d), 63.444(b) and (c),
63.445(b) and (c), 63.446(c), (d), and (e), 63.447(b) or
63.450(d), shall install, calibrate, certify, operate, and
maintain according to the manufacturer's specifications, a
continuous monitoring system (CMS, as defined in 63.2 of
this part) as specified in paragraphs (b) through (m) of
this section, except as allowed in paragraph (m) of this
section. The CMS shall include a continuous recorder.
(b) A CMS shall be operated to measure the temperature
in the firebox or in the ductwork immediately downstream of
the firebox and before any substantial heat exchange occurs
for each thermal oxidizer used to comply with the
requirements of 63.443(d)(1) through (d)(3). Owners and
operators complying with the requirements in 63.443(d)(2)
or (d)(3) shall monitor the parameter specified and for the
temperature and concentration limits specified.
(c) A CMS shall be operated to measure the following
parameters for each gas scrubber used to comply with the
bleaching system requirements of 63.445(c) or the sulfite
pulping system requirements of 63.444(c).
(1) The pH or the oxidation/reduction potential of the
gas scrubber effluent;
(2) The gas scrubber vent gas inlet flow rate; and
(3) The gas scrubber liquid influent flow rate.
(d) As an option to the requirements specified in
paragraph (c) of this section, a CMS shall be operated to
measure the chlorine outlet concentration of each gas
scrubber used to comply with the bleaching system outlet
concentration requirement specified in 63.445(c)(2).
(e) The owner or operator of a bleaching system
complying with 40 CFR 430.24, subpart B, shall monitor the
chlorine and hypochlorite application rates, in kg of
bleaching agent per megagram of ODP, of the bleaching system
during the extended compliance period specified in
63.440(d)(3).
(f) A CMS shall be operated to measure the gas
scrubber parameters specified in paragraphs (c)(1) through
(c)(3) of this section or those site specific parameters
determined according to the procedures specified in
paragraph (n) of this section to comply with the sulfite
pulping system requirements specified in 63.444(c).
(g) A CMS shall be operated to measure the following
parameters for each steam stripper used to comply with the
treatment requirements in 63.446(e)(3), (4), or (5):
(1) The process wastewater feed rate;
(2) The steam feed rate; and
(3) The process wastewater column feed temperature.
(h) As an option to the requirements specified in
paragraph (g) of this section, a CMS shall be operated to
measure the methanol outlet concentration to comply with the
steam stripper outlet concentration requirement specified in
63.446(e)(4) or (e)(5).
(i) A CMS shall be operated to measure the appropriate
parameters determined according to the procedures specified
in paragraph (n) of this section to comply with the
condensate applicability requirements specified in
63.446(c).
(j) Each owner or operator using a biological
treatment system to comply with 63.446(e)(2) shall perform
the following monitoring procedures.
(1) On a daily basis, monitor the following parameters
for each biological treatment unit:
(i) Composite daily sample of outlet soluble BOD5
concentration to monitor for maximum daily and maximum
monthly average;
(ii) Mixed liquor volatile suspended solids;
(iii) Horsepower of aerator unit(s);
(iv) Inlet liquid flow; and
(v) Liquid temperature.
(2) Obtain daily inlet and outlet liquid grab samples
from each biological treatment unit to have HAP data
available to perform quarterly percent reduction tests
specified in paragraph (j)(2)(ii) of this section and the
compliance percent reduction tests specified in
paragraph (p)(1)(i) of this section. Perform the following
procedures with the liquid samples:
(i) Store the samples for 5 days as specified in
63.457(n). The 5 day storage requirement is required
since the soluble BOD5 test requires 5 days to obtain
results. If the results of the soluble BOD5 test are
outside of the range established during the initial
performance test, then the archive sample shall be used to
perform the percent reduction test specified in 63.457(1).
(ii) Perform the percent reduction test procedures
specified in 63.457(l) within 45 days after the beginning
of each quarter as follows.
(A) The percent reduction test performed in the first
quarter (annually) shall be performed for total HAP and the
percent reduction obtained from the test shall be at least
as great as the total HAP reduction specified in
63.446(e)(2).
(B) The remaining quarterly percent reduction tests
shall be performed for methanol and the percent reduction
obtained from the test shall be at least as great as the
methanol reduction determined in the previous first-quarter
test specified in paragraph (j)(2)(ii)(A) of this section.
(C) The parameter values used to calculate the percent
reductions required in paragraphs (j)(2)(ii)(A) and
(j)(2)(ii)(B) of this section shall be parameter values
measured and samples taken in paragraph (j)(1) of this
section.
(k) Each enclosure and closed-vent system used to
comply with 63.450(a) shall comply with the requirements
specified in paragraphs (k)(1) through (k)(6) of this
section.
(1) For each enclosure opening, a visual inspection of
the closure mechanism specified in 63.450(b) shall be
performed at least once every 30 days to ensure the opening
is maintained in the closed position and sealed.
(2) Each closed-vent system required by 63.450(a)
shall be visually inspected every 30 days and at other times
as requested by the Administrator. The visual inspection
shall include inspection of ductwork, piping, enclosures,
and connections to covers for visible evidence of defects.
(3) For positive pressure closed-vent systems or
portions of closed-vent systems, demonstrate no detectable
leaks as specified in 63.450(c) measured initially and
annually by the procedures in 63.457(d).
(4) Demonstrate initially and annually that each
enclosure opening is maintained at negative pressure as
specified in 63.457(e).
(5) The valve or closure mechanism specified in
63.450(d)(2) shall be inspected at least once every 30
days to ensure that the valve is maintained in the closed
position and the emission point gas stream is not diverted
through the bypass line.
(6) If an inspection required by paragraphs (k)(1)
through (k)(5) of this section identifies visible defects in
ductwork, piping, enclosures or connections to covers
required by 63.450, or if an instrument reading of 500
parts per million by volume or greater above background is
measured, or if enclosure openings are not maintained at
negative pressure, then the following corrective actions
shall be taken as soon as practicable.
(i) A first effort to repair or correct the closed-vent system shall be made as soon as practicable but no
later than 5 calendar days after the problem is identified.
(ii) The repair or corrective action shall be
completed no later than 15 calendar days after the problem
is identified.
(l) Each pulping process condensate closed collection
system used to comply with 63.446(d) shall be visually
inspected every 30 days and shall comply with the inspection
and monitoring requirements specified in 63.964 of subpart
RR of this part, except for the closed-vent system and
control device inspection and monitoring requirements
specified in 63.964(a)(2) of subpart RR of this part, the
closed-vent system and the control device shall meet the
requirements specified in paragraphs (a) and (k) of this
section.
(m) Each owner or operator using a control device,
technique or an alternative parameter other than those
specified in paragraphs (b) through (l) of this section
shall install a CMS and establish appropriate operating
parameters to be monitored that demonstrate, to the
Administrator's satisfaction, continuous compliance with the
applicable control requirements.
(n) To establish or reestablish, the value for each
operating parameter required to be monitored under
paragraphs (b) through (j), (l), and (m) of this section or
to establish appropriate parameters for paragraphs (f), (i),
and (m) of this section, each owner or operator shall use
the following procedures:
(1) During the initial performance test required in
63.457(a) or any subsequent performance test, continuously
record the operating parameter;
(2) Determinations shall be based on the control
performance and parameter data monitored during the
performance test, supplemented if necessary by engineering
assessments and the manufacturer's recommendations;
(3) The owner or operator shall provide for the
Administrator's approval the rationale for selecting the
monitoring parameters necessary to comply with paragraphs
(f), (i), and (m) of this section; and
(4) Provide for the Administrator's approval the
rationale for the selected operating parameter value, and
monitoring frequency, and averaging time. Include all data
and calculations used to develop the value and a description
of why the value, monitoring frequency, and averaging time
demonstrate continuous compliance with the applicable
emission standard.
(o) Each owner or operator of a control device subject
to the monitoring provisions of this section shall operate
the control device in a manner consistent with the minimum
or maximum (as appropriate) operating parameter value or
procedure required to be monitored under paragraphs (a)
through (n) of this section and established under this
subpart. Except as provided in paragraph (p) of this
section, 63.443 (e), or 63.446 (g), operation of the
control device below minimum operating parameter values or
above maximum operating parameter values established under
this subpart or failure to perform procedures required by
this subpart shall constitute a violation of the applicable
emission standard of this subpart and be reported as a
period of excess emissions.
(p) Each owner or operator of a biological treatment
system complying with paragraph (j) of this section shall
perform all the following requirements when the monitoring
parameters specified in paragraphs (j)(1)(i) through (j)(1)
(iii) of this section are below minimum operating parameter
values or above maximum operating parameter values
established in paragraph (n) of this section.
(1) The following shall occur and be recorded as soon
as practical:
(i) Determine compliance with 63.446(e)(2) using the
percent reduction test procedures specified in 63.457(l)
and the monitoring data specified in paragraph (j)(1) of
this section that coincide with the time period of the
parameter excursion;
(ii) Steps shall be taken to repair or adjust the
operation of the process to end the parameter excursion
period; and
(iii) Steps shall be taken to minimize total HAP
emissions to the atmosphere during the parameter excursion
period.
(2) A parameter excursion is not a violation of the
applicable emission standard if the percent reduction test
specified in paragraph (p)(1)(i) of this section
demonstrates compliance with 63.446(e)(2), and no
maintenance or changes have been made to the process or
control device after the beginning of a parameter excursion
that would influence the results of the determination.
63.454 Recordkeeping Requirements.
(a) The owner or operator of each affected source
subject to the requirements of this subpart shall comply
with the recordkeeping requirements of 63.10 of subpart A
of this part, as shown in table 1, and the requirements
specified in paragraphs (b) through (d) of this section for
the monitoring parameters specified in 63.453.
(b) For each applicable enclosure opening, closed-vent
system, and closed collection system, the owner or operator
shall prepare and maintain a site-specific inspection plan
including a drawing or schematic of the components of
applicable affected equipment and shall record the following
information for each inspection:
(1) Date of inspection;
(2) The equipment type and identification;
(3) Results of negative pressure tests for enclosures;
(4) Results of leak detection tests;
(5) The nature of the defect or leak and the method of
detection (i.e., visual inspection or instrument detection);
(6) The date the defect or leak was detected and the
date of each attempt to repair the defect or leak;
(7) Repair methods applied in each attempt to repair
the defect or leak;
(8) The reason for the delay if the defect or leak is
not repaired within 15 days after discovery;
(9) The expected date of successful repair of the
defect or leak if the repair is not completed within
15 days;
(10) The date of successful repair of the defect or
leak;
(11) The position and duration of opening of bypass
line valves and the condition of any valve seals; and
(12) The duration of the use of bypass valves on
computer controlled valves.
(c) The owner or operator of a bleaching system
complying paragraph 63.440(d)(3)(ii)(B) shall record the
daily average chlorine and hypochlorite application rates,
in kg of bleaching agent per megagram of ODP, of the
bleaching system until the requirements specified in
63.440(d)(3)(ii)(A) are met.
(d) The owner or operator shall record the CMS
parameters specified in 63.453 and meet the requirements
specified in paragraph (a) of this section for any new
affected process equipment or pulping process condensate
stream that becomes subject to the standards in this subpart
due to a process change or modification.
63.455 Reporting Requirements.
(a) Each owner or operator of a source subject to this
subpart shall comply with the reporting requirements of
subpart A of this part as specified in table 1 and all the
following requirements in this section. The initial
notification report specified under 63.9(b)(2) of
subpart A of this part shall be submitted by [insert date
1 year after date published in the FEDERAL REGISTER].
(b) Each owner or operator of a kraft pulping system
specified in 63.440(d)(1) or a bleaching system specified
in 63.440(d)(3)(ii) shall submit, with the initial
notification report specified under 63.9(b)(2) of
subpart A of this part and paragraph (a) of this section and
update every two years thereafter, a non-binding control
strategy report containing, at a minimum, the information
specified in paragraphs (b)(1) through (b)(3) of this
section in addition to the information required in
63.9(b)(2) of subpart A of this part.
(1) A description of the emission controls or process
modifications selected for compliance with the control
requirements in this standard.
(2) A compliance schedule, including the dates by
which each step toward compliance will be reached for each
emission point or sets of emission points. At a minimum,
the list of dates shall include:
(i) The date by which the major study(s) for
determining the compliance strategy will be completed;
(ii) The date by which contracts for emission controls
or process modifications will be awarded, or the date by
which orders will be issued for the purchase of major
components to accomplish emission controls or process
changes;
(iii) The date by which on-site construction,
installation of emission control equipment, or a process
change is to be initiated;
(iv) The date by which on-site construction,
installation of emissions control equipment, or a process
change is to be completed;
(v) The date by which final compliance is to be
achieved;
(vi) For compliance with paragraph 63.440(d)(3)(ii),
the tentative dates by which compliance with effluent
limitation guidelines and standards intermediate pollutant
load effluent reductions and as available, all the dates for
the best available technology's milestones reported in the
National Pollutant Discharge Elimination System authorized
under section 402 of the Clean Water Act and for the best
professional milestones in the Voluntary Advanced Technology
Incentives Program under 40 CFR 430.24 (b)(2); and
(vii) The date by which the final compliance tests
will be performed.
(3) Until compliance is achieved, revisions or updates
shall be made to the control strategy report required by
paragraph (b) of this section indicating the progress made
towards completing the installation of the emission controls
or process modifications during the 2-year period.
(c) The owner or operator of each bleaching system
complying with 63.440(d)(3)(ii)(B) shall certify in the
report specified under 63.10(e)(3) of subpart A of this
part that the daily application rates of chlorine and
hypochlorite for that bleaching system have not increased as
specified in 63.440(d)(3)(ii)(B) until the requirements of
63.440(d)(3)(ii)(A) are met.
(d) The owner or operator shall meet the requirements
specified in paragraph (a) of this section upon startup of
any new affected process equipment or pulping process
condensate stream that becomes subject to the standards of
this subpart due to a process change or modification.
63.456 [Reserved]
63.457 Test methods and procedures.
(a) Initial performance test. An initial performance
test is required for all emission sources subject to the
limitations in 63.443, 63.444, 63.445, 63.446, and
63.447, except those controlled by a combustion device that
is designed and operated as specified in 63.443(d)(3) or
(d)(4).
(b) Vent sampling port locations and gas stream
properties. For purposes of selecting vent sampling port
locations and determining vent gas stream properties,
required in 63.443, 63.444, 63.445, and 63.447, each
owner or operator shall comply with the applicable
procedures in paragraphs (b)(1) through (b)(6) of this
section.
(1) Method 1 or 1A of part 60, appendix A, as
appropriate, shall be used for selection of the sampling
site as follows:
(i) To sample for vent gas concentrations and
volumetric flow rates, the sampling site shall be located
prior to dilution of the vent gas stream and prior to
release to the atmosphere;
(ii) For determining compliance with percent reduction
requirements, sampling sites shall be located prior to the
inlet of the control device and at the outlet of the control
device; measurements shall be performed simultaneously at
the two sampling sites; and
(iii) For determining compliance with concentration
limits or mass emission rate limits, the sampling site shall
be located at the outlet of the control device.
(2) No traverse site selection method is needed for
vents smaller than 0.10 meter (4.0 inches) in diameter.
(3) The vent gas volumetric flow rate shall be
determined using Method 2, 2A, 2C, or 2D of part 60,
appendix A, as appropriate.
(4) The moisture content of the vent gas shall be
measured using Method 4 of part 60, appendix A.
(5) To determine vent gas concentrations, the owner or
operator shall collect a minimum of three samples that are
representative of normal conditions and average the
resulting pollutant concentrations using the following
procedures.
(i) Method 308 in Appendix A of this part shall be
used to determine the methanol concentration.
(ii) Except for the modifications specified in
paragraphs (b)(5)(ii)(A) through (b)(5)(ii)(K) of this
section, Method 26A of part 60, appendix A shall be used to
determine chlorine concentration in the vent stream.
(A) Probe/Sampling Line. A separate probe is not
required. The sampling line shall be an appropriate length
of 0.64 cm (0.25 in) OD Teflon tubing. The sample inlet
end of the sampling line shall be inserted into the stack in
such a way as to not entrain liquid condensation from the
vent gases. The other end shall be connected to the
impingers. The length of the tubing may vary from one
sampling site to another, but shall be as short as possible
in each situation. If sampling is conducted in sunlight,
opaque tubing shall be used. Alternatively, if transparent
tubing is used, it shall be covered with opaque tape.
(B) Impinger Train. Three 30 milliliter (ml) capacity
midget impingers shall be connected in series to the
sampling line. The impingers shall have regular tapered
stems. Silica gel shall be placed in the third impinger as
a desiccant. All impinger train connectors shall be glass
and/or Teflon .
(C) Critical Orifice. The critical orifice shall have
a flow rate of 200 to 250 ml/min and shall be followed by a
vacuum pump capable of providing a vacuum of 640 millimeters
of mercury (mm Hg). A 45 millimeter diameter in-line
Teflon 0.8 micrometer filter shall follow the impingers to
project the critical orifice and vacuum pump.
(D) The following are necessary for the analysis
apparatus:
(1) Wash bottle filled with deionized water;
(2) 25 or 50 ml graduated burette and stand;
(3) Magnetic stirring apparatus and stir bar;
(4) Calibrated pH Meter;
(5) 150-250 ml beaker or flask; and
(6) A 5 ml pipette.
(E) The procedures listed in
paragraphs (b)(5)(ii)(E)(1) through (b)(5)(ii)(E)(7) of this
section shall be used to prepare the reagents.
(1) To prepare the 1 molarity (M) potassium dihydrogen
phosphate solution, dissolve 13.61 grams (g) of potassium
dihydrogen phosphate in water and dilute to 100 ml.
(2) To prepare the 1 M sodium hydroxide solution
(NaOH), dissolve 4.0 g of sodium hydroxide in water and
dilute to 100 ml.
(3) To prepare the buffered 2 percent potassium iodide
solution, dissolve 20 g of potassium iodide in 900 ml water.
Add 50 ml of the 1 M potassium dihydrogen phosphate solution
and 30 ml of the 1 M sodium hydroxide solution. While
stirring solution, measure the pH of solution
electrometrically and add the 1 M sodium hydroxide solution
to bring pH to between 6.95 and 7.05.
(4) To prepare the 0.1 normality (N) sodium
thiosulfate solution, dissolve 25 g of sodium thiosulfate,
pentahydrate, in 800 ml of freshly boiled and cooled
distilled water in a 1-liter volumetric flask. Dilute to
volume. To prepare the 0.01 N sodium thiosulfate solution,
add 10.0 ml standardized 0.1 N sodium thiosulfate solution
to a 100 ml volumetric flask, and dilute to volume with
water.
(5) To standardize the 0.1 N sodium thiosulfate
solution, dissolve 3.249 g of anhydrous potassium bi-iodate,
primary standard quality, or 3.567 g potassium iodate dried
at 103 +/- 2 degrees Centigrade for 1 hour, in distilled
water and dilute to 1000 ml to yield a 0.1000 N solution.
Store in a glass-stoppered bottle. To 80 ml distilled
water, add, with constant stirring, 1 ml concentrated
sulfuric acid, 10.00 ml 0.1000 N anhydrous potassium bi-iodate, and 1 g potassium iodide. Titrate immediately with
0.1 n sodium thiosulfate titrant until the yellow color of
the liberated iodine is almost discharged. Add 1 ml starch
indicator solution and continue titrating until the blue
color disappears. The normality of the sodium thiosulfate
solution is inversely proportional to the ml of sodium
thiosulfate solution consumed:
(6) To prepare the starch indicator solution, add a
small amount of cold water to 5 g starch and grind in a
mortar to obtain a thin paste. Pour paste into 1 L of
boiling distilled water, stir, and let settle overnight.
Use clear supernate for starch indicator solution.
(7) To prepare the 10 percent sulfuric acid solution,
add 10 ml of concentrated sulfuric acid to 80 ml water in an
100 ml volumetric flask. Dilute to volume.
(F) The procedures specified in paragraphs
(b)(5)(ii)(F)(1) through (b)(5)(ii)(F)(5) of this section
shall be used to perform the sampling.
(1) Preparation of Collection Train. Measure 20 ml
buffered potassium iodide solution into each of the first
two impingers and connect probe, impingers, filter, critical
orifice, and pump. The sampling line and the impingers
shall be shielded from sunlight.
(2) Leak and Flow Check Procedure. Plug sampling line
inlet tip and turn on pump. If a flow of bubbles is visible
in either of the liquid impingers, tighten fittings and
adjust connections and impingers. A leakage rate not in
excess of 2 percent of the sampling rate is acceptable.
Carefully remove the plug from the end of the probe. Check
the flow rate at the probe inlet with a bubble tube flow
meter. The flow should be comparable or slightly less than
the flow rate of the critical orifice with the impingers
off-line. Record the flow and turn off the pump.
(3) Sample Collection. Insert the sampling line into
the stack and secure it with the tip slightly lower than the
port height. Start the pump, recording the time. End the
sampling after 60 minutes, or after yellow color is
observed in the second in-line impinger. Record time and
remove the tubing from the vent. Recheck flow rate at
sampling line inlet and turn off pump. If the flow rate has
changed significantly, redo sampling with fresh capture
solution. A slight variation (less than 5 percent) in flow
may be averaged. With the inlet end of the line elevated
above the impingers, add about 5 ml water into the inlet tip
to rinse the line into the first impinger.
(4) Sample Analysis. Fill the burette with 0.01 N
sodium thiosulfate solution to the zero mark. Combine the
contents of the impingers in the beaker or flask. Stir the
solution and titrate with thiosulfate until the solution is
colorless. Record the volume of the first endpoint (TN,
ml). Add 5 ml of the 10 percent sulfuric acid solution, and
continue the titration until the contents of the flask are
again colorless. Record the total volume of titrant
required to go through the first and to the second endpoint
(TA, ml). If the volume of neutral titer is less than
0.5 ml, repeat the testing for a longer period of time. It
is important that sufficient lighting be present to clearly
see the endpoints, which are determined when the solution
turns from pale yellow to colorless. A lighted stirring
plate and a white background are useful for this purpose.
(5) Interferences. Known interfering agents of this
method are sulfur dioxide and hydrogen peroxide. Sulfur
dioxide, which is used to reduce oxidant residuals in some
bleaching systems, reduces formed iodine to iodide in the
capture solution. It is therefore a negative interference
for chlorine, and in some cases could result in erroneous
negative chlorine concentrations. Any agent capable of
reducing iodine to iodide could interfere in this manner. A
chromium trioxide impregnated filter will capture sulfur
dioxide and pass chlorine and chlorine dioxide. Hydrogen
peroxide, which is commonly used as a bleaching agent in
modern bleaching systems, reacts with iodide to form iodine
and thus can cause a positive interference in the chlorine
measurement. Due to the chemistry involved, the precision
of the chlorine analysis will decrease as the ratio of
chlorine dioxide to chlorine increases. Slightly negative
calculated concentrations of chlorine may occur when
sampling a vent gas with high concentrations of chlorine
dioxide and very low concentrations of chlorine.
(G) The following calculation shall be performed to
determine the corrected sampling flow rate:
where:
SC = Corrected (dry standard) sampling flow rate,
liters per minute;
SU = Uncorrected sampling flow rate, L/min;
BP = Barometric pressure at time of sampling;
PW = Saturated partial pressure of water vapor, mm
Hg at temperature; and
t = Ambient temperature, øC.
(H) The following calculation shall be performed to
determine the moles of chlorine in the sample:
where:
TN = Volume neutral titer, ml;
TA = Volume acid titer (total), ml; and
NThio = Normality of sodium thiosulfate titrant.
(I) The following calculation shall be performed to
determine the concentration of chlorine in the sample:
where:
SC = Corrected (dry standard) sampling flow rate,
liters per minute;
tS = Time sampled, minutes;
TN = Volume neutral titer, ml;
TA = Volume acid titer (total), ml; and
NThio = Normality of sodium thiosulfate titrant.
(J) The following calculation shall be performed to
determine the moles of chlorine dioxide in the sample:
where:
TA = Volume acid titer (total), ml;
TN = Volume neutral titer, ml; and
NThio = Normality of sodium thiosulfate titrant.
(K) The following calculation shall be performed to
determine the concentration of chlorine dioxide in the
sample:
where:
SC = Corrected (dry standard) sampling flow
rate, liters per minute;
tS = Time sampled, minutes;
TA = Volume acid titer (total), ml;
TN = Volume neutral titer, ml; and
NThio = Normality of sodium thiosulfate titrant.
(iii) Any other method that measures the total HAP or
methanol concentration that has been demonstrated to the
Administrator's satisfaction.
(6) The minimum sampling time for each of the three
runs per method shall be 1 hour in which either an
integrated sample or four grab samples shall be taken. If
grab sampling is used, then the samples shall be taken at
approximately equal intervals in time, such as 15 minute
intervals during the run.
(c) Liquid sampling locations and properties. For
purposes of selecting liquid sampling locations and for
determining properties of liquid streams such as
wastewaters, process waters, and condensates required in
63.444, 63.446, and 63.447, the owner or operator shall
comply with the following procedures:
(1) Samples shall be collected using the sampling
procedures specified in Method 305 of part 60, appendix A;
(i) Where feasible, samples shall be taken from an
enclosed pipe prior to the liquid stream being exposed to
the atmosphere; and
(ii) When sampling from an enclosed pipe is not
feasible, samples shall be collected in a manner to minimize
exposure of the sample to the atmosphere and loss of HAP
compounds prior to sampling.
(2) The volumetric flow rate of the entering and
exiting liquid streams shall be determined using the inlet
and outlet flow meters or other methods demonstrated to the
Administrator's satisfaction. The volumetric flow rate
measurements to determine actual mass removal shall be taken
at the same time as the concentration measurements;
(3) To determine liquid stream total HAP or methanol
concentrations, the owner or operator shall collect a
minimum of three samples that are representative of normal
conditions and average the resulting pollutant
concentrations using one of the following:
(i) Method 305 in Appendix A of this part, adjusted
using the following equation:
where:
_
C = Pollutant concentration for the liquid
stream, parts per million by weight.
Ci = Measured concentration of pollutant i in the
liquid stream sample determined using
Method 305, parts per million by weight.
fmi = Pollutant-specific constant that adjusts
concentration measured by Method 305 to
actual liquid concentration; the fm for
methanol is 0.85. Additional pollutant fm
values can be found in table 34, subpart G of
this part.
n = Number of individual pollutants, i, summed to
calculate total HAP.
(ii) Any other method that measures total HAP
concentration that has been demonstrated to the
Administrator's satisfaction.
(4) To determine soluble BOD5 in the effluent stream
from a biological treatment unit used to comply with
63.446(e)(2) and 63.453(j), the owner or operator shall
use Method 405.1, of part 136, with the following
modifications:
(i) Filter the sample through the filter paper, into
Erlenmeyer flask by applying a vacuum to the flask sidearm.
Minimize the time for which vacuum is applied to prevent
stripping of volatile organics from the sample. Replace
filter paper as often as needed in order to maintain filter
times of less than approximately 30 seconds per filter
paper. No rinsing of sample container or filter bowl into
the Erlenmeyer flask is allowed.
(ii) Perform Method 405.1 on the filtrate obtained in
paragraph (c)(4) of this section. Dilution water shall be
seeded with 1 milliliter of final effluent per liter of
dilution water. Dilution ratios may require adjustment to
reflect the lower oxygen demand of the filtered sample in
comparison to the total BOD5. Three BOD bottles and
different dilutions shall be used for each sample.
(d) Detectable leak procedures. To measure detectable
leaks for closed-vent systems as specified in 63.450 or
for pulping process wastewater collection systems as
specified in 63.446(d)(2)(i), the owner or operator shall
comply with the following:
(1) Method 21, of part 60, appendix A; and
(2) The instrument specified in Method 21 shall be
calibrated before use according to the procedures specified
in Method 21 on each day that leak checks are performed.
The following calibration gases shall be used:
(i) Zero air (less than 10 parts per million by volume
of hydrocarbon in air); and
(ii) A mixture of methane or n-hexane and air at a
concentration of approximately, but less than, 10,000 parts
per million by volume methane or n-hexane.
(e) Negative pressure procedures. To demonstrate
negative pressure at process equipment enclosure openings as
specified in 63.450(b), the owner or operator shall use
one of the following procedures:
(1) An anemometer to demonstrate flow into the
enclosure opening;
(2) Measure the static pressure across the opening;
(3) Smoke tubes to demonstrate flow into the enclosure
opening; or
(4) Any other industrial ventilation test method
demonstrated to the Administrator's satisfaction.
(f) HAP concentration measurements. For purposes of
complying with the requirements in 63.443, 63.444, and
63.447, the owner or operator shall measure the total HAP
concentration as one of the following:
(1) As the sum of all individual HAP's; or
(2) As methanol.
(g) Condensate HAP concentration measurement. For
purposes of complying with the kraft pulping condensate
requirements in 63.446, the owner or operator shall
measure the total HAP concentration as methanol except for
the purposes of complying with the initial performance test
specified in 63.457(a) for 63.446(e)(2) and as specified
in 63.453 (j)(2)(ii).
(h) Bleaching HAP concentration measurement. For
purposes of complying with the bleaching system requirements
in 63.445, the owner or operator shall measure the total
HAP concentration as the sum of all individual chlorinated
HAP's or as chlorine.
(i) Vent gas stream calculations. To demonstrate
compliance with the mass emission rate, mass emission rate
per megagram of ODP, and percent reduction requirements for
vent gas streams specified in 63.443, 63.444, 63.445, and
63.447, the owner or operator shall use the following:
(1) The total HAP mass emission rate shall be
calculated using the following equation:
where:
E = Mass emission rate of total HAP from the
sampled vent, kilograms per hour.
K2 = Constant, 2.494 x 10-6 (parts per million by
volume)-1 (gram-mole per standard cubic
meter) (kilogram/gram) (minutes/hour), where
standard temperature for (gram-mole per
standard cubic meter) is 20 oC.
Cj = Concentration on a dry basis of pollutant j
in parts per million by volume as measured by
the test methods specified in paragraph (b)
of this section.
Mj = Molecular weight of pollutant j, gram/gram-mole.
Qs = Vent gas stream flow rate (dry standard cubic
meter per minute) at a temperature of 20 oC
as indicated in paragraph (b) of this
section.
n = Number of individual pollutants, i, summed to
calculate total HAP.
(2) The total HAP mass emission rate per megagram of
ODP shall be calculated using the following equation:
where:
F = Mass emission rate of total HAP from the
sampled vent, in kilograms per megagram of
ODP.
E = Mass emission rate of total HAP from the
sampled vent, in kilograms per hour
determined as specified in paragraph (i)(1)
of this section.
P = The production rate of pulp during the
sampling period, in megagrams of ODP per
hour.
(3) The total HAP percent reduction shall be
calculated using the following equation:
where:
R = Efficiency of control device, percent.
Ei = Inlet mass emission rate of total HAP from
the sampled vent, in kilograms of pollutant
per hour, determined as specified in
paragraph (i)(1) of this section.
Eo = Outlet mass emission rate of total HAP from
the sampled vent, in kilograms of pollutant
per hour, determined as specified in
paragraph (i)(1) of this section.
(j) Liquid stream calculations. To demonstrate
compliance with the mass flow rate, mass per megagram of
ODP, and percent reduction requirements for liquid streams
specified in 63.446, the owner or operator shall use the
following:
(1) The mass flow rates of total HAP or methanol
entering and exiting the treatment process shall be
calculated using the following equations:
where:
Eb = Mass flow rate of total HAP or methanol in
the liquid stream entering the treatment
process, kilograms per hour.
Ea = Mass flow rate of total HAP or methanol in
the liquid exiting the treatment process,
kilograms per hour.
K = Density of the liquid stream, kilograms per
cubic meter.
Vbi = Volumetric flow rate of liquid stream
entering the treatment process during each
run i, cubic meters per hour, determined as
specified in paragraph (c) of this section.
Vai = Volumetric flow rate of liquid stream exiting
the treatment process during each run i,
cubic meters per hour, determined as
specified in paragraph (c) of this section.
Cbi = Concentration of total HAP or methanol in the
stream entering the treatment process during
each run i, parts per million by weight,
determined as specified in paragraph (c) of
this section.
Cai = Concentration of total HAP or methanol in the
stream exiting the treatment process during
each run i, parts per million by weight,
determined as specified in paragraph (c) of
this section.
n = Number of runs.
(2) The mass of total HAP or methanol per megagram ODP
shall be calculated using the following equation:
where:
F = Mass loading of total HAP or methanol in the
sample, in kilograms per megagram of ODP.
Ea = Mass flow rate of total HAP or methanol in
the wastewater stream in kilograms per hour
as determined using the procedures in
paragraph (j)(1) of this section.
P = The production rate of pulp during the
sampling period in megagrams of ODP per hour.
(3) The percent reduction of total HAP across the
applicable treatment process shall be calculated using the
following equation:
where:
R = Control efficiency of the treatment process,
percent.
Eb = Mass flow rate of total HAP in the stream
entering the treatment process, kilograms per
hour, as determined in paragraph (j)(1) of
this section.
Ea = Mass flow rate of total HAP in the stream
exiting the treatment process, kilograms per
hour, as determined in paragraph (j)(1) of
this section.
(4) Compounds that meet the requirements specified in
paragraphs (j)(4)(i) or (4)(ii) of this section are not
required to be included in the mass flow rate, mass per
megagram of ODP, or the mass percent reduction
determinations.
(i) Compounds with concentrations at the point of
determination that are below 1 part per million by weight;
or
(ii) Compounds with concentrations at the point of
determination that are below the lower detection limit where
the lower detection limit is greater than 1 part per million
by weight.
(k) Oxygen concentration correction procedures. To
demonstrate compliance with the total HAP concentration
limit of 20 ppmv in 63.443(d)(2), the concentration
measured using the methods specified in paragraph (b)(5) of
this section shall be corrected to 10 percent oxygen using
the following procedures:
(1) The emission rate correction factor and excess air
integrated sampling and analysis procedures of Methods 3A or
3B of part 60, appendix A shall be used to determine the
oxygen concentration. The samples shall be taken at the
same time that the HAP samples are taken.
(2) The concentration corrected to 10 percent oxygen
shall be computed using the following equation:
where:
Cc = Concentration of total HAP corrected to
10 percent oxygen, dry basis, parts per
million by volume.
Cm = Concentration of total HAP dry basis,
parts per million by volume, as
specified in paragraph (b) of this
section.
%02d = Concentration of oxygen, dry basis,
percent by volume.
(l) Biological treatment system percent reduction
calculation. To determine compliance with an open biological
treatment system option specified in 63.446(e)(2) and the
monitoring requirements specified in 63.453(j)(2), the
percent reduction due to destruction in the biological
treatment system shall be calculated using the following
equation:
where:
R = Destruction of total HAP or methanol in the
biological treatment process, percent.
fbio = The fraction of total HAP or methanol removed
in the biological treatment system. The
site-specific biorate constants shall be
determined using the procedures specified and
as limited in Appendix C of part 63.
(m) Condensate segregation procedures. The following
procedures shall be used to demonstrate compliance with the
condensate segregation requirements specified in
63.446(c).
(1) To demonstrate compliance with the percent mass
requirements specified in 63.446(c)(1), the procedures
specified in paragraphs (m)(1)(i) through (1)(iii) of this
section shall be performed.
(i) Determine the total HAP mass of all condensates
from each equipment system listed in 63.446(b)(1) through
(b)(3) using the procedures specified in paragraphs (c) and
(j) of this section.
(ii) Multiply the total HAP mass determine in
paragraph (m)(1)(i) of this section by 0.65 to determine the
target HAP mass for the high-HAP fraction condensate stream
or streams.
(iii) Compliance with the segregation requirements
specified in 63.446(c)(1) is demonstrated if the
condensate stream or streams from each equipment system
listed in 63.446(b)(1) through (b)(3) being treated as
specified in 63.446(e) contain at least as much total HAP
mass as the target total HAP mass determined in paragraph
(m)(1)(ii) of this section.
(2) To demonstrate compliance with the percent mass
requirements specified in 63.446(c)(2), the procedures
specified in paragraphs (m)(2)(i) through (2)(ii) of this
section shall be performed.
(i) Determine the total HAP mass contained in the
high-HAP fraction condensates from each equipment system
listed in 63.446(b)(1) through (b)(3) and the total
condensates streams from the equipment systems listed in
63.446(b)(4) and (b)(5), using the procedures specified in
paragraphs (c) and (j) of this section.
(ii) Compliance with the segregation requirements
specified in 63.446(c)(2) is demonstrated if the total HAP
mass determined in paragraph (m)(2)(i) of this section is
equal to or greater than the appropriate mass requirements
specified in 63.446(c)(2).
(n) Biological treatment system monitoring sampling
storage. The inlet and outlet grab samples required to be
collected in 63.453(j)(2) shall be stored at 4o C (40o F)
to minimize the biodegradation of the organic compounds in
the samples.
63.458 Delegation of authority.
(a) In delegating implementation and enforcement
authority to a State under section 112(d) of the CAA, the
authorities contained in paragraph (b) of this section shall
be retained by the Administrator and not transferred to a
State.
(b) Authorities which will not be delegated to States:
63.6(g) - Use of an alternative nonopacity emission
standard;
63.453(m) - Use of an alternative monitoring
parameter;
63.457(b)(5)(iii) - Use of an alternative test method
for total HAP or methanol in vents; and
63.457(c)(3)(ii) - Use of an alternative test method
for total HAP or methanol in wastewater.
63.459 [Reserved]
TABLE 1 TO SUBPART S. GENERAL PROVISIONS APPLICABILITY TO
SUBPART Sa
Reference
Applies to
Subpart S
Comment
63.1(a)(1)- (3)
Yes
63.1(a)(4)
Yes
Subpart S (this table)
specifies applicability of
each paragraph in subpart A
to subpart S
63.1(a)(5)
No
Section reserved
63.1(a)(6)-(8)
Yes
63.1(a)(9)
No
Section reserved
63.1(a)(10)
No
Subpart S and other
cross-referenced subparts
specify calendar or
operating day
63.1(a)(11)-(14)
Yes
63.1(b)(1)
No
Subpart S specifies its own
applicability
63.1(b)(2)-(3)
Yes
63.1(c)(1)-(2)
Yes
63.1(c)(3)
No
Section reserved
63.1(c)(4)-(5)
Yes
63.1(d)
No
Section reserved
63.1(e)
Yes
63.2
Yes
63.3
Yes
63.4(a)(1)-
63.4(a)(3)
Yes
63.4(a)(4)
No
Section reserved
63.4(a)(5)
Yes
63.4(b)
Yes
63.4(c)
Yes
63.5(a)
Yes
63.5(b)(1)
Yes
63.5(b)(2)
No
Section reserved
63.5(b)(3)
Yes
63.5(b)(4)-(6)
Yes
63.5(c)
No
Section reserved
63.5(d)
Yes
63.5(e)
Yes
63.5(f)
Yes
63.6(a)
Yes
63.6(b)
No
Subpart S specifies
compliance dates for
sources subject to
subpart S
63.6(c)
No
Subpart S specifies
compliance dates for
sources subject to
subpart S
63.6(d)
No
Section reserved
63.6(e)
Yes
63.6(f)
Yes
63.6(g)
Yes
63.6(h)
No
Pertains to continuous
opacity monitors that are
not part of this standard
63.6(i)
Yes
63.6(j)
Yes
63.7
Yes
63.8(a)(1)
Yes
63.8(a)(2)
Yes
63.8(a)(3)
No
Section reserved
63.8(a)(4)
Yes
63.8(b)(1)
Yes
63.8(b)(2)
No
Subpart S specifies
locations to conduct
monitoring
63.8(b)(3)
Yes
63.8(c)(1)
Yes
63.8(c)(2)
Yes
63.8(c)(3)
Yes
63.8(c)(4)
No
Subpart S allows site
specific determination of
monitoring frequency in
63.453 (n)(4)
63.8(c)(5)
No
Pertains to continuous
opacity monitors that are
not part of this standard
63.8(c)(6)
Yes
63.8(c)(7)
Yes
63.8(c)(8)
Yes
63.8(d)
Yes
63.8(e)
Yes
63.8(f)(1)-(5)
Yes
63.8(f)(6)
No
Subpart S does not specify
relative accuracy test for
CEM's
63.8(g)
Yes
63.9(a)
Yes
63.9(b)
Yes
Initial notifications must
be submitted within one
year after the source
becomes subject to the
relevant standard
63.9(c)
Yes
63.9(d)
No
Special compliance
requirements are only
applicable to kraft mills
63.9(e)
Yes
63.9(f)
No
Pertains to continuous
opacity monitors that are
not part of this standard
63.9(g)(1)
Yes
63.9(g)(2)
No
Pertains to continuous
opacity monitors that are
not part of this standard
63.9(g)(3)
No
Subpart S does not specify
relative accuracy tests,
therefore no notification
is required for an
alternative
63.9(h)
Yes
63.9(i)
Yes
63.9(j)
Yes
63.10(a)
Yes
63.10(b)
Yes
63.10(c)
Yes
63.10(d)(1)
Yes
63.10(d)(2)
Yes
63.10(d)(3)
No
Pertains to continuous
opacity monitors that are
not part of this standard
63.10(d)(4)
Yes
63.10(d)(5)
Yes
63.10(e)(1)
Yes
63.10(e)(2)(i)
Yes
63.10(e)(2)(ii)
No
Pertains to continuous
opacity monitors that are
not part of this standard
63.10(e)(3)
Yes
63.10(e)(4)
No
Pertains to continuous
opacity monitors that are
not part of this standard
63.10(f)
Yes
63.11-63.15
Yes
a Wherever subpart A specifies "postmark" dates, submittals
may be sent by methods other than the U.S. Mail (e.g., by
fax or courier). Submittals shall be sent by the
specified dates, but a postmark is not required.
3. Appendix A of part 63 is amended by adding
Method 308 in numerical order to read as follows:
Appendix A to Part 63--Test Methods
* * * * *
Method 308--Procedure for Determination of Methanol Emission
from Stationary Sources
1.0 Scope and Application.
1.1 Analyte. Methanol. Chemical Abstract Service
(CAS) No. 67-56-1.
1.2 Applicability. This method applies to the
measurement of methanol emissions from specified stationary sources.
2.0 Summary of Method. A gas sample is extracted from the
sampling point in the stack. The methanol is collected in
deionized distilled water and adsorbed on silica gel. The
sample is returned to the laboratory where the methanol in
the water fraction is separated from other organic compounds
with a gas chromatograph (GC) and is then measured by a
flame ionization detector (FID). The fraction adsorbed on
silica gel is extracted with an aqueous solution of
n-propanol and is then separated and measured by GC/FID.
3.0 Definitions. [Reserved]
4.0 Interferences. [Reserved]
5.0 Safety.
5.1 Disclaimer. This method may involve hazardous
materials, operations, and equipment. This test method does
not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this
test method to establish appropriate safety and health
practices and to determine the applicability of regulatory
limitations before performing this test method.
5.2 Methanol Characteristics. Methanol is flammable
and a dangerous fire and explosion risk. It is moderately
toxic by ingestion and inhalation.
6.0 Equipment and Supplies.
6.1 Sample Collection. The following items are
required for sample collection:
6.1.1 Sampling Train. The sampling train is shown in
Figure 308-1 and component parts are discussed below.
6.1.1.1 Probe. Teflon , approximately 6-millimeter
(mm) (0.24 inch) outside diameter.
6.1.1.2 Impinger. A 30-milliliter (ml) midget
impinger. The impinger must be connected with leak-free
glass connectors. Silicone grease may not be used to
lubricate the connectors.
6.1.1.3 Adsorbent Tube. Glass tubes packed with the
required amount of the specified adsorbent.
6.1.1.4 Valve. Needle valve, to regulate sample gas
flow rate.
6.1.1.5 Pump. Leak-free diaphragm pump, or
equivalent, to pull gas through the sampling train. Install
a small surge tank between the pump and rate meter to
eliminate the pulsation effect of the diaphragm pump on the
rotameter.
6.1.1.6 Rate Meter. Rotameter, or equivalent, capable
of measuring flow rate to within 2 percent of the selected
flow rate of up to 1000 milliliter per minute (ml/min).
Alternatively, the tester may use a critical orifice to set
the flow rate.
6.1.1.7 Volume Meter. Dry gas meter (DGM),
sufficiently accurate to measure the sample volume to within
2 percent, calibrated at the selected flow rate and
conditions actually encountered during sampling, and
equipped with a temperature sensor (dial thermometer, or
equivalent) capable of measuring temperature accurately to
within 3 oC (5.4 oF).
6.1.1.8 Barometer. Mercury (Hg), aneroid, or other
barometer capable of measuring atmospheric pressure to
within 2.5 mm (0.1 inch) Hg. See the NOTE in Method 5
(40 CFR part 60, appendix A), section 6.1.2.
6.1.1.9 Vacuum Gauge and Rotameter. At least 760-mm
(30-inch) Hg gauge and 0- to 40-ml/min rotameter, to be used
for leak-check of the sampling train.
6.2 Sample Recovery. The following items are required
for sample recovery:
6.2.1 Wash Bottles. Polyethylene or glass, 500-ml,
two.
6.2.2 Sample Vials. Glass, 40-ml, with Teflon -lined
septa, to store impinger samples (one per sample).
6.2.3 Graduated Cylinder. 100-ml size.
6.3 Analysis. The following are required for
analysis:
6.3.1 Gas Chromatograph. GC with an FID, programmable
temperature control, and heated liquid injection port.
6.3.2 Pump. Capable of pumping 100 ml/min. For
flushing sample loop.
6.3.3 Flow Meter. To monitor accurately sample loop
flow rate of 100 ml/min.
6.3.4 Regulators. Two-stage regulators used on gas
cylinders for GC and for cylinder standards.
6.3.5 Recorder. To record, integrate, and store
chromatograms.
6.3.6 Syringes. 1.0- and 10-microliter (l) size,
calibrated, for injecting samples.
6.3.7 Tubing Fittings. Stainless steel, to plumb GC
and gas cylinders.
6.3.8 Vials. Two 5.0-ml glass vials with screw caps
fitted with Teflon -lined septa for each sample.
6.3.9 Pipettes. Volumetric type, assorted sizes for
preparing calibration standards.
6.3.10 Volumetric Flasks. Assorted sizes for
preparing calibration standards.
6.3.11 Vials. Glass 40-ml with Teflon -lined septa,
to store calibration standards (one per standard).
7.0 Reagents and Standards.
NOTE: Unless otherwise indicated, all reagents must
conform to the specifications established by the Committee
on Analytical Reagents of the American Chemical Society.
Where such specifications are not available, use the best
available grade.
7.1 Sampling. The following are required for
sampling:
7.1.1 Water. Deionized distilled to conform to the
American Society for Testing and Materials (ASTM)
Specification D 1193-77, Type 3. At the option of the
analyst, the potassium permanganate (KMnO4) test for
oxidizable organic matter may be omitted when high
concentrations of organic matter are not expected to be
present.
7.1.2 Silica Gel. Deactivated chromatographic grade
20/40 mesh silica gel packed in glass adsorbent tubes. The
silica gel is packed in two sections. The front section
contains 520 milligrams (mg) of silica gel, and the back
section contains 260 mg.
7.2 Analysis. The following are required for
analysis:
7.2.1 Water. Same as specified in section 7.1.1.
7.2.2 n-Propanol, 3 Percent. Mix 3 ml of n-propanol
with 97 ml of water.
7.2.3 Methanol Stock Standard. Prepare a methanol
stock standard by weighing 1 gram of methanol into a 100-ml
volumetric flask. Dilute to 100 ml with water.
7.2.3.1 Methanol Working Standard. Prepare a methanol
working standard by pipetting 1 ml of the methanol stock
standard into a 100-ml volumetric flask. Dilute the
solution to 100 ml with water.
7.2.3.2 Methanol Standards For Impinger Samples.
Prepare a series of methanol standards by pipetting 1, 2, 5,
10, and 25 ml of methanol working standard solution
respectively into five 50-ml volumetric flasks. Dilute the
solutions to 50 ml with water. These standards will have 2,
4, 10, 20, and 50 g/ml of methanol, respectively. After
preparation, transfer the solutions to 40-ml glass vials
capped with Teflon septa and store the vials under
refrigeration. Discard any excess solution.
7.2.3.3 Methanol Standards for Adsorbent Tube Samples.
Prepare a series of methanol standards by first pipetting
10 ml of the methanol working standard into a 100-ml
volumetric flask and diluting the contents to exactly 100 ml
with 3 percent n-propanol solution. This standard will
contain 10 g/ml of methanol. Pipette 5, 15, and 25 ml of
this standard, respectively, into four 50-ml volumetric
flasks. Dilute each solution to 50 ml with 3 percent
n-propanol solution. These standards will have 1, 3, and
5 g/ml of methanol, respectively. Transfer all four
standards into 40-ml glass vials capped with Teflon -lined
septa and store under refrigeration. Discard any excess
solution.
7.2.4 GC Column. Capillary column, 30 meters
(100 feet) long with an inside diameter (ID) of 0.53 mm
(0.02 inch), coated with DB 624 to a film thickness of
3.0 micrometers, ( m) or an equivalent column.
Alternatively, a 30-meter capillary column coated with
polyethylene glycol to a film thickness of 1 m such as AT-WAX or its equivalent.
7.2.5 Helium. Ultra high purity.
7.2.6 Hydrogen. Zero grade.
7.2.7 Oxygen. Zero grade.
8.0 Procedure.
8.1 Sampling. The following items are required for
sampling:
8.1.1 Preparation of Collection Train. Measure 20 ml
of water into the midget impinger. The adsorbent tube must
contain 520 mg of silica gel in the front section and 260 mg
of silica gel in the backup section. Assemble the train as
shown in Figure 308-1. An optional, second impinger that is
left empty may be placed in front of the water-containing
impinger to act as a condensate trap. Place crushed ice and
water around the impinger.
8.1.2 Leak Check. A leak check prior to the sampling
run is optional; however, a leak check after the sampling
run is mandatory. The leak-check procedure is as follows:
Temporarily attach a suitable (e.g., 0- to 40-ml/min)
rotameter to the outlet of the DGM, and place a vacuum gauge
at or near the probe inlet. Plug the probe inlet, pull a
vacuum of at least 250 mm (10 inch) Hg, and note the flow
rate as indicated by the rotameter. A leakage rate not in
excess of 2 percent of the average sampling rate is
acceptable. NOTE: Carefully release the probe inlet plug
before turning off the pump.
8.1.3 Sample Collection. Record the initial DGM
reading and barometric pressure. To begin sampling,
position the tip of the Teflon tubing at the sampling
point, connect the tubing to the impinger, and start the
pump. Adjust the sample flow to a constant rate between
200 and 1000 ml/min as indicated by the rotameter. Maintain
this constant rate (ñ10 percent) during the entire sampling
run. Take readings (DGM, temperatures at DGM and at
impinger outlet, and rate meter) at least every 5 minutes.
Add more ice during the run to keep the temperature of the
gases leaving the last impinger at 20 oC (68 oF) or less.
At the conclusion of each run, turn off the pump, remove the
Teflon tubing from the stack, and record the final
readings. Conduct a leak check as in section 8.1.2. (This
leak check is mandatory.) If a leak is found, void the test
run or use procedures acceptable to the Administrator to
adjust the sample volume for the leakage.
8.2 Sample Recovery. The following items are required
for sample recovery:
8.2.1 Impinger. Disconnect the impinger. Pour the
contents of the midget impinger into a graduated cylinder.
Rinse the midget impinger and the connecting tubes with
water, and add the rinses to the graduated cylinder. Record
the sample volume. Transfer the sample to a glass vial and
cap with a Teflon septum. Discard any excess sample.
Place the samples in an ice chest for shipment to the
laboratory.
8.2.2. Adsorbent Tubes. Seal the silica gel adsorbent
tubes and place them in an ice chest for shipment to the
laboratory.
9.0 Quality Control.
9.1 Miscellaneous Quality Control Measures. The
following quality control measures are required:
Section
Quality control measure
Effect
8.1.2,
8.1.3,
10.1
Sampling equipment leak
check and calibration
Ensures accurate
measurement of
sample volume
10.2
GC calibration
Ensures precision of
GC analysis
9.2 Applicability. When the method is used to analyze
samples to demonstrate compliance with a source emission
regulation, an audit sample must be analyzed, subject to
availability.
9.3 Audit Procedure. Analyze an audit sample with
each set of compliance samples. Concurrently analyze the
audit sample and a set of compliance samples in the same
manner to evaluate the technique of the analyst and the
standards preparation. The same analyst, analytical
reagents, and analytical system shall be used both for the
compliance samples and the EPA audit sample.
9.4 Audit Sample Availability. Audit samples will be
supplied only to enforcement agencies for compliance tests.
Audit samples may be obtained by writing:
Source Test Audit Coordinator (MD-77B)
Air Measurement Research Division
National Exposure Research Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
or by calling the Source Test Audit Coordinator (STAC) at
(919) 541-7834. The audit sample request must be made at
least 30 days prior to the scheduled compliance sample
analysis.
9.5 Audit Results. Calculate the audit sample
concentration according to the calculation procedure
provided in the audit instructions included with the audit
sample. Fill in the audit sample concentration and the
analyst's name on the audit response form included with the
audit instructions. Send one copy to the EPA Regional
Office or the appropriate enforcement agency and a second
copy to the STAC. The EPA Regional office or the
appropriate enforcement agency will report the results of
the audit to the laboratory being audited. Include this
response with the results of the compliance samples in
relevant reports to the EPA Regional Office or the
appropriate enforcement agency.
10.0 Calibration and Standardization.
10.1 Metering System. The following items are
required for the metering system:
10.1.1 Initial Calibration.
10.1.1.1 Before its initial use in the field, first
leak-check the metering system (drying tube, needle valve,
pump, rotameter, and DGM) as follows: Place a vacuum gauge
at the inlet to the drying tube, and pull a vacuum of 250 mm
(10 inch) Hg; plug or pinch off the outlet of the flow
meter, and then turn off the pump. The vacuum shall remain
stable for at least 30 seconds. Carefully release the
vacuum gauge before releasing the flow meter end.
10.1.1.2 Next, remove the drying tube, and calibrate
the metering system (at the sampling flow rate specified by
the method) as follows: Connect an appropriately sized wet
test meter (e.g., 1 liter per revolution (0.035 cubic feet
per revolution)) to the inlet of the drying tube. Make
three independent calibrations runs, using at least five
revolutions of the DGM per run. Calculate the calibration
factor, Y (wet test meter calibration volume divided by the
DGM volume, both volumes adjusted to the same reference
temperature and pressure), for each run, and average the
results. If any Y-value deviates by more than 2 percent
from the average, the metering system is unacceptable for
use. Otherwise, use the average as the calibration factor
for subsequent test runs.
10.1.2 Posttest Calibration Check. After each field
test series, conduct a calibration check as in
section 10.1.1 above, except for the following variations:
(a) the leak check is not to be conducted, (b) three, or
more revolutions of the DGM may be used, and (c) only two
independent runs need be made. If the calibration factor
does not deviate by more than 5 percent from the initial
calibration factor (determined in section 10.1.1), then the
DGM volumes obtained during the test series are acceptable.
If the calibration factor deviates by more than 5 percent,
recalibrate the metering system as in section 10.1.1, and
for the calculations, use the calibration factor (initial or
recalibration) that yields the lower gas volume for each
test run.
10.1.3 Temperature Sensors. Calibrate against
mercury-in-glass thermometers.
10.1.4 Rotameter. The rotameter need not be
calibrated, but should be cleaned and maintained according
to the manufacturer's instruction.
10.1.5 Barometer. Calibrate against a mercury
barometer.
10.2 Gas Chromatograph. The following procedures are
required for the gas chromatograph:
10.2.1 Initial Calibration. Inject 1 l of each of
the standards prepared in sections 7.2.3.3 and 7.2.3.4 into
the GC and record the response. Repeat the injections for
each standard until two successive injections agree within
5 percent. Using the mean response for each calibration
standard, prepare a linear least squares equation relating
the response to the mass of methanol in the sample. Perform
the calibration before analyzing each set of samples.
10.2.2 Continuing Calibration. At the beginning of
each day, analyze the mid level calibration standard as
described in section 10.5.1. The response from the daily
analysis must agree with the response from the initial
calibration within 10 percent. If it does not, the initial
calibration must be repeated.
11.0 Analytical Procedure.
11.1 Gas Chromatograph Operating Conditions. The
following operating conditions are required for the GC:
11.1.1 Injector. Configured for capillary column,
splitless, 200 oC (392 oF).
11.1.2 Carrier. Helium at 10 ml/min.
11.1.3 Oven. Initially at 45 oC for 3 minutes; then
raise by 10 oC to 70 oC; then raise by 70 oC/min to 200 oC.
11.2 Impinger Sample. Inject 1 l of the stored
sample into the GC. Repeat the injection and average the
results. If the sample response is above that of the
highest calibration standard, either dilute the sample until
it is in the measurement range of the calibration line or
prepare additional calibration standards. If the sample
response is below that of the lowest calibration standard,
prepare additional calibration standards. If additional
calibration standards are prepared, there shall be at least
two that bracket the response of the sample. These
standards should produce approximately 50 percent and 150
percent of the response of the sample.
11.3 Silica Gel Adsorbent Sample. The following items
are required for the silica gel adsorbent samples:
11.3.1 Preparation of Samples. Extract the front and
backup sections of the adsorbent tube separately. With a
file, score the glass adsorbent tube in front of the first
section of silica gel. Break the tube open. Remove and
discard the glass wool. Transfer the first section of the
silica gel to a 5-ml glass vial and stopper the vial.
Remove the spacer between the first and second section of
the adsorbent tube and discard it. Transfer the second
section of silica gel to a separate 5-ml glass vial and
stopper the vial.
11.3.2 Desorption of Samples. Add 3 ml of the
10 percent n-propanol solution to each of the stoppered
vials and shake or vibrate the vials for 30 minutes.
11.3.3 Inject a 1- l aliquot of the diluted sample
from each vial into the GC. Repeat the injection and
average the results. If the sample response is above that
of the highest calibration standard, either dilute the
sample until it is in the measurement range of the
calibration line or prepare additional calibration
standards. If the sample response is below that of the
lowest calibration standard, prepare additional calibration
standards. If additional calibration standards are
prepared, there shall be at least two that bracket the
response of the sample. These standards should produce
approximately 50 percent and 150 percent of the response of
the sample.
12.0 Data Analysis and Calculations.
12.1 Nomenclature.
Caf = Concentration of methanol in the front of
the adsorbent tube, g/ml.
Cab = Concentration of methanol in the back of the
adsorbent tube, g/ml.
Ci = Concentration of methanol in the impinger
portion of the sample train, g/ml.
E = Mass emission rate of methanol, g/hr
(lb/hr).
Mtot = Total mass of methanol collected in the
sample train, g.
Pbar = Barometric pressure at the exit orifice of
the DGM, mm Hg (in. Hg).
Pstd = Standard absolute pressure, 760 mm Hg
(29.92 in. Hg).
Qstd = Dry volumetric stack gas flow rate corrected
to standard conditions, dscm/hr (dscf/hr).
Tm = Average DGM absolute temperature, degrees K
(oR).
Tstd = Standard absolute temperature, 293 degrees K
(528 oR).
Vaf = Volume of front half adsorbent sample, ml.
Vab = Volume of back half adsorbent sample, ml.
Vi = Volume of impinger sample, ml.
Vm = Dry gas volume as measured by the DGM, dry
cubic meters (dcm), dry cubic feet (dcf).
Vm(std) = Dry gas volume measured by the DGM,
corrected to standard conditions, dry
standard cubic meters (dscm), dry standard
cubic feet (dscf).
12.2 Mass of Methanol. Calculate the total mass of
methanol collected in the sampling train using
Equation 308-1.
12.3 Dry Sample Gas Volume, Corrected to Standard
Conditions. Calculate the volume of gas sampled at standard
conditions using Equation 308-2.
12.4 Mass Emission Rate of Methanol. Calculate the
mass emission rate of methanol using Equation 308-3.
13.0 Method Performance. [Reserved]
14.0 Pollution Prevention. [Reserved]
15.0 Waste Management. [Reserved]
16.0 Bibliography.
1. Rom, J.J. "Maintenance, Calibration, and Operation
of Isokinetic Source Sampling Equipment." Office of Air
Programs, Environmental Protection Agency. Research
Triangle Park, NC. APTD-0576. March 1972.
2. Annual Book of ASTM Standards. Part 31; Water,
Atmospheric Analysis. American Society for Testing and
Materials. Philadelphia, PA. 1974. pp. 40-42.
3. Westlin, P.R. and R.T. Shigehara. "Procedure for
Calibrating and Using Dry Gas Volume Meters as Calibration
Standards." Source Evaluation Society Newsletter.
3(1):17-30. February 1978.
4. Yu, K.K. "Evaluation of Moisture Effect on Dry Gas
Meter Calibration." Source Evaluation Society Newsletter.
5(1):24-28. February 1980.
5. NIOSH Manual of Analytical Methods, Volume 2. U.S.
Department of Health and Human Services National Institute
for Occupational Safety and Health. Center for Disease
Control. 4676 Columbia Parkway, Cincinnati, OH 45226.
(available from the Superintendent of Documents, Government
Printing Office, Washington, DC 20402.)
6. Pinkerton, J.E. "Method for Measuring Methanol in
Pulp Mill Vent Gases." National Council of the Pulp and
Paper Industry for Air and Stream Improvement, Inc., New
York, NY.
17.0 Tables, Diagrams, Flowcharts, and Validation Data.
[Reserved]
* * * * *
PART 261--[AMENDED]
1. The authority citation of part 261 continues to
read as follows:
Authority: 42 U.S.C. 6905, 6912(a), 6921, 6922, and
6938.
2. Section 261.4, is amended by adding (a)(15) to read
as follows:
261.4 Exclusions.
(a) * * *
(15) Condensates derived from the overhead gases from
kraft mill steam strippers that are used to comply with
40 CFR part 63, subpart S, 63.446(e). The exemption
applies only to combustion at the mill generating the
condensates.
* * * * *
Please e-mail any comments or questions to the Clean Air Act Information
Network.
Return to the
Clean Air Act
Information Network Home Page