Two Optional Methods for Relative Accuracy Test Audits of Mercury Monitoring Systems Installed on Combustion Flue Gas Streams and Several Amendments to Related Mercury Monitoring Provisions, 51494-51531 [07-4147]
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51494
Federal Register / Vol. 72, No. 173 / Friday, September 7, 2007 / Rules and Regulations
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Parts 60, 72 and 75
[EPA–HQ–OAR–2007–0164, FRL–8459–8]
RIN 2060–AO01
Two Optional Methods for Relative
Accuracy Test Audits of Mercury
Monitoring Systems Installed on
Combustion Flue Gas Streams and
Several Amendments to Related
Mercury Monitoring Provisions
Environmental Protection
Agency (EPA).
ACTION: Direct final rule.
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AGENCY:
SUMMARY: EPA is taking direct final
action on two optional methods for
relative accuracy audits of mercury
monitoring systems installed on
combustion flue gas streams and several
amendments to related mercury
monitoring provisions. This action
approves two optional mercury (Hg)
emissions test methods for potential use
in conjunction with an existing
regulatory requirement for Hg emissions
monitoring, as well as several revisions
to the mercury monitoring provisions
themselves. This action is in regard to
the testing and monitoring requirements
for mercury specified in the Federal
Register on May 18, 2005. Since that
publication, EPA has received
numerous comments concerning the
desirability of EPA evaluating and
allowing use of the measurement
techniques addressed in the two
optional methods in lieu of the methods
identified in the cited Federal Register
publication, as they can produce equally
acceptable measures of the relative
accuracy achieved by Hg monitoring
systems. This action allows use of these
two optional methods entirely at the
discretion of the owner or operator of an
affected emission source in place of the
two currently specified methods. This
direct final rule also amends
Performance Specification 12A by
adding Methods 30A and 30B to the list
of reference methods acceptable for
measuring Hg concentration and the Hg
monitoring provisions of May 18, 2005,
to reflect technical insights since gained
by EPA which will help to facilitate
implementation including clarification
and increased regulatory flexibility for
affected sources.
DATES: This rule is effective on
November 6, 2007 without further
notice, unless EPA receives adverse
comment by October 9, 2007. If EPA
receives adverse comment, EPA will
publish a timely withdrawal in the
Federal Register informing the public
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that some or all of the amendments in
this rule will not take effect.
ADDRESSES: Submit your comments,
identified by Docket ID No. EPA–HQ–
OAR–2007–0164, by one of the
following methods:
• www.regulations.gov. Follow the
on-line instructions for submitting
comments.
• E-mail: a-and-r-docket@epa.gov.
• Fax: (202) 566–9744.
• Mail: Two Optional Methods for
Relative Accuracy Test Audits of
Mercury Monitoring Systems Installed
on Combustion Flue Gas Streams and
Several Amendments to the Related
Mercury Monitoring Provisions,
Environmental Protection Agency,
Mailcode: 2822T, 1200 Pennsylvania
Avenue, NW., Washington, DC 20460.
Please include a total of two copies.
• Hand Delivery: EPA Docket Center,
1301 Constitution Avenue, NW., EPA
Headquarters Library, Room 3334, EPA
West Building, Washington, DC 20460.
Such deliveries are only accepted
during the Docket’s normal hours of
operation, and special arrangements
should be made for deliveries of boxed
information.
Instructions: Direct your comments to
Docket ID No. EPA–HQ–OAR–2007–
0164. EPA’s policy is that all comments
received will be included in the public
docket without change and may be
made available online at
www.regulations.gov, including any
personal information provided, unless
the comment includes information
claimed to be Confidential Business
Information (CBI) or other information
whose disclosure is restricted by statute.
Do not submit information that you
consider to be CBI or otherwise
protected through www.regulations.gov
or e-mail. The www.regulations.gov Web
site is an ‘‘anonymous access’’ system,
which means EPA will not know your
identity or contact information unless
you provide it in the body of your
comment. If you send an e-mail
comment directly to EPA without going
through www.regulations.gov, your email address will be automatically
captured and included as part of the
comment that is placed in the public
docket and made available on the
Internet. If you submit an electronic
comment, EPA recommends that you
include your name and other contact
information in the body of your
comment and with any disk or CD–ROM
you submit. If EPA cannot read your
comment due to technical difficulties
and cannot contact you for clarification,
EPA may not be able to consider your
comment. Electronic files should avoid
the use of special characters, any form
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of encryption, and be free of any defects
or viruses. For additional information
about EPA’s public docket, visit the EPA
Docket Center homepage at https://
www.epa.gov/epahome/dockets.htm.
Docket: All documents in the docket
are listed in the www.regulations.gov
index. Although listed in the index,
some information is not publicly
available, e.g., CBI or other information
whose disclosure is restricted by statute.
Certain other material, such as
copyrighted material, will be publicly
available only in hard copy. Publicly
available docket materials are available
either electronically in
www.regulations.gov or in hard copy at
the Two Optional Methods for Relative
Accuracy Audits of Mercury Monitoring
Systems Installed on Combustion Flue
Gas Streams Air and Radiation Docket,
EPA/DC, EPA West Building, EPA
Headquaters Library, Room 3334, 1301
Constitution Avenue, NW., Washington,
DC. The Public Reading Room is open
from 8:30 a.m. to 4:30 p.m., Monday
through Friday, excluding legal
holidays. The telephone number for the
Public Reading Room is (202) 566–1744,
and the telephone number for the Air
and Radiation Docket is (202) 566–1742.
FOR FURTHER INFORMATION CONTACT:
Either Mr. William Grimley, Office of
Air Quality Planning and Standards, Air
Quality Assessment Division,
Measurement Technology Group (E143–
02), EPA, Research Triangle Park, NC
27711, telephone (919) 541–1065,
facsimile number (919) 541–0516, email address: grimley.william@epa.gov
or Ms. Robin Segall, Office of Air
Quality Planning and Standards, Air
Quality Assessment Division,
Measurement Technology Group (E143–
02), EPA, Research Triangle Park, NC
27711, telephone (919) 541–0893,
facsimile number (919) 541–0516, email address: segall.robin@epa.gov.
SUPPLEMENTARY INFORMATION:
I. Why is EPA using a Direct Final
Rule?
EPA is publishing this rule without a
prior proposed rule because we view
this as a noncontroversial action and
anticipate no adverse comment. The
most important benefit of direct final
rulemaking for this action is to provide:
(1) Additional reference method
options, and (2) judicious revisions to
mercury monitoring provisions
specified in the Federal Register on
May 18, 2005 that, if successful, relieve
affected facilities of uncertainty
regarding final emission monitoring
requirements and certification details as
opposed to waiting through a
potentially protracted proposal/final
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rulemaking process. Insofar as the two
methods are concerned, EPA believes
that they contain the necessary elements
to generate acceptable data quality
without being unduly burdensome.
Through experience gained from
developing existing performance based
methods and trading rules, EPA has
learned to identify test method criteria
significant to effective rule
implementation. EPA believes each of
the two methods adopted in this action
contain adequate specific criteria and
procedures essential to the accurate
measurement of Hg emissions, without
adversely compromising the goals of
performance-based methodology. EPA
will continue to support and advance
the principles and practicality of these
methods by adding detailed method
application information to facilitate
their use to the Web site www.epa.gov/
NAICS a
Category
Industry ............................................
Federal government .........................
State/local governments ..................
Tribal governments ..........................
a North
airmarkets/ as it becomes available.
Since use of either of these methods is
not mandatory, but optional, there
should be no objection to their
availability. Regarding the amendments
to the Hg emission monitoring
provisions of 40 CFR parts 72 and 75,
these amendments reflect EPA’s
increased technical understanding since
the May 18, 2005 rulemaking. However,
in the ‘‘Proposed Rules’’ section of
today’s Federal Register, we are
publishing a separate document that
will serve as the proposed rule to
approve provisions, if any, of this direct
final rule that receive relevant adverse
comments on this direct final rule. We
will not institute a second comment
period on this action. Any parties
interested in commenting must do so at
this time. For further information about
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commenting on this rule, see the
ADDRESSES section of this document.
If EPA receives adverse comment on
one or more distinct provisions of this
rulemaking, we will publish a timely
withdrawal in the Federal Register
indicating which provisions we are
withdrawing and informing the public
that those provisions will not take
effect. The provisions that are not
withdrawn will become effective on the
date set out above, notwithstanding
adverse comment on any other
provision. We would address all public
comments in a subsequent final rule
based on the proposed rule.
II. Does This Action Apply to Me?
Regulated Entities. The regulated
categories and entities affected by this
direct final rule include:
Examples of regulated entities
Fossil
Fossil
Fossil
Fossil
fuel-fired
fuel-fired
fuel-fired
fuel-fired
electric
electric
electric
electric
utility
utility
utility
utility
steam
steam
steam
steam
generating
generating
generating
generating
units.
units owned by the Federal government.
units owned by municipalities.
units in Indian country.
American Industry Classification System.
State, or local government-owned and operated establishments are classified according to the activity in which they are engaged.
b Federal,
This table is not intended to be
exhaustive, but rather provides a guide
for readers regarding entities likely to be
affected by this direct final rule. If you
have any questions regarding the
applicability of this direct final rule to
a particular entity, consult either the air
permit authority for the entity or your
EPA regional representative as listed in
40 CFR 63.13.
III. Where Can I Obtain a Copy of This
Action?
In addition to being available in the
docket, an electronic copy of this direct
final rule is also available on the World
Wide Web through the Technology
Transfer Network (TTN). Following
signature, a copy of this direct final rule
will be posted on the TTN’s policy and
guidance page for newly proposed or
promulgated rules at the following
address: https://www.epa.gov/ttn/oarpg.
The TTN provides information and
technology exchange in various areas of
air pollution control.
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IV. How Is This Document Organized?
The information presented in this
preamble is organized as follows:
I. Why Is EPA Using a Direct Final Rule?
II. Does This Action Apply to Me?
III. Where Can I Obtain a Copy of This
Action?
IV. How Is This Document Organized?
V. Background
VI. This Action
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VII. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory
Planning and Review
B. Paperwork Reduction Act
C. Regulatory Flexibility Act
D. Unfunded Mandates Reform Act
E. Executive Order: 13132: Federalism
F. Executive Order 13175: Consultation
and Coordination With Indian Tribal
Governments
G. Executive Order 13045: Protection of
Children From Environmental Health
and Safety Risks
H. Executive Order 13211: Actions That
Significantly Affect Energy Supply,
Distribution, or Use
I. National Technology Transfer and
Advancement Act
J. Executive Order 12898: Federal Actions
To Address Environmental Justice in
Minority Populations and Low-Income
Populations
K. Congressional Review Act
V. Background
On May 18, 2005, in the preamble of
the Clean Air Mercury Rule (CAMR) (70
FR 28608), EPA stated its intention to
propose and promulgate an
instrumental reference method as an
alternative to the use of ASTM Method
D6784–02 (the Ontario Hydro Method)
to perform Relative Accuracy Test
Audits (RATAs) of Hg continuous
emission monitoring systems (CEMS)
and sorbent trap monitoring systems
used to monitor Hg emissions from coalfired power plants.
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In comments on the proposed CAMR,
commenters had two primary objections
to the use of the Ontario Hydro Method
as the reference test method for RATAs.
Some expressed concern that the
complexity of this wet chemical method
could lead to results that would cause
a properly functioning Hg CEMS to fail
a RATA. Other commenters noted that,
unlike instrumental reference methods
used to audit CEMS for SO2 and NOX
that provide real-time values, test
results from the Ontario Hydro Method
can take weeks to be received from the
laboratory. Commenters stated that this
time lag can lead to implementation
problems with regard to both missing
data and emissions reporting.
Since the CAMR was promulgated,
EPA has proposed changes to 40 CFR
part 75, which would allow the use of
EPA Method 29, with enhanced qualityassurance procedures, as an alternative
Hg reference method (71 FR 49257;
August 22, 2006). Although Method 29
is somewhat simpler than the Ontario
Hydro Method and is more familiar to
stack testers and State regulatory
agencies, it is also a wet chemistry
method and is, therefore, subject to the
same limitations that make the Ontario
Hydro method less than optimal for
RATA testing.
In view of these considerations, EPA
believes that for RATA testing, an
instrumental Hg reference method
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would be preferable to both the Ontario
Hydro Method and to Method 29. An
instrumental method would provide
real-time data that would best facilitate
implementation of a mercury cap and
trade program. Therefore, this action
approves a performance-based
instrumental reference method for
measuring Hg emission concentrations.
Another commenter to the proposed
CAMR recommended that the sorbent
trap monitoring approach, now
specified in 40 CFR part 75, appendix
K, be considered for use as a reference
method. Although EPA did not commit
to establishing a sorbent trap reference
method at the time of CAMR
promulgation, stakeholder interest in
this methodology has increased
significantly. In an August 22, 2006
Federal Register notice, EPA solicited
comment on the use of sorbent trap
technology for Hg reference method
testing, and numerous supportive
comments were received. In view of
this, we initiated a review of available
historical test data where concurrent
measurements of Hg concentration were
made with sorbent trap systems and
either the Ontario Hydro Method or
Method 29. These data, taken together
with additional supporting data from
recent field tests that were performed
after the CAMR was promulgated,
suggest that using the sorbent trap
methodology for Hg reference method
testing is viable. The Hg sorbent trap
approach is less onerous to use than
either Ontario Hydro or Method 29, and
although it does not measure real-time
Hg concentrations, a thermal technique
can be used to analyze the samples on
the same day that they are collected,
facilitating RATA testing in the context
of a cap and trade program. Therefore,
this action also approves a sorbent trap
reference method for Hg, as an
alternative to the Ontario Hydro Method
and Method 29.
This direct final rule also includes
several carefully considered
amendments to the Hg emission
monitoring provisions of 40 CFR parts
72 and 75. EPA believes these
amendments will facilitate
implementation of the CAMR by
clarifying portions of that rule and by
providing added regulatory flexibility to
the affected sources.
VI. This Action
This direct final rule allows for the
earliest possible use of two optional
reference test methods for measuring
total vapor phase mercury emissions
from stationary sources as well as
several related amendments to the Hg
monitoring provisions of the CAMR.
Both an instrumental test method and a
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sorbent trap test method for
measurement of total vapor phase
mercury emissions are being added to
Appendix A–8 of 40 CFR part 60 as
approved alternatives to the Ontario
Hydro Method and EPA Method 29 to
perform RATAs of installed mercury
monitoring systems. The two methods
are discussed below, and the related
amendments are explained in detail
later in this section.
The first method being added to
appendix A–8 of 40 CFR part 60 today
is titled ‘‘Method 30A—Determination
of Total Vapor Phase Mercury Emissions
from Stationary Sources (Instrumental
Analyzer Procedure).’’ In Method 30A, a
sample of the effluent gas is
continuously extracted and conveyed to
an analyzer capable of measuring the
total vapor phase Hg concentration.
Elemental and oxidized mercury (i.e.,
Hg0 and Hg∂2) may be measured
separately or simultaneously but, for
purposes of this method, total vapor
phase Hg is the sum of Hg0 and Hg∂2.
Method 30A provides test programspecific verification of method
performance using a dynamic spiking
approach, coupled with other
performance criteria, which include
system calibration, interference testing,
and system integrity/drift checks. The
dynamic spiking requirement, which is
a gaseous ‘‘method of standard
additions,’’ is the only part of Method
30A not parallel to the routinely applied
instrumental reference methods used to
perform relative accuracy testing of
CEMS for SO2 and NOX. The dynamic
spiking procedure is included in
Method 30A to characterize
measurement bias for Hg, which can be
highly reactive on a site-specific basis
(i.e., for each emissions sample matrix),
with recovery criteria set to ensure that
the bias is held to a minimal level. All
performance requirements of Method
30A must be met for the data to be
considered valid. The availability of an
instrumental reference method for Hg
testing is consistent with the approach
EPA has taken in the successful Acid
Rain and NOX Budget emissions trading
programs.
Method 30A is performance based in
keeping with the criteria established
under our Notice of Intent to Implement
Performance Based Measurement
Systems for Environmental Monitoring
(62 FR 52098, October 6, 1997). Use of
the performance-based measurement
approach will allow for continued
development and application of new,
improved, and more cost-effective Hg
measurement technologies while
ensuring the collection of data of known
quality.
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Based on EPA’s experience in
conducting test programs to evaluate the
procedures and performance criteria
included in Method 30A, EPA
recognizes that although prototypes of
all equipment needed to perform this
method have been successfully
demonstrated in the field, at present the
equipment needed to follow all
procedures required by the method is
commercially available only on a
limited basis, and is being further
refined. One of the issues of greatest
concern in the development of an
instrumental reference method for Hg
has been the design of the sampling
probe. Most of the commerciallyavailable probes suitable for Hg
measurement are very heavy (over 100
lbs.) making it difficult to move the
probe from point-to-point and port-toport for Hg stratification testing and/or
sample traverses. Much progress is
being made in probe redesign. One
manufacturer has recently developed a
probe that weighs less than 40 lbs.,
samples at significantly lower flow
rates, and is suitable for dynamic
spiking. Additional field testing of this
probe and others currently under
development is underway, and EPA
plans to continue to actively encourage
equipment development and evaluation.
To encourage the use of Method 30A,
including further development of the
supporting equipment, which we
believe will eventually enable source
testers to perform Hg monitoring system
RATAs more efficiently and will
become the reference method of choice
for many testing companies and affected
sources, we are deferring the
requirement for implementation of the
dynamic spiking and Hg stratification
test procedures until January 1, 2009.
EPA believes this deferral is reasonable
because Hg monitoring data reported to
EPA in 2009 will not be used in the
trading of Hg allowances, as allowance
accounting under the CAMR does not
begin until 2010. Source testers are
encouraged to use this time to acquire
the necessary equipment and familiarize
themselves with these procedures. Also,
for all emissions test programs and
RATAs performed under CAMR prior to
January 1, 2009, we are allowing either:
(1) A 12-point traverse for sulfur dioxide
(SO2) to be substituted for a 12-point Hg
traverse, in cases where stratification
testing is used to determine the
appropriate number and location of the
reference method sampling points, or (2)
use of the alternate three-point traverse
line (0.4, 1.2, and 2.0 meters from the
stack wall) as specified in section
8.1.3.2 of Performance Specification 2
(40 CFR part 60, appendix B). We
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believe that in the short-term, these
temporary deferrals will encourage the
application of Method 30A and will
help affected CAMR sources meet the
January 1, 2009 deadline for initial
certification of the required Hg
monitoring systems. Several additional
Method 30A development
considerations are worthy of note. A
preliminary draft of Method 30A was
first available for public consideration
on an EPA Web site (www.epa.gov/ttn/
emc/) on February 28, 2006. Since that
time, EPA and several stakeholder
groups have evaluated the various
technical aspects of the method. Based
on the combined laboratory and field
observations, EPA has been able to
simplify several procedural
requirements that we believe are
essential to the method. The dynamic
spiking requirement (for test programspecific verification of measurement
system data quality) has been reduced to
only a pretest requirement. The
interference test has been made
optional. The three-point system
calibration error test using Hg∂2 has
been streamlined to a system integrity
check using a zero gas and a single
upscale Hg∂2 gas. Another change has
been to relax the Hg0 calibration error
specification from 2 percent to 5 percent
of span, in recognition of the fact that
this procedure is a check of the entire
measurement system, as well as the
current knowledge regarding the
uncertainty of NIST traceable standards.
EPA does plan, however, to reconsider
this specification relaxation as more
field data become available. A final
consideration in development of
Method 30A has been the requirement
for calibration with both Hg0 and Hg∂2.
Some stakeholders have recommended
that we eliminate the Hg0 calibration
and rely solely on the Hg∂2 calibration.
EPA, however, believes this approach
would not be adequate, because if only
Hg∂2 were used, instrument calibration
response adjustment could compensate
for an unknown amount of converter
inefficiency, which would then result in
an inaccurate total mercury
measurement in situations where Hg0 is
an appreciable fraction of the total stack
gas Hg.
The second method being added to
appendix A–8 of 40 CFR part 60 today
is titled ‘‘Method 30B—Use of Sorbent
Traps to Measure Total Vapor Phase
Mercury Emissions from Coal-Fired
Combustion Sources.’’ In Method 30B, a
sample of the effluent gas is
continuously drawn through a series of
tubes containing activated carbon or
another sorbent material. After
sampling, the tubes are sealed. The Hg
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captured by the sorbent is then either:
(1) Thermally desorbed and analyzed; or
(2) the tubes are transferred to a
laboratory for extraction of Hg and
analysis. Like Method 30A, Method 30B
is a performance-based method and
contains performance specifications and
procedures for hardware selection and
calibration, sorbent spiking, and
analytical recovery/analysis which
allow for development and application
of new, improved, and more costeffective Hg measurement technologies
while still ensuring the collection of
data of known quality. In particular,
Method 30B contains five key
measurement performance tests
designed to ensure: (1) Selection of a
sorbent and analytical technique
combination capable of quantitative
collection and analysis of gaseous Hg,
(2) collection during field testing of
enough Hg on each sorbent trap to be
reliably quantified, and (3) adequate
performance of the method for each test
program.
In considering development of a
sorbent trap-based reference method,
EPA has reviewed historical emissions
data where sorbent trap measurement
systems were operated concurrently
with either the Ontario Hydro Method
or Method 29 (40 CFR part 60, appendix
A–8). EPA has also conducted several
field test evaluations of sorbent trap
systems versus the Ontario Hydro
Method in collaboration with the
Electric Power Research Institute (EPRI).
Based on these efforts, we have
concluded that a sorbent trap-based
technique coupled with appropriate
performance criteria and QA procedures
can provide Hg emissions data of
quality comparable to that produced by
the Ontario Hydro Method. Data
supporting this conclusion are
presented in the docket, EPA–HQ–
OAR–2007–0164.
As we have done for Method 30A, for
Method 30B emission tests and RATAs
performed prior to January 1, 2009, we
are allowing either: (1) A 12-point
traverse for sulfur dioxide (SO2) to be
substituted for a 12-point Hg traverse for
the stratification testing used to
determine the number and location of
the reference method sampling points,
or (2) use of the alternate three-point
traverse line (0.4, 1.2, and 2.0 meters
from the stack wall) as specified in
section 8.1.3.2 of Performance
Specification 2 (40 CFR part 60,
appendix B). We also intend to extend
this temporary deferral of mercury
stratification testing to application of
the Ontario Hydro Method and Method
29. EPA believes this deferral is
reasonable because Hg monitoring data
reported to EPA in 2009 will not be
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used in the trading of Hg allowances, as
allowance accounting under the CAMR
does not begin until 2010.
This direct final rule also amends
Performance Specification 12A of
appendix B to part 60 by adding
Methods 30A and 30B to the list of
reference methods acceptable for
relative accuracy testing of Hg emissions
monitoring systems. Once this direct
final rule becomes effective, the
reference methods acceptable for Hg
measurement in Performance
Specification 12A will include Methods
29, 30A, 30B, and ASTM D6784–02.
With today’s action, EPA is taking the
opportunity to include several
considered revisions to the Hg emission
monitoring provisions of 40 CFR parts
72 and 75 as described in detail below.
EPA is including these revisions in this
direct final rule because we believe that
they will facilitate implementation of
the Hg monitoring under CAMR.
First, § 75.81(a) is being revised to
confirm that the Hg CEMS and sorbent
trap monitoring systems required under
subpart I of part 75 are to measure the
total vapor phase mass concentration of
Hg in the flue gas, including both the
elemental and oxidized forms of Hg,
expressed in units of micrograms per
standard cubic meter (µg/scm).
Although it is generally understood that
total vapor phase Hg is the regulated
pollutant under CAMR, it recently was
brought to EPA’s attention that subpart
I of part 75 does not explicitly state that
Hg monitoring systems only need to
measure total vapor phase Hg. The
amended language in § 75.81(a) clarifies
this.
Second, paragraph (i) in § 75.15 is
being revised and a new paragraph
(d)(2)(ix) is being added to § 75.20, to
codify the rules for using optional nonredundant (‘‘cold’’) backup Hg
monitoring systems and like-kind
replacement Hg analyzers, when the
primary Hg monitoring system is unable
to provide quality-assured data. For the
other types of monitoring systems
required by part 75, these monitoring
options have been in place since May
1999 (see 64 FR 28597, May 26, 1999).
Today’s action simply extends these
provisions to Hg monitoring systems.
Through the years, the regulated
community has found these backup
monitoring options to be beneficial, in
that they minimize the use of missing
data substitution procedures during
outages of the primary monitoring
system.
In particular, § 75.20(d)(2)(ix)
specifies that a non-redundant backup
Hg monitoring system can either be a Hg
CEMS or a sorbent trap monitoring
system. The non-redundant backup Hg
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monitoring system must be initially
certified at each unit or stack location
where it will be used, in accordance
with § 75.20(d)(2)(i). For a nonredundant backup Hg CEMS, all of the
initial certification tests specified in
§ 75.20(c)(1) are required, except for the
7-day calibration error test. However, for
ongoing quality assurance (QA), a RATA
is required only once every two years (8
calendar quarters), as specified in
§ 75.20(d)(2)(vi). For a non-redundant
backup sorbent trap monitoring system,
a RATA is required for initial
certification, and once every two years
thereafter for ongoing QA.
When a certified non-redundant
backup Hg CEMS or a like-kind
replacement Hg analyzer is brought into
service, a three-point linearity check
with elemental Hg standards and a
single-point system integrity check will
be required. Alternatively, a three-level
system integrity check may be
performed instead of these two tests.
When a certified non-redundant backup
sorbent trap monitoring system is
brought into service, only the routine
sampling and QA procedures of § 75.15
and appendix K of part 75 will be
required.
Each non-redundant backup Hg
monitoring system and each like-kind
replacement Hg analyzer will be subject
to the applicable ongoing QA
requirements, restrictions and
conditions specified in § 75.20(d)(2). For
certified non-redundant backup Hg
CEMS and like-kind replacement Hg
analyzers, the weekly system integrity
checks described in section 2.6 of
appendix B of 40 CFR part 75 will also
be required as long as the system or
analyzer remains in service, unless the
daily calibration error tests of the
analyzer are done using NIST-traceable
oxidized Hg standards.
Third, a new paragraph (k) is being
added to § 75.15 that: (1) Clarifies that,
when the RATA of an appendix K
sorbent trap monitoring system is
performed, the type of sorbent material
used in the appendix K sorbent traps
must be the same as that used for daily
operation of the appendix K monitoring
system, and (2) allows the appendix K
traps used during RATA testing to be
smaller than the traps used for daily
operation of the appendix K monitoring
system. This change will be particularly
advantageous at very low Hg
concentrations as it will facilitate
shorter RATA test run times. Parallel
changes are being made to section 6.5.7
of appendix A of part 75 to be consistent
with the provisions of § 75.15(k).
Section 6.5.7 currently requires the
appendix K sorbent traps used for the
RATA to be the same size as the traps
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used for daily operation of the appendix
K monitoring system.
Fourth, today’s action revises a
number of sections of part 75, appendix
K, pertaining to the use of sorbent trap
monitoring systems. EPA is
withdrawing the requirement to use the
percentage recovery of the elemental Hg
spike in section 3 of each sorbent trap
to adjust or ‘‘normalize’’ the Hg mass
collected in sections 1 and 2 of the trap.
The requirement to spike the third
section of each trap is being retained
and data from each pair of traps must
still be invalidated if either or both
spike recovery percentages fall outside
the acceptable limits;1 however, the
results of the spike recoveries will no
longer be used to adjust the Hg mass
collected in the first two sections of the
traps. EPA is making this rule change
based on an analysis of recent spike
recovery data from long-term appendix
K field demonstrations. Although the
vast majority of the spike recoveries in
these studies have been within the
currently acceptable limits of 75 to 125
percent, the requirement to normalize
based on spike recovery could affect
data precision. For a given pair of traps,
if one spike recovery was high (e.g., 110
percent) and the other one low (e.g., 90
percent), normalization of the Hg mass
collected in the first two trap sections
using third section spike recoveries
could make it difficult for a pair of
sorbent traps to meet the relative
deviation (RD) specifications in
appendix K. In the example cited,
normalization of the data would cause
the Hg concentrations measured by the
traps to be adjusted by 10 percent in
opposite directions, i.e., one upward
and one downward. Thus, two Hg
concentrations that may have been in
close agreement without normalization
now might not be able to meet the RD
specifications. In view of this, EPA has
concluded that evaluating the spike
recovery data on a pass/fail basis
instead of using the percent recovery
values to adjust the emissions data is
more technically sound and is also
consistent with the way in which the
results of daily and quarterly QA
assessments of CEMS are interpreted.
Regarding the range of acceptable
third section spike recoveries, EPA is
1 On August 22, 2006, EPA proposed to amend
Appendix K to allow the data from a pair of sorbent
traps to be validated in cases where the third
section spike recovery from only one of the traps
meets the percent recovery specifications (see 71 FR
49275). EPA proposed to allow the results from the
trap that meets the specifications to be used for
reporting, provided that a single trap adjustment
factor (STAF) of 1.222 is applied. EPA is evaluating
the comments received on this proposal and
expects to publish the final rule in the summer of
2007.
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not changing the 75 to 125 percent
acceptance criteria. As previously
noted, early field experience with
appendix K monitoring systems has
demonstrated that spike recoveries
within this range are achievable.
However, recent appendix K data
indicate that more stringent acceptance
criteria may be justifiable. It appears
that there has been a marked
improvement in third section spike
recovery percentages. Recoveries in the
range from 85 to 115 percent are
consistently being achieved. If this trend
continues, EPA may propose to tighten
the spike recovery acceptance criteria in
a future rulemaking. Toward that end,
EPA will continue to collect and
evaluate third section spike recovery
data from appendix K monitoring
systems in the months ahead.
To effect these changes to appendix K,
section 11.5 is being removed and
reserved; section 10.4 is being revised;
Equations K–6 and K–7 are being
redesignated as Equations K–5 and K–6,
respectively; and the definition of ‘‘M*’’
in redesignated Equation K–5 is being
revised.
EPA is also revising appendix K to
allow the owner or operator to use other
types of gas flow meters besides the
conventional dry gas meter (DGM) to
quantify sample gas volume. Since the
publication of appendix K (see 70 FR
28695, May 18, 2005), numerous
requests have been received from the
regulated community to allow this
flexibility. In response to these requests,
EPA initiated an investigation of the
feasibility of replacing the DGM in a
sorbent trap monitoring system with a
thermal mass flow meter. As a result of
its investigation, EPA has concluded
that a properly calibrated thermal mass
flow meter can be at least as accurate as
a DGM. The mass flow meter is also a
more modern technology than the DGM;
since it has no moving parts, it may be
more reliable than a DGM for
continuous duty.
Having found one type of gas flow
meter that can measure as accurately as
a DGM, EPA is persuaded that there
may be other commercially available gas
flow meter technologies that are equally
capable and may be suitable for
appendix K applications. Accordingly,
EPA has decided that a performancebased approach, rather than a
prescriptive one, is more appropriate for
appendix K gas flow meters. Today’s
action allows the use of any type of gas
flow meter that is capable of accurately
measuring gas volumes to within 2
percent.
Section 9.2.2.1 of appendix K now
requires the manufacturer of the gas
flow meter to perform all necessary set-
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up, testing, programming, etc. of the
meter and to provide any necessary
instructions so that for the particular
field application, the meter will give an
accurate readout of dry gas volume in
units of standard cubic meters. Then,
prior to its initial use, the flow meter
must be calibrated at a minimum of
three settings covering the expected
range of sample flow rates for the
appendix K system. The initial
calibration may be performed either by
the manufacturer or by the end user.
The calibration of the gas flow meter
must be checked quarterly thereafter, at
an intermediate flow rate. For mass flow
meters, the initial three-point
calibration must be performed by using
either a compressed gas mixture
containing CO2, O2, and N2 in
proportions representative of the stack
gas composition or by using the actual
stack gas. However, when the initial
calibration is done with a compressed
gas mixture, the mass flow meter may
not be used until an additional on-site
calibration check of the flow meter at an
intermediate flow rate is performed and
passed, using the actual stack gas.
To calibrate the gas flow meter, the
owner or operator may either follow the
basic procedures in section 10.3 or
section 16 of Method 5 in appendix
A–3 of part 60 for calibration of dry gas
meters, or alternatively, may
temporarily install a reference gas flow
meter (RGFM) at the discharge of the
appendix K monitoring system while
the monitoring system is in operation
and make concurrent measurements of
dry stack gas volume with the RGFM
and the appendix K gas flow meter. If
the latter option is chosen, the RGFM
may either be a gas flow metering device
that has been calibrated according to
section 10.3.1 or section 16 of Method
5 or a NIST-traceable volumetric
calibration device with an accuracy of
±1 percent. Note that this alternative
calibration technique allows required
QA checks to be performed with little or
no disruption of the operation of the
sorbent trap monitoring system.
Regardless of which calibration
approach is used, a calibration factor,
Yi, must be obtained at each tested flow
rate, where Yi is the ratio of the volume
measured by the reference meter to the
volume measured by the flow meter
being calibrated. For the initial threepoint calibration, the three Yi values
must be averaged, and each individual
Yi must be within ± 0.02 of the average
value. The average value, Y, must then
be used to correct the gas volumes
measured by the gas flow meter. For
single-level calibration checks (e.g., the
quarterly checks performed for routine
QA), the Yi value obtained at the tested
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flow rate must be compared with the
current value of Y. If Yi differs from Y
by more than 5 percent, a full threepoint recalibration is then required to
determine a new Y value.
In this direct final action, the majority
of the revised rule provisions pertaining
to gas flow meters can be found in
sections 5.1.5 and 9.2 of appendix K.
Minor revisions to sections 7.2.3 and
7.2.5, Figure K–1, and Table K–1 are
being made to be consistent with the
changes to sections 5.1.5 and 9.2. In
several other places throughout part 75
and in the definition of ‘‘Sorbent trap
monitoring system’’ in part 72, the term
‘‘dry gas meter,’’ when used in reference
to a sorbent trap monitoring system, is
being replaced with the more general
term ‘‘gas flow meter.’’ Revisions to
section 1.5.2 of appendix B of part 75
will require the gas flow meter
calibration procedures and protocols for
periodic recalibration of reference gas
flow meters to be included in the QA
plan for the affected unit.
This direct final action, which
approves the use of two optional
methods (Methods 30A and 30B) for
determining total vapor phase Hg
emissions from stationary sources, is
being taken in response to numerous
public comments concerning the
desirability of allowing the use of these
types of methods to comply with the Hg
emission monitoring requirements of
the CAMR for electric utility steam
generating units. In the May 18, 2005
final rule (70 FR 28636), we
summarized the public comments that
we received regarding the use of an
instrumental method as an alternative to
the Ontario Hydro Method specified in
the proposed CAMR. As noted earlier in
this preamble, the commenters
primarily objected to the required use of
the Ontario Hydro Method as the
reference method for the RATAs of Hg
monitoring systems and expressed
concern about the complexities in the
method and the amount of time that is
required to perform the testing and to
receive the results. Commenters pointed
out that it could take days to complete
the testing and weeks to receive the
results from a laboratory. Commenters
claimed that for the cap and trade
program proposed under CAMR, these
delays could lead to significant
implementation problems with respect
to the timely reporting of emissions
data. Further, if a RATA should be
failed or invalidated (e.g., if fewer than
nine test runs meet the relative
deviation criterion for the paired
Ontario Hydro trains), data from the Hg
monitoring system would be invalidated
from the hour of the failed or
invalidated test until the hour of
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51499
completion of a successful RATA.
Conservatively high substitute data
values would have to be reported during
that entire time period. In our response
to those comments in the final CAMR
rule, we stated that the alternative use
of an instrumental method for the
required RATAs of Hg monitoring
systems and sorbent trap monitoring
systems is allowed by the final rule but
is subject to approval by the
Administrator. We also stated our
commitment to propose and promulgate
a Hg instrumental reference method
once sufficient supporting field test data
become available. We further stated that
‘‘A Hg instrumental reference method
for RATA testing is vastly preferable to
the Ontario Hydro Method and will
greatly facilitate the implementation of
a Hg cap-and-trade program.’’
Since promulgation of CAMR, we
have continued to communicate with
stakeholders interested in the Hg
monitoring requirements of the rule,
and we have come to more clearly
understand that it is of great interest to
the affected entities to have additional
reference method options available for
relative accuracy testing of installed Hg
monitoring systems as soon as possible.
Accordingly, at the end of 2005, we
began developing an instrumental test
method for Hg and solicited feedback
from the stakeholders on a working draft
of the method (referred to as PRE–009
at https://www.epa.gov/ttn/emc/
prelim.html). More recently, we have
been developing a viable sorbent trap
reference method. These efforts have
resulted in Methods 30A and 30B.
The general beneficial impacts of this
direct final rule to approve the two
optional Hg test methods and amend
targeted portions of 40 CFR parts 72 and
75 include: Allowing affected sources to
choose the use of an alternative to the
Ontario Hydro Method without the
administrative burden of applying for
Administrator approval on a case-bycase basis; providing the availability of
real-time RATA results (Method 30A);
reducing the overall RATA testing
times; reducing costs relative to the
Ontario Hydro Method; and providing
additional flexibility in appendix K
sorbent trap monitoring and backup
monitoring approaches. The two
optional methods being approved by
this direct final rule are considered to be
comparable to the Ontario Hydro
Method in terms of the quality of the
results produced. Over the last year,
EPA has collaborated with EPRI and
some of its members in a number of
field test programs that have confirmed
that the instrumental reference method
approved/established in this notice will
provide data comparable to or better
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than that of the ‘‘Ontario Hydro
Method.’’
Assuming we do not receive adverse
comment on this direct final rulemaking
and Methods 30A and 30B become final,
we plan to post information relevant to
Method 30A and 30B applications and
equipment advances on EPA’s Web site
at https://www.epa.gov/airmarkets.
VII. Statutory and Executive Order
Reviews
A. Executive Order 12866: Regulatory
Planning and Review
This action is not a ‘‘significant
regulatory action’’ under the terms of
Executive Order (EO) 12866 (58 FR
51735, October 4, 1993) and is therefore
not subject to review under the EO.
jlentini on PROD1PC65 with RULES2
B. Paperwork Reduction Act
This action does not impose an
information collection burden under the
provisions of the Paperwork Reduction
Act, 44 U.S.C. 3501 et seq. Burden
means the total time, effort, or financial
resources expended by persons to
generate, maintain, retain, or disclose or
provide information to or for a Federal
agency. This includes the time needed
to review instructions; develop, acquire,
install, and utilize technology and
systems for the purposes of collecting,
validating, and verifying information,
processing and maintaining
information, and disclosing and
providing information; adjust the
existing ways to comply with any
previously applicable instructions and
requirements; train personnel to be able
to respond to a collection of
information; search data sources;
complete and review the collection of
information; and transmit or otherwise
disclose the information.
An agency may not conduct or
sponsor, and a person is not required to
respond to a collection of information,
unless it displays a currently valid OMB
control number. The OMB control
numbers for EPA’s regulations in 40
CFR are listed in 40 CFR part 9.
C. Regulatory Flexibility Act
The Regulatory Flexibility Act (RFA)
generally requires an agency to prepare
a regulatory flexibility analysis of any
rule subject to notice and comment
rulemaking requirements under the
Administrative Procedure Act or any
other statute unless the agency certifies
that the rule will not have a significant
economic impact on a substantial
number of small entities. Small entities
include small businesses, small
organizations, and small governmental
jurisdictions.
For purposes of assessing the impacts
of today’s rule on small entities, small
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entity is defined as: (1) A small business
whose parent company has fewer than
100 or 1,000 employees, or fewer than
4 billion kilowatt-hr per year of
electricity usage, depending on the size
definition for the affected North
American Industry Classification
System code; (2) a small governmental
jurisdiction that is a government of a
city, county, town, school district or
special district with a population of less
than 50,000; and (3) a small
organization that is any not-for-profit
enterprise which is independently
owned and operated and is not
dominant in its field.
After considering the economic
impacts of today’s direct final rule on
small entities, I certify that this action
will not have a significant economic
impact on a substantial number of small
entities. This direct final rule will not
impose any requirements on small
entities because it does not impose any
additional regulatory requirements, but
rather provides clarification and
additional regulatory flexibilty.
D. Unfunded Mandates Reform Act
Title II of the Unfunded Mandates
Reform Act of 1995 (UMRA), Pub. L.
104–4, establishes requirements for
Federal agencies to assess the effects of
their regulatory actions on State, local,
and tribal governments and the private
sector. Under section 202 of the UMRA,
EPA generally must prepare a written
statement, including a cost-benefit
analysis, for proposed and final rules
with ‘‘Federal mandates’’ that may
result in expenditures to State, local,
and tribal governments, in the aggregate,
or to the private sector, of $100 million
or more in any one year. Before
promulgating an EPA rule for which a
written statement is needed, section 205
of the UMRA generally requires EPA to
identify and consider a reasonable
number of regulatory alternatives and
adopt the least costly, most costeffective or least burdensome alternative
that achieves the objectives of the rule.
The provisions of section 205 do not
apply when they are inconsistent with
applicable law. Moreover, section 205
allows EPA to adopt an alternative other
than the least costly, most cost-effective,
or least burdensome alternative if the
Administrator publishes with the final
rule an explanation why that alternative
was not adopted. Before EPA establishes
any regulatory requirements that may
significantly or uniquely affect small
governments, including tribal
governments, it must have developed
under section 203 of the UMRA a small
government agency plan. The plan must
provide for notifying potentially
affected small governments, enabling
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officials of affected small governments
to have meaningful and timely input in
the development of EPA regulatory
proposals with significant Federal
intergovernmental mandates, and
informing, educating, and advising
small governments on compliance with
the regulatory requirements.
EPA has determined that this direct
final rule does not contain a Federal
mandate that may result in expenditures
of $100 million or more for State, local,
and tribal governments in the aggregate,
or to the private sector in any 1 year, nor
does this rule significantly or uniquely
impact small governments, because it
contains no requirements that impose
new obligations upon them. Thus, this
direct final rule is not subject to the
requirements of sections 202 and 205 of
the UMRA.
E. Executive Order 13132: Federalism
Executive Order 13132, entitled
‘‘Federalism’’ (64 FR 43255, August 10,
1999), requires EPA to develop an
accountable process to ensure
‘‘meaningful and timely input by State
and local officials in the development of
regulatory policies that have federalism
implications.’’ ‘‘Policies that have
federalism implications’’ is defined in
the Executive Order to include
regulations that have ‘‘substantial direct
effects on the States, on the relationship
between the national government and
the States, or on the distribution of
power and responsibilities among the
various levels of government.’’
This direct final rule does not have
federalism implications. It will not have
substantial direct effects on the States,
on the relationship between the national
government and the States, or on the
distribution of power and
responsibilities among the various
levels of government, as specified in
Executive Order 13132. The use of these
methods is optional on the part of the
regulated entities listed. Thus,
Executive Order 13132 does not apply
to this direct final rule.
F. Executive Order 13175: Consultation
and Coordination With Indian Tribal
Governments
Executive Order 13175, entitled
‘‘Consultation and Coordination with
Indian Tribal Governments’’ (65 FR
67249, November 9, 2000), requires EPA
to develop an accountable process to
ensure ‘‘meaningful and timely input by
tribal officials in the development of
regulatory policies that have tribal
implications.’’ This direct final rule
does not have tribal implications, as
specified in Executive Order 13175. It
will not have substantial direct effects
on tribal governments, on the
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51501
EPA to provide Congress, through OMB,
explanations when the Agency decides
not to use available and applicable
voluntary consensus standards. This
rulemaking involves technical
standards. Consistent with the NTTAA,
EPA in a previous related rulemaking
(70 FR 28606, May 18, 2005) identified
an acceptable VCS for measuring Hg
emissions. The standard ASTM D6784–
02, Standard Test Method for Elemental,
Oxidized, Particle-Bound and Total
Mercury Gas Generated from Coal-Fired
Stationary sources (Ontario Hydro
Method) was cited in that final rule for
measuring Hg emissions. After today’s
action becomes effective, the Ontario
Hydro Method will remain an
acceptable method for measuring Hg
emissions.
cannot take effect until 60 days after it
is published in the Federal Register.
This action is not a ‘‘major rule’’ as
defined by 5 U.S.C. 804(2). This rule
will be effective on November 6, 2007.
40 CFR Part 75
Environmental protection,
Administrative practice and procedures,
Air pollution control, Continuous
emission monitors, Electric utilities,
Mercury, Test methods and procedures.
H. Executive Order 13211: Actions That
Significantly Affect Energy Supply,
Distribution, or Use
This rule is not subject to Executive
Order 13211, ‘‘Actions Concerning
Regulations That Significantly Affect
Energy Supply, Distribution, or Use’’ (66
FR 28355, May 22, 2001) because it is
not a significant regulatory action under
Executive Order 12866.
J. Executive Order 12898: Federal
Actions To Address Environmental
Justice in Minority Populations and
Low-Income Populations
Executive Order 12898 (59 FR 7629
(Feb. 16, 1994)) establishes federal
executive policy on environmental
justice. Its main provision directs
federal agencies, to the greatest extent
practicable and permitted by law, to
make environmental justice part of their
mission by identifying and addressing,
as appropriate, disproportionately high
and adverse human health or
environmental effects of their programs,
policies, and activities on minority
populations and low-income
populations in the United States.
EPA has determined that this direct
final rule will not have
disproportionately high and adverse
human health or environmental effects
on minority or low-income populations
because it does not affect the level of
protection provided to human health or
the environment. This direct final rule
does not affect or relax the control
measures on sources impacted by this
rule and therefore will not cause
emissions increases from these sources.
I. National Technology Transfer
Advancement Act
Section 12(d) of the National
Technology Transfer and Advancement
Act of 1995 (NTTAA), Public Law No.
104–113, section 12(d) (15 U.S.C. 272
note) directs EPA to use voluntary
consensus standards in its regulatory
activities unless to do so would be
inconsistent with applicable law or
otherwise impractical. Voluntary
consensus standards are technical
standards (e.g., materials specifications,
test methods, sampling procedures, and
business practices) that are developed or
adopted by voluntary consensus
standards bodies. The NTTAA directs
K. Congressional Review Act
The Congressional Review Act, 5
U.S.C. 801 et seq., as added by the Small
Business Regulatory Enforcement
Fairness Act of 1996, generally provides
that before a rule may take effect, the
Agency promulgating the rule must
submit a rule report, which includes a
copy of the rule, to each House of the
Congress and to the Comptroller General
of the United States. EPA will submit a
report containing this rule and other
required information to the U.S. Senate,
the U.S. House of Representatives, and
the Comptroller General of the United
States prior to publication of the rule in
the Federal Register. A major rule
relationship between the Federal
government and Indian tribes, or on the
distribution of power and
responsibilities between the Federal
government and Indian tribes. Thus,
Executive Order 13175 does not apply
to this final rule.
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G. Executive Order 13045: Protection of
Children From Environmental Health
and Safety Risks
Executive Order 13045: ‘‘Protection of
Children from Environmental Health
Risks and Safety Risks’’ (62 FR 19885,
April 23, 1997) applies to any rule that:
(1) Is determined to be ‘‘economically
significant’’ as defined under Executive
Order 12866, and (2) concerns an
environmental health or safety risk that
EPA has reason to believe may have a
disproportionate effect on children. If
the regulatory action meets both criteria,
the Agency must evaluate the
environmental health or safety effects of
the planned rule on children, and
explain why the planned regulation is
preferable to other potentially effective
and reasonably feasible alternatives
considered by the Agency. EPA
interprets Executive Order 13045 as
applying only to those regulatory
actions that are based on health or safety
risks, such that the analysis required
under section 5–501 of the Order has
the potential to influence the regulation.
This rule is not subject to Executive
Order 13045 because it does not
establish an environmental standard
intended to mitigate health or safety
risks.
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List of Subjects
40 CFR Part 60
Environmental protection,
Administrative practice and procedures,
Air pollution control, Continuous
emission monitors, Electric utilities,
Mercury, Test methods and procedures.
40 CFR Part 72
Environmental protection,
Administrative practice and procedures,
Air pollution control, Continuous
emission monitors, Electric utilities,
Mercury, Test methods and procedures.
Dated: August 17, 2007.
Stephen L. Johnson,
Administrator.
For the reasons set out in the
preamble, title 40, chapter I, parts 60,
72, and 75 of the Code of Federal
Regulations are amended as follows:
I
PART 60—STANDARDS OF
PERFORMANCE FOR NEW
STATIONARY SOURCES
1. The authority citation for part 60
continues to read as follows:
I
Authority: 42 U.S.C. 7401–7601.
Appendix A–8 [Amended]
2. Amend Appendix A–8 by revising
the heading and adding in numerical
order Methods 30A and 30B to read as
follows:
I
APPENDIX A–8 TO PART 60—TEST
METHODS 26 THROUGH 30B
*
*
*
*
*
Method 30A—Determination of Total Vapor
Phase Mercury Emissions From Stationary
Sources (Instrumental Analyzer Procedure)
1.0 Scope and Application
What Is Method 30A?
Method 30A is a procedure for measuring
total vapor phase mercury (Hg) emissions
from stationary sources using an
instrumental analyzer. This method is
particularly appropriate for performing
emissions testing and for conducting relative
accuracy test audits (RATAs) of mercury
continuous emissions monitoring systems
(Hg CEMS) and sorbent trap monitoring
systems at coal-fired combustion sources.
Quality assurance and quality control
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requirements are included to assure that you,
the tester, collect data of known and
acceptable quality for each testing site. This
method does not completely describe all
equipment, supplies, and sampling
procedures and analytical procedures you
will need but refers to other test methods for
some of the details. Therefore, to obtain
reliable results, you should also have a
thorough knowledge of these additional
methods which are also found in appendices
A–1 and A–3 to this part:
(a) Method 1—Sample and Velocity
Traverses for Stationary Sources.
(b) Method 4—Determination of Moisture
Content in Stack Gases.
Analyte
CAS No.
Elemental Hg (Hg0) ....................................................................
Oxidized Hg (Hg∂2) ...................................................................
1.2 Applicability. When is this method
required? Method 30A is offered as a
reference method for emission testing and for
RATAs of Hg CEMS and sorbent trap
monitoring systems at coal-fired boilers.
Method 30A may also be specified for other
source categories in the future, either by New
Source Performance Standards (NSPS),
National Emission Standards for Hazardous
Air Pollutants (NESHAP), emissions trading
programs, State Implementation Plans (SIP),
or operating permits that require
measurement of Hg concentrations in
stationary source emissions to determine
compliance with an applicable emission
standard or limit, or to conduct RATAs of Hg
CEMS and sorbent trap monitoring systems.
1.3 Data Quality Objectives (DQO). How
good must my collected data be? Method 30A
has been designed to provide data of high
and known quality for Hg emission testing
and for relative accuracy testing of Hg
monitoring systems including Hg CEMS and
sorbent trap monitoring systems. In these and
other applications, the principle objective is
to ensure the accuracy of the data at the
actual emission levels encountered. To meet
this objective, calibration standards prepared
according to an EPA traceability protocol
must be used and measurement system
performance tests are required.
2.0
Summary of Method
In this method, a sample of the effluent gas
is continuously extracted and conveyed to an
analyzer capable of measuring the total vapor
phase Hg concentration. Elemental and
oxidized mercury (i.e., Hg0 and Hg∂2) may
be measured separately or simultaneously
but, for purposes of this method, total vapor
phase Hg is the sum of Hg0 and Hg∂2. You
must meet the performance requirements of
this method (i.e., system calibration,
interference testing, dynamic spiking, and
system integrity/drift checks) to validate your
data. The dynamic spiking requirement is
deferred until January 1, 2009.
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3.0
Definitions
3.1 Calibration Curve means the
relationship between an analyzer’s response
to the injection of a series of calibration gases
and the actual concentrations of those gases.
3.2 Calibration Gas means a gas standard
containing Hg0 or HgCl2 at a known
concentration that is produced and certified
in accordance with an EPA traceability
protocol for certification of Hg calibration
standards.
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1.1 Analytes. What does this method
determine? This method is designed to
measure the mass concentration of total
vapor phase Hg in flue gas, which represents
the sum of elemental Hg (Hg0) and oxidized
forms of Hg (Hg∂2), in mass concentration
units of micrograms per cubic meter (µg/m3).
7439–97–6
Sensitivity
Typically <2% of Calibration Span.
(Same).
3.2.1 Zero Gas means a calibration gas
with a concentration that is below the level
detectable by the measurement system.
3.2.2 Low-Level Gas means a calibration
gas with a concentration that is 10 to 30
percent of the calibration span.
3.2.3 Mid-Level Gas means a calibration
gas with a concentration that is 40 to 60
percent of the calibration span.
3.2.4 High-Level Gas means a calibration
gas whose concentration is equal to the
calibration span.
3.3 Converter means a device that reduces
oxidized mercury (Hg∂2) to elemental
mercury (Hg0).
3.4 Calibration Span means the upper
limit of valid instrument response during
sampling. To the extent practicable the
measured emissions are to be between 10 and
100 percent of the selected calibration span
(i.e., the measured emissions should be
within the calibrated range determined by
the Low- and High-Level gas standards). It is
recommended that the calibration span be at
least twice the native concentration to
accommodate the dynamic spiking
procedure.
3.5 Centroidal Area means the central
area that has the same shape as the stack or
duct cross section and is no greater than one
percent of the stack or duct total crosssectional area.
3.6 Data Recorder means the equipment
that permanently records the concentrations
reported by the analyzer.
3.7 Drift Check means the test to
determine the difference between the
measurement system readings obtained in a
post-run system integrity check and the prior
pre-run system integrity check at a specific
calibration gas concentration level (i.e., zero,
mid-level, or high-level).
3.8 Dynamic Spiking means a procedure
in which a known mass or concentration of
vapor phase HgCl2 is injected into the probe
sample gas stream at a known flow rate, in
order to assess the effects of the flue gas
matrix on the accuracy of the measurement
system.
3.9 Gas Analyzer means the equipment
that detects the total vapor phase Hg being
measured and generates an output
proportional to its concentration.
3.10 Interference Test means the test to
detect analyzer responses to compounds
other than Hg, usually gases present in the
measured gas stream, that are not adequately
accounted for in the calibration procedure
and may cause measurement bias.
3.11 Measurement System means all of
the equipment used to determine the Hg
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concentration. The measurement system may
generally include the following major
subsystems: sample acquisition, Hg∂2 to Hg0
converter, sample transport, sample
conditioning, flow control/gas manifold, gas
analyzer, and data recorder.
3.12 Native Concentration means the
total vapor phase Hg concentration in the
effluent gas stream.
3.13 NIST means the National Institute of
Standards and Technology, located in
Gaithersburg, Maryland.
3.14 Response Time means the time it
takes for the measurement system, while
operating normally at its target sample flow
rate or dilution ratio, to respond to a known
step change in gas concentration (from a lowlevel to a high-level gas) and to read within
5 percent of the stable high-level gas
response.
3.15 Run means a series of gas samples
taken successively from the stack or duct. A
test normally consists of a specific number of
runs.
3.16 System Calibration Error means the
difference between the measured
concentration of a low-, mid-, or high-level
Hg0 calibration gas and the certified
concentration of the gas when it is
introduced in system calibration mode.
3.17 System Calibration Mode means
introducing the calibration gases into the
measurement system at the probe, upstream
of all sample conditioning components.
3.18 Test refers to the series of runs
required by the applicable regulation.
4.0
Interferences
Interferences will vary among instruments
and potential instrument-specific spectral
and matrix interferences must be evaluated
through the interference test and the dynamic
spiking tests.
5.0
Safety
What safety measures should I consider
when using this method?
This method may require you to work with
hazardous materials and in hazardous
conditions. You are encouraged to establish
safety procedures before using the method.
Among other precautions, you should
become familiar with the safety
recommendations in the gas analyzer user’s
manual. Occupational Safety and Health
Administration (OSHA) regulations
concerning use of compressed gas cylinders
and noxious gases may apply.
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6.0 Equipment and Supplies
6.1 What do I need for the measurement
system? This method is intended to be
applicable to multiple instrumental
technologies. You may use any equipment
and supplies that meet the following
specifications.
6.1.1 All wetted sampling system
components, including probe components
prior to the point at which the calibration gas
is introduced, must be chemically inert to all
Hg species. Materials such as perfluoroalkoxy
(PFA) TeflonTM, quartz, treated stainless steel
(SS) are examples of such materials. [Note:
These materials of construction are required
because components prior to the calibration
gas injection point are not included in the
system calibration error, system integrity,
and interference tests.]
6.1.2 The interference, system calibration
error, system integrity, drift and dynamic
spiking test criteria must all be met by the
system used.
6.1.3 The system must be capable of
measuring and controlling sample flow rate.
6.1.4 All system components prior to the
Hg∂2 to Hg0 converter must be maintained at
a sample temperature above the acid gas dew
point.
6.2 Measurement System Components.
Figure 30A–1 in Section 17.0 is an example
schematic of a Method 30A measurement
system.
6.2.1 Sample Probe. The probe must be
made of the appropriate materials as noted in
Section 6.1.1, heated when necessary (see
Section 6.1.4), configured with ports for
introduction of calibration and spiking gases,
and of sufficient length to traverse all of the
sample points.
6.2.2 Filter or Other Particulate Removal
Device. The filter or other particulate
removal device is considered to be a part of
the measurement system, must be made of
appropriate materials as noted in Section
6.1.1, and must be included in all system
tests.
6.2.3 Sample Line. The sample line that
connects the probe to the converter,
conditioning system and analyzer must be
made of appropriate materials as noted in
Section 6.1.1.
6.2.4 Conditioning Equipment. For dry
basis measurements, a condenser, dryer or
other suitable device is required to remove
moisture continuously from the sample gas.
Any equipment needed to heat the probe, or
sample line to avoid condensation prior to
the moisture removal component is also
required. For wet basis systems, you must
keep the sample above its dew point either
by: (1) Heating the sample line and all
sample transport components up to the inlet
of the analyzer (and, for hot-wet extractive
systems, also heating the analyzer) or (2) by
diluting the sample prior to analysis using a
dilution probe system. The components
required to do either of the above are
considered to be conditioning equipment.
6.2.5 Sampling Pump. A pump is needed
to push or pull the sample gas through the
system at a flow rate sufficient to minimize
the response time of the measurement
system. If a mechanical sample pump is used
and its surfaces are in contact with the
sample gas prior to detection, the pump must
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be leak free and must be constructed of a
material that is non-reactive to the gas being
sampled (see Section 6.1.1). For dilution-type
measurement systems, an ejector pump
(eductor) may be used to create a sufficient
vacuum that sample gas will be drawn
through a critical orifice at a constant rate.
The ejector pump may be constructed of any
material that is non-reactive to the gas being
sampled.
6.2.6 Calibration Gas System(s). One or
more systems may be needed to introduce
calibration gases into the measurement
system. A system should be able to flood the
sampling probe sufficiently to prevent entry
of gas from the effluent stream.
6.2.7 Dynamic Spiking Port. For the
purposes of the dynamic spiking procedure
described in Section 8.2.7, the measurement
system must be equipped with a port to allow
introduction of the dynamic spike gas stream
with the sample gas stream, at a point as
close as possible to the inlet of the probe so
as to ensure adequate mixing. The same port
used for system calibrations and calibration
error checks may be used for dynamic
spiking purposes.
6.2.8 Sample Gas Delivery. The sample
line may feed directly to a converter, to a bypass valve (for speciating systems), or to a
sample manifold. All valve and/or manifold
components must be made of material that is
non-reactive to the gas sampled and the
calibration gas, and must be configured to
safely discharge any excess gas.
6.2.9 Hg Analyzer. An instrument is
required that continuously measures the total
vapor phase Hg in the gas stream and meets
the applicable specifications in Section 13.0.
6.2.10 Data Recorder. A recorder, such as
a computerized data acquisition and
handling system (DAHS), digital recorder,
strip chart, or data logger, is required for
recording measurement data.
6.3 Moisture Measurement System. If
correction of the measured Hg emissions for
moisture is required (see Section 8.5), either
Method 4 in appendix A–3 to this part or
other moisture measurement methods
approved by the Administrator will be
needed to measure stack gas moisture
content.
7.0 Reagents and Standards
7.1 Calibration Gases. What calibration
gases do I need? You will need calibration
gases of known concentrations of Hg0 and
HgCl2. Special reagents and equipment may
be required to prepare the HgCl2 gas
standards (e.g., a NIST-traceable solution of
HgCl2 and a gas generator equipped with
mass flow controllers).
The following calibration gas
concentrations are required:
7.1.1 High-Level Gas. Equal to the
selected calibration span.
7.1.2 Mid-Level Gas. 40 to 60 percent of
the calibration span.
7.1.3 Low-Level Gas. 10 to 30 percent of
the calibration span.
7.1.4 Zero Gas. No detectable Hg.
7.1.5 Dynamic Spike Gas. The exact
concentration of the HgCl2 calibration gas
used to perform the pre-test dynamic spiking
procedure described in Section 8.2.7 depends
on the native Hg concentration in the stack
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The spike gas must produce a spiked sample
concentration above the native concentration,
as specified in Section 8.2.7.2.2.
7.2 Interference Test. What reagents do I
need for the interference test? Use the
appropriate test gases listed in Table 30A–3
in Section 17.0 (i.e., the potential interferents
for the source to be tested, as identified by
the instrument manufacturer) to conduct the
interference check. These gases need not be
of protocol gas quality.
8.0 Sample Collection
Emission Test Procedure
Figure 30A–2 in Section 17.0 presents an
overview of the test procedures required by
this method. Since you may choose different
options to comply with certain performance
criteria, you must identify the specific
options and associated frequencies you select
and document your results in regard to the
performance criteria.
8.1 Sample Point Selection. What
sampling site and sampling points do I
select?
8.1.1 When this method is used solely for
Hg emission testing (e.g., to determine
compliance with an emission standard or
limit), use twelve sampling points located
according to Table 1–1 or Table 1–2 of
Method 1 in appendix A–1 to this part.
Alternatively, you may conduct a
stratification test as described in Section
8.1.3 to determine the number and location
of the sampling points.
8.1.2 When this method is used for
relative accuracy testing of a Hg CEMS or
sorbent trap monitoring system, follow the
sampling site selection and sampling point
layout procedures for gas monitor RATA
testing described in the appropriate
performance specification or applicable
regulation (e.g., Performance Specification 2,
section 8.1.3 of appendix B to this part or
section 6.5.6 of appendix A to part 75 of this
chapter), with one exception. If you elect to
perform stratification testing as part of the
sampling point selection process, perform the
testing in accordance with Section 8.1.3 of
this method (see also ‘‘Summary Table of
QA/QC Requirements’’ in Section 9.0).
8.1.3 Determination of Stratification. If
you elect to perform stratification testing as
part of the sampling point selection process
and the test results show your effluent gas
stream to be unstratified or minimally
stratified, you may be allowed to sample at
fewer points or at different points than would
otherwise be required.
8.1.3.1 Test Procedure. To test for
stratification, use a probe of appropriate
length to measure the total vapor phase Hg
concentration at twelve traverse points
located according to Table 1–1 or Table 1–
2 of Method 1 in appendix A–1 to this part.
Alternatively, for a sampling location where
stratification is expected (e.g., after a wet
scrubber or at a point where dissimilar gas
streams are combined together), if a 12-point
Hg stratification test has been previously
performed at that location and the results of
the test showed the location to be minimally
stratified or unstratified according to the
criteria in section 8.1.3.2, you may perform
an abbreviated 3-point or 6-point Hg
stratification test at the points specified in
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section 6.5.6.2(a) of appendix A to part 75 of
this chapter in lieu of performing the 12point test. Sample for a minimum of twice
the system response time (see Section 8.2.6)
at each traverse point. Calculate the
individual point and mean Hg
concentrations.
8.1.3.2 Acceptance Criteria and Sampling
Point Location.
8.1.3.2.1 If the Hg concentration at each
traverse point differs from the mean
concentration for all traverse points by no
more than: (a) ±5 percent of the mean
concentration; or (b) ±0.2 µg/m3 (whichever
is less restrictive), the gas stream is
considered to be unstratified and you may
collect samples from a single point that most
closely matches the mean.
8.1.3.2.2 If the 5 percent or 0.2 µg/m3
criterion in Section 8.1.3.2.1 is not met, but
the Hg concentration at each traverse point
differs from the mean concentration for all
traverse points by no more than: (a)±10
percent of the mean; or (b)±0.5 µg/m3
(whichever is less restrictive), the gas stream
is considered to be minimally stratified, and
you may take samples from three points,
provided the points are located on the
measurement line exhibiting the highest
average Hg concentration during the
stratification test. If the stack diameter (or
equivalent diameter, for a rectangular stack
or duct) is greater than 2.4 meters (7.8 ft),
locate the three sampling points at 0.4, 1.0,
and 2.0 meters from the stack or duct wall.
Alternatively, if a RATA required by part 75
of this chapter is being conducted, you may
locate the three points at 4.4, 14.6, and 29.6
percent of the duct diameter, in accordance
with Method 1 in appendix A–1 to this part.
For stack or duct diameters of 2.4 meters (7.8
ft) or less, locate the three sampling points
at 16.7, 50.0, and 83.3 percent of the
measurement line.
8.1.3.2.3 If the gas stream is found to be
stratified because the 10 percent or 0.5 µg/m3
criterion in Section 8.1.3.2.2 is not met, then
either locate three sampling points at 16.7,
50.0, and 83.3 percent of the measurement
line that exhibited the highest average Hg
concentration during the stratification test, or
locate twelve traverse points for the test in
accordance with Table 1–1 or Table 1–2 of
Method 1 in appendix A–1 to this part; or,
if a RATA required by part 75 of this chapter
is being conducted, locate six Method 1
points along the measurement line that
exhibited the highest average Hg
concentration.
8.1.3.3 Temporal Variations. Temporal
variations in the source Hg concentration
during a stratification test may complicate
the determination of stratification. If
temporal variations are a concern, you may
use the following procedure to normalize the
stratification test data. A second Hg
measurement system, i.e., either an installed
Hg CEMS or another Method 30A system, is
required to perform this procedure. Position
the sampling probe of the second Hg
measurement system at a fixed point in the
stack or duct, at least one meter from the
stack or duct wall. Then, each time that the
Hg concentration is measured at one of the
stratification test points, make a concurrent
measurement of Hg concentration at the fixed
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point. Normalize the Hg concentration
measured at each traverse point, by
multiplying it by the ratio of CF,avg to CF,
where CF is the corresponding fixed-point Hg
concentration measurement, and CF,avg is the
average of all of the fixed-point
measurements over the duration of the
stratification test. Evaluate the results of the
stratification test according to section 8.1.3.2,
using the normalized Hg concentrations.
8.1.3.4 Stratification Testing Exemption.
Stratification testing need not be performed
at a test location where it would otherwise
be required to justify using fewer sample
points or different sample points, if the
owner or operator documents that the Hg
concentration in the stack gas is expected to
be 3 µg/m3 or less at the time of a Hg
monitoring system RATA or an Hg emissions
test. To demonstrate that a particular test
location qualifies for the stratification testing
exemption, representative Hg emissions data
must be collected just prior to the RATA or
emissions test. At least one hour of Hg
concentration data is required for the
demonstration. The data used for the
demonstration shall be recorded at process
operating conditions that closely
approximate the operating conditions that
will exist during the RATA or emissions test.
It is recommended that collection of the
demonstration data be integrated with the onsite pretest procedures required by the
reference method being used for the RATA or
emissions test (whether this method or
another approved Hg reference method is
used). Quality-assured data from an installed
Hg monitoring system may also be used for
the demonstration. If a particular test
location qualifies for the stratification testing
exemption, sampling shall be performed at
three points, as described in section 8.1.3.2.2
of this method. The owner or operator shall
fully document the method used to collect
the demonstration data and shall keep this
documentation on file with the data from the
associated RATA or Hg emissions test.
8.1.3.5 Interim Alternative Stratification
Test Procedures. In the time period between
the effective date of this method and January
1, 2009, you may follow one of the following
two procedures. Substitute a stratification
test for sulfur dioxide (SO2) for the Hg
stratification test described in section 8.1.3.1.
If this option is chosen, follow the test
procedures in section 6.5.6.1 of appendix A
to part 75 of this chapter. Evaluate the test
results and determine the sampling point
locations according to section 6.5.6.3 of
appendix A to part 75 of this chapter. If the
sampling location is found to be minimally
stratified or unstratified for SO2, it shall be
considered minimally stratified or
unstratified for Hg. Alternatively, you may
forgo stratification testing, assume the gas
stream is minimally stratified, and sample at
three points as described in section 8.1.3.2.2
of this method.
8.2 Initial Measurement System
Performance Tests. What initial performance
criteria must my system meet before I begin
sampling? Before measuring emissions,
perform the following procedures:
(a) Interference Test;
(b) Calibration Gas Verification;
(c) Measurement System Preparation;
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(d) 3-Point System Calibration Error Test;
(e) System Integrity Check;
(f) Measurement System Response Time
Test; and
(g) Dynamic Spiking Test.
8.2.1 Interference Test (Optional). Your
measurement system should be free of known
interferences. It is recommended that you
conduct this interference test of your
measurement system prior to its initial use in
the field to verify that the candidate test
instrument is free from inherent biases or
interferences resulting from common
combustion emission constituents. If you
have multiple measurement systems with
components of the same make and model
numbers, you need only perform this
interference check on one system and you
may also rely on an interference test
conducted by the manufacturer on a system
having components of the same make and
model(s) of the system that you use. The
interference test procedure is found in
Section 8.6 of this method.
8.2.2 Calibration Gas Verification. How
must I verify the concentrations of my
calibration gases?
8.2.2.1 Cylinder Gas Standards. When
cylinder gas standards are used for Hg0,
obtain a certificate from the gas manufacturer
and confirm that the documentation includes
all information required by an EPA
traceability protocol (see Section 16).
Confirm that the manufacturer certification is
complete and current. Ensure that the
calibration gas certifications have not
expired.
8.2.2.2 Other Calibration Standards. All
other calibration standards for HgCl2 and
Hg0, such as gas generators, must meet the
requirements of an EPA traceability protocol
(see Section 16), and the certification
procedures must be fully documented in the
test report.
8.2.2.3 Calibration Span. Select the
calibration span (i.e., high-level gas
concentration) so that the measured source
emissions are 10 to 100 percent of the
calibration span. This requirement is waived
for applications in which the Hg
concentrations are consistently below 1 µg/
m3; however, the calibration span for these
low-concentration applications shall not
exceed 5 µg/m3.
8.2.3 Measurement System Preparation.
How do I prepare my measurement system
for use? Assemble, prepare, and precondition
the measurement system according to your
standard operating procedure. Adjust the
system to achieve the correct sampling rate
or dilution ratio (as applicable). Then,
conduct a 3-point system calibration error
test using Hg0 as described in Section 8.2.4,
an initial system integrity check using HgCl2
and a zero gas as described in Section 8.2.5,
and a pre-test dynamic spiking test as
described in Section 8.2.7.
8.2.4 System Calibration Error Test.
Conduct a 3-point system calibration error
test before the first test run. Use Hg0
standards for this test. Introduce the low-,
mid-, and high-level calibration gases in any
order, in system calibration mode, unless you
desire to determine the system response time
during this test, in which case, inject the
gases such that the high-level injection
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directly follows the low-level injection. For
non-dilution systems, you may adjust the
system to maintain the correct flow rate at
the analyzer during the test, but you may not
make adjustments for any other purpose. For
dilution systems, you must operate the
measurement system at the appropriate
dilution ratio during all system calibration
error checks, and you may make only the
adjustments necessary to maintain the proper
ratio. After each gas injection, wait until a
stable response has been obtained. Record
the analyzer’s final, stable response to each
calibration gas on a form similar to Table
30A–1 in Section 17.0. For each calibration
gas, calculate the system calibration error
using Equation 30A–1 in Section 12.2. The
calibration error specification in Section 13.1
must be met for the low-, mid-, and highlevel gases. If the calibration error
specification is not met for all three gases,
take corrective action and repeat the test
until an acceptable 3-point calibration is
achieved.
8.2.5 System Integrity Check. Perform a
two-point system integrity check before the
first test run. Use the zero gas and either the
mid- or high-level HgCl2 calibration gas for
the check, whichever one best represents the
total vapor phase Hg concentration levels in
the stack. Record the data on a form similar
to Table 30A–2 in Section 17.0. The system
integrity check specification in Section 13.2
must be met for both the zero gas and the
mid- or high-level gas. If the system integrity
specification is not met for both gases, take
corrective action and repeat the test until an
acceptable system integrity check is
achieved.
8.2.6 Measurement System Response
Time. The measurement system response
time is used to determine the minimum
sampling time for each sampling point and
is equal to the time that is required for the
measured Hg concentration to increase from
the stable low-level calibration gas response
to a value within 5 percent of the stable highlevel calibration gas response during the
system calibration error test in Section 8.2.4.
Round off the measured system response
time to the nearest minute.
8.2.7 Dynamic Spiking Test. You must
perform dynamic spiking prior to the first
test run to validate your test data. The
purpose of this procedure is to demonstrate
that the site-specific flue gas matrix does not
adversely affect the accuracy of the
measurement system. The specifications in
Section 13.5 must be met to validate your
data. If these specifications are not met for
the pre-test dynamic spiking, you may not
proceed with the test until satisfactory results
are obtained. For the time period between the
effective date of this method and January 1,
2009, the dynamic spiking requirement is
waived.
8.2.7.1 How do I perform dynamic
spiking? Dynamic spiking is a gas phase
application of the method of standard
additions, which involves injecting a known
quantity of Hg into the measurement system
upstream of all sample conditioning
components, similar to system calibration
mode, except the probe is not flooded and
the resulting sample stream includes both
effluent gas and the spike gas. You must
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follow a written procedure that details how
the spike is added to the system, how the
spike dilution factor (DF) is measured, and
how the Hg concentration data are collected
and processed.
8.2.7.2 Spiking Procedure Requirements.
8.2.7.2.1 Spiking Gas Requirements. The
spike gas must also be a HgCl2 calibration gas
certified by an EPA traceability protocol. You
must choose concentrations that can produce
the target levels while being injected at a
volumetric flow rate that is ≤20 percent of the
total volumetric flow rate through the
measurement system (i.e., sample flow rate
plus spike gas flow rate).
8.2.7.2.2 Target Spiking Level. The target
level for spiking must be 150 to 200 percent
of the native Hg concentration; however, if
the native Hg concentration is <1 µg/m3, set
the target level to add between 1 and 4 µg/
m3 Hg∂2 to the native concentration. Use
Equation 30A–5 in Section 12.5 to calculate
the acceptable range of spike gas
concentrations at the target level. Then select
a spike gas concentration in that range.
8.2.7.2.3 Spike Injections. You must
inject spikes in such a manner that the
spiking does not alter the total volumetric
sample system flow rate and dilution ratio (if
applicable). You must collect at least 3 data
points, and the relative standard deviation
(RSD) specification in Section 13.5 must be
met. Each data point represents a single spike
injection, and pre- and post-injection
measurements of the native Hg concentration
(or diluted native concentration, as
applicable) are required for each spike
injection.
8.2.7.2.4 Spike Dilution Factor (DF). For
each spike injection, DF, the dilution factor
must be determined. DF is the ratio of the
total volumetric flow rate of gas through the
measurement system to the spike gas flow
rate. This factor must be ≥5. The spiking
mass balance calculation is directly
dependent on the accuracy of the DF
determination. As a result, high accuracy
total volumetric flow rate and spike gas
flowrate measurements are required. These
flow rates may be determined by direct or
indirect measurement. Calibrated flow
meters, venturies, orifices or tracer gas
measurements are examples of potential flow
measurement techniques.
8.2.7.2.5 Concentrations. The
measurement system must record total vapor
phase Hg concentrations continuously during
the dynamic spiking procedure. It is possible
that dynamic spiking at a level close to 200
percent of the native Hg concentration may
cause the measured Hg concentration to
exceed the calibration span value. Avoid this
by choosing a lower spiking level or by
recalibration at a higher span. The
measurements shall not exceed 120 percent
of the calibration span. The ‘‘baseline’’
measurements made between spikes may
represent the native Hg concentration (if
spike gas flow is stopped between injections)
or the native Hg concentration diluted by
blank or carrier gas flowing at the same rate
as the spike gas (if gas flow cannot be
stopped between injections). Each baseline
measurement must include at least 4 readings
or 1 minute (whichever is greater) of stable
responses. Use Equation 30A–10 or 30A–11
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51505
in Section 12.10 (as applicable) to convert
baseline measurements to native
concentration.
8.2.7.2.6 Recovery. Calculate spike
recoveries using Equation 30A–7 in Section
12.7. Mass recoveries may be calculated from
stable responses based on injected mass
flows or from integrated response peaks
based on total mass injected. Calculate the
mean and RSD for the three (or more) spike
injections and compare to the specifications
in Section 13.5.
8.2.7.2.7 Error Adjustment Option. You
may adjust the measurement data collected
during dynamic spiking for the system
calibration error using Equation 30A–3 in
Section 12. To do this, perform the initial
system integrity check prior to the dynamic
spiking test, and perform another system
integrity check following the dynamic
spiking test and before the first test run. If
you choose this option, you must apply
Equation 30A–3 to both the spiked sample
concentration measurement (Css) and the
baseline or native concentration
measurement (Cnative), each substituted in
place of Cavg in the equation.
8.2.7.3 Example Spiking Procedure Using
a Hot Vapor Calibration Source Generator.
(a) Introduce the spike gas into the probe
using a hot vapor calibration source generator
and a solution of HgCl2 in dilute HC1 and
HNO3. The calibrator uses a mass flow
controller (accurate within 2 percent) to
measure the gas flow, and the solution feed
is measured using a top-loading balance
accurate to 0.01g. The challenges of injecting
oxidized Hg may make it impractical to stop
the flow of gas between spike injections. In
this case, operate the hot vapor calibration
source generator continuously during the
spiking procedure, swapping blank solutions
for HgCl2 solutions when switching between
spiking and baseline measurements.
(b) If applicable, monitor the measurement
system to make sure the total sampling
system flow rate and the sample dilution
ratio do not change during this procedure.
Record all data on a data sheet similar to
Table 30A–5 in Section 17.0. If the Hg
measurement system design makes it
impractical to measure the total volumetric
flow rate through the system, use a spike gas
that includes a tracer for measuring the
dilution factor, DF (see Equation 30A–9 in
Section 12.9). Allow the measurements to
stabilize between each spike injection,
average the pre- and post-injection baseline
measurements, and calculate the native
concentration. If this measurement shifts by
more than 5 percent during any injection, it
may be necessary to discard that data point
and repeat the injection to achieve the
required RSD among the injections. If the
spikes persistently show poor repeatability,
or if the recoveries are not within the range
specified in Section 13.5, take corrective
action.
8.2.8 Run Validation. How do I confirm
that each run I conduct is valid?
8.2.8.1 System Integrity Checks.
(a) Before and after each test run, perform
a two-point system integrity check using the
same procedure as the initial system integrity
check described in Section 8.2.5. You may
use data from that initial system integrity
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check as the pre-run data for the first test run,
provided it is the most recent system
integrity check done before the first run. You
may also use the results of a successful postrun system integrity check as the pre-run
data for the next test run. Do not make any
adjustments to the measurement system
during these checks, other than to maintain
the target calibration gas flow rate and the
proper dilution ratio.
(b) As a time-saving alternative, you may,
at the risk of invalidating multiple test runs,
skip one or more integrity checks during a
test day. Provided there have been no autocalibrations or other instrument alterations, a
single integrity check may suffice as a postrun check to validate (or invalidate) as many
consecutive test runs as can be completed
during a single test day. All subsequent test
days must begin with a pre-run system
integrity check subject to the same
performance criteria and corrective action
requirements as a post-run system integrity
check.
(c) Each system integrity check must meet
the criteria for system integrity checks in
Section 13.2. If a post-run system integrity
check is failed, all test runs since the last
passed system integrity check are invalid. If
a post-run or a pre-run system integrity check
is failed, you must take corrective action and
pass another 3-point Hg0 system calibration
error test (Section 8.2.4) followed by another
system integrity check before conducting any
additional test runs. Record the results of the
pre- and post-run system integrity checks on
a form similar to Table 30A–2 in Section
17.0.
8.2.8.2 Drift Check. Using the data from
the successful pre- and post-run system
integrity checks, calculate the zero and
upscale drift, using Equation 30A–2 in
Section 12.3. Exceeding the Section 13.3
specification does not invalidate the run, but
corrective action must be taken and a new 3point Hg0 system calibration error test and a
system integrity check must be passed before
any more runs are made.
8.3 Dilution-Type Systems—Special
Considerations. When a dilution-type
measurement system is used, there are three
important considerations that must be taken
into account to ensure the quality of the
emissions data. First, the critical orifice size
and dilution ratio must be selected properly
so that the sample dew point will be below
the sample line and analyzer temperatures.
Second, a high-quality, accurate dilution
controller must be used to maintain the
correct dilution ratio during sampling. The
dilution controller should be capable of
monitoring the dilution air pressure, orifice
upstream pressure, eductor vacuum, and
sample flow rates. Third, differences between
the molecular weight of calibration gas
mixtures, dilution air, and the stack gas
molecular weight must be considered
because these can affect the dilution ratio
and introduce measurement bias.
8.4 Sampling.
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(a) Position the probe at the first sampling
point. Allow the system to flush and
equilibrate for at least two times the
measurement system response time before
recording any data. Then, traverse and record
measurements at all required sampling
points. Sample at each traverse point for an
equal length of time, maintaining the
appropriate sample flow rate or dilution ratio
(as applicable). For all Hg instrumental
method systems, the minimum sampling
time at each sampling point must be at least
two times the system response time, but not
less than 10 minutes. For concentrating
systems, the minimum sampling time must
also include at least 4 concentration
measurement cycles.
(b) After recording data for the appropriate
period of time at the first traverse point, you
may move the sample probe to the next point
and continue recording, omitting the
requirement to allow the system to
equilibrate for two times the system response
time before recording data at the subsequent
traverse points. You must, however, sample
at this and all subsequent traverse points for
the required minimum amount of time
specified in this section. If you must remove
the probe from the stack for any reason, you
must again allow the sampling system to
equilibrate for at least two times the system
response time prior to resuming data
recording.
(c) If at any point the measured Hg
concentration exceeds the calibration span
value, you must at a minimum identify and
report this as a deviation from the method.
Depending on the data quality objectives of
the test, this event may require corrective
action before proceeding. If the average Hg
concentration for any run exceeds the
calibration span value, the run is invalidated.
8.5 Moisture Correction. If the moisture
basis (wet or dry) of the measurements made
with this method is different from the
moisture basis of either: (1) The applicable
emission limit; or (2) a Hg CEMS or sorbent
trap monitoring system being evaluated for
relative accuracy, you must determine the
moisture content of the flue gas and correct
the measured gas concentrations to a dry
basis using Method 4 in appendix A–3 of this
part or other appropriate methods, subject to
the approval of the Administrator.
8.6 Optional Interference Test Procedure.
(a) Select an appropriate calibration span
that reflects the source(s) to be tested and
perform the interference check at 40 percent
of the lowest calibration span value
anticipated, e.g., 10 µg/m3. Alternatively,
successfully conducting the interference test
at an absolute Hg concentration of 2 µg/m3
will demonstrate performance for an
equivalent calibration span of 5 µg/m3, the
lowest calibration span allowed for Method
30A testing. Therefore, performing the
interference test at the 2 µ/m3 level will serve
to demonstrate acceptable performance for all
calibration spans greater than or equal to 5
µg/m3.
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(b) Introduce the interference test gases
listed in Table 30A–3 in Section 17.0 into the
measurement system separately or as a
mixture. The interference test gases HCl and
NO must be introduced as a mixture. The
interference test gases must be introduced
into the sampling system at the probe such
that the interference gas mixtures pass
through all filters, scrubbers, conditioners,
and other components as would be
configured for normal sampling.
(c) The interference test must be performed
using HgCl2, and each interference test gas
(or gas mixture) must be evaluated in
triplicate. This is accomplished by measuring
the Hg response first with only the HgCl2 gas
present and then when adding the
interference test gas(es) while maintaining
the HgCl2 concentration of the test stream
constant. It is important that the equipment
used to conduct the interference test be of
sufficient quality so as to be capable of
blending the HgCl2 and interference gases
while maintaining the Hg concentration
constant. Gas blending system or manifolds
may be used.
(d) The duration of each test should be for
a sufficient period of time to ensure the Hg
measurement system surfaces are
conditioned and a stable output is obtained.
Measure the Hg response of the analyzer to
these gases in µg/m3. Record the responses
and determine the overall interference
response using Table 30A–4 in Section 17.0
and the equations presented in Section 12.11.
The specification in Section 13.4 must be
met.
(e) A copy of these data, including the date
completed and a signed certification, must be
included with each test report. The intent of
this test is that the interference test results
are intended to be valid for the life of the
system. As a result, the Hg measurement
system should be operated and tested in a
configuration consistent with the
configuration that will be used for field
applications. However, if the system used for
field testing is not consistent with the system
that was interference-tested, the interference
test must be repeated before it is used for any
field applications. Examples of such
conditions include, but are not limited to:
major changes in dilution ratio (for dilution
based systems), changes in catalyst materials,
changes in filtering device design or
materials, changes in probe design or
configuration, and changes in gas
conditioning materials or approaches.
9.0
Quality Control
What quality control measures must I take?
The table which follows is a summary of
the mandatory, suggested, and alternative
quality assurance and quality control
measures and the associated frequency and
acceptance criteria. All of the QC data, along
with the run data, must be documented and
included in the test report.
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51507
SUMMARY TABLE OF QA/QC REQUIREMENTS
Process or element
QA/QC specification
Acceptance criteria
S ...............
Identify Data User .........
........................................
M ..............
Analyzer Design ............
Analyzer range ..............
S ...............
........................................
........................................
Analyzer resolution or
sensitivity.
Interference response ...
Regulatory Agency or other primary end user of
data.
Sufficiently > high-level gas to allow determination of system calibration error.
< 2.0 % of full-scale range ....................................
S ...............
M ..............
M ..............
Calibration Gases ..........
........................................
Traceability protocol ......
High-level Hg0 gas ........
Overall response ≤ 3% of calibration span ...........
Alternatively, overall response ≤ 0.3 µg/m3.
Validation of concentration required.
Equal to the calibration span ................................
M ..............
........................................
Mid-level Hg0 gas ..........
40 to 60% of calibration span ...............................
M ..............
........................................
Low-level Hg0 gas .........
10 to 30% of calibration span ...............................
M ..............
........................................
High-level HgCl2 gas .....
Equal to the calibration span ................................
M ..............
........................................
Mid-level HgCl2 ..............
40 to 60% of calibration span ...............................
M ..............
........................................
Zero gas ........................
................................................................................
M ..............
........................................
Dynamic spike gas
(Cnative ≥ 1 µg/m3).
M ..............
........................................
Dynamic spike gas
(Cnative < 1 µg/m3).
S ...............
M ..............
Data Recorder Design ...
Sample Extraction .........
Data resolution ..............
Probe material ...............
M ..............
Sample Extraction .........
Probe, filter and sample
line temperature.
M ..............
Sample Extraction .........
S ...............
M ..............
M ..............
Sample Extraction .........
Sample Extraction .........
Particulate Removal ......
Calibration valve material.
Sample pump material ..
Manifold material ...........
Filter inertness ...............
A high-concentration HgCl2 gas, used to produce
a spiked sample concentration that is 150 to
200% of the native concentration.
A high-concentration HgCl2 gas, used to produce
a spiked sample concentration that is 1 to 2
µg/m3 above the native concentration.
≤ 0.5% of full-scale ................................................
Inert to sample constituents (e.g., PFA Teflon, or
quartz if stack > 500 °F).
For dry-basis analyzers, keep sample above the
dew point, by heating prior to moisture removal.
For wet-basis analyzers, keep sample above dew
point at all times, by heating or dilution.
Inert to sample constituents (e.g., PFA Teflon or
PFA Teflon coated).
Inert to sample constituents ..................................
Inert to sample constituents ..................................
Pass calibration error check ..................................
M ..............
System Calibration Performance.
System calibration error
(CE) test.
M ..............
System Calibration Performance.
System integrity check ..
M ..............
System Performance .....
System response time ...
Used to determine minimum sampling time per
point.
M ..............
System Performance .....
Drift ................................
M ..............
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Status 1
System Performance .....
Minimum sampling time
M ..............
System Performance .....
Percentage spike recovery and relative standard deviation.
≤ 3.0% of calibration span for the zero and midor high-level gas.
Alternative specification: ≤ 0.3 µg/m3 absolute difference between pre- and post-run system calibration error percentages..
The greater of two times the system response
time or 10 minutes. Concentrating systems
must also include at least 4 cycles.
Percentage spike recovery, at the target level:
100 ± 10%.
Relative standard deviation: ≤ 5 percent ...............
Alternative specification: absolute difference between calculated and measured spike values
≤ 0.5 µg/m3.
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CE ≤ 5.0 % of the calibration span for the low-,
mid-or high-level Hg0 calibration gas.
Alternative specification: ≤ 0.5 µg/m3 absolute difference between system response and reference value.
Error ≤ 5.0% of the calibration span for the zero
and mid- or high-level HgCl2 calibration gas.
Alternative specification: ≤ 0.5 µg/m3 absolute difference between system response and reference value.
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Before designing test.
Manufacturer design.
Each calibration error
test.
Each calibration error
test.
Each calibration error
test.
Each system integrity
check (if it better represents Cnative than
the mid level gas).
Each system gas integrity check (if it better
represents Cnative than
the high level gas).
Each system integrity
check.
Pre-test; dynamic spiking not required until
1/1/09.
Pre-test; dynamic spiking not required until
1/1/09.
Manufacturer design.
Each run.
Each run.
Each test.
Each test.
Each test.
Each calibration error
check.
Before initial run and
after a failed system
integrity check or drift
test.
Before initial run, after
each run, at the beginning of subsequent
test days, and after a
failed system integrity
check or drift test.
During initial 3-point system calibration error
test.
At least once per test
day.
Each sampling point.
Before initial dynamic
spiking not required
until 1/1/09.
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SUMMARY TABLE OF QA/QC REQUIREMENTS—Continued
Status 1
Process or element
QA/QC specification
Acceptance criteria
M ..............
Sample Point Selection
Number and Location of
Sample Points.
........................................
........................................
........................................
........................................
........................................
........................................
........................................
........................................
........................................
........................................
........................................
........................................
Sample Point Selection
Stratification Test (see
Section 8.1.3).
........................................
........................................
For emission testing applications, use 12 points,
located according to Method 1 in appendix A–1
to this part, unless the results of a stratification
test allow fewer points to be used.
For Part 60 RATAs, follow the procedures in Performance Specification 2, section 8.1.3, and for
Part 75 RATAs, follow the procedures in section 6.5.6 of appendix A to Part 75. That is:
• At any test location, you may use 3 sample
points located at 16.7, 50.0, and 83.3% of a
‘‘long’’ measurement line passing through the
centroidal area; or
• At any test location, you may use 6 sample
points along a diameter, located according to
Method 1 (Part 75 RATAs, only); or
• At a location where stratification is not expected and the measurement line is > 2.4 m
(7.8 ft), you may use 3 sample points located
along a ‘‘short’’ measurement line at 0.4, 1.0,
and 2.0 m from the stack or duct wall or, for
Part 75 only, sample points may be located at
4.4, 14.6, and 29.6% of the measurement line;
or
• After a wet scrubber or at a point where dissimilar gas streams are combined, either locate
3 sample points along the ‘‘long’’ measurement
line or locate 6 Method 1 points along a diameter (Part 75, only), unless the results of a stratification test allow you to use a ‘‘short’’ 3-point
measurement line or to sample at a single
point.
• If it can be demonstrated that stack gas concentration is ≤ 3 µg/m3, then the test site is exempted from stratification testing. Use the 3point ‘‘short’’ measurement line if the stack diameter is > 2.4 m (7.8 ft) and the 3-point ‘‘long’’
line for stack diameters ≤ 2.4 m (7.8 ft).
If the Hg concentration 2 at each traverse point
during the stratification test is:
• Within ± 5% of mean, use 1-point sampling (at
the point closest to the mean); or
• Not within ± 5% of mean, but is within ± 10% of
mean, use 3-point sampling. Locate points according to Section 8.1.3.2.2 of this method.
Alternatively, if the Hg concentration at each
point is:
• Within ± 0.2 µg/m3 of mean, use 1-point sampling (at the point closest to the mean); or
• Not within ± 0.2 µg/m3 of mean, use 3-point
sampling. Locate points according to Section
8.1.3.2.2 of this method.
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A ...............
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Prior to first run.
Prior to first run.
Prior to 1/1/09, you may
(1) forgo stratification
testing and use 3
sampling points (as
per Section 8.1.3.2.2)
or (2) perform a SO2
stratification test (see
Sections 6.5.6.1 and
6.5.6.3 of appendix A
to part 75), in lieu of a
Hg stratification test. If
the test location is
unstratified or minimally stratified for
SO2, it can be considered unstratified or
minimally stratified for
Hg also.
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SUMMARY TABLE OF QA/QC REQUIREMENTS—Continued
Status 1
Process or element
QA/QC specification
Acceptance criteria
........................................
........................................
M ..............
S ...............
Data Recording .............
Data Parameters ...........
M ..............
Data Parameters ...........
M ..............
Data Parameters ...........
Frequency ......................
Sample concentration
and calibration span.
Sample concentration
and calibration span.
Sample concentration
and calibration span.
If the Hg concentration is > 10% of the mean at
any point, then, if the alternative specification
is not met or if the stack diameter is ≤ 2.4 m
(7.8 ft):
• Perform sampling at 12 Method 1 points; or .....
• Sample at 3 points located at 16.7, 50.0 and
83.3% of the measurement line that exhibited
the highest average Hg concentration during
stratification test; or.
• Sample at 6 Method 1 points along the line
that exhibited the highest average Hg concentration (Part 75 RATAs, only).
Once per cycle ......................................................
All analyzer readings during each run within calibration span.
All analyzer readings during dynamic spiking
tests within 120% of calibration span.
Average Hg concentration for the run ≤ calibration span.
1M
Checking frequency
On and after 1/1/09,
only Hg stratification
tests are acceptable
for the purposes of
this method.
During run.
Each run.
Each spike injection.
Each run.
= Mandatory; S = Suggested; A = Alternative.
may either be the unadjusted Hg concentrations or concentrations normalized to account for temporal variations.
2 These
12.0 Calculations and Data Analysis
You must follow the procedures for
calculations and data analysis listed in this
section.
12.1 Nomenclature. The terms used in the
equations are defined as follows:
Bws = Moisture content of sample gas as
measured by Method 4 in Appendix A–
3 to this part, percent/100.
Cavg = Average unadjusted Hg concentration
for the test run, as indicated by the data
recorder µg/m3.
Cbaseline = Average Hg concentration measured
before and after dynamic spiking
injections, µg/m3.
Cd = Hg concentration, dry basis, µg/m3.
Cdif = Absolute value of the difference
between the measured Hg concentrations
of the reference HgCl2 calibration gas,
with and without the individual or
combined interference gases, µg/m3.
Cdif avg = Average of the 3 absolute values of
the difference between the measured Hg
concentrations of the reference HgCl2
calibration gas, with and without the
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Cv = Certified Hg° or HgCl2 concentration of
a calibration gas (zero, low, mid, or
high), µg/m3.
Cw = Hg concentration measured under moist
sample conditions, wet basis, µg/m3.
CS = Calibration span, µg/m3.
D = Zero or upscale drift, percent of
calibration span.
DF = Dilution factor of the spike gas,
dimensionless.
I = Interference response, percent of
calibration span.
Qprobe = Total flow rate of the stack gas
sample plus the spike gas, liters/min.
Qspike = Flow rate of the spike gas, liters/min.
Ri = Individual injection spike recovery, %;.
R= Mean value of spike recoveries at a
particular target level, %;.
RSD = Relative standard deviation, %;.
SCE = System calibration error, percent of
calibration span.
SCEi = Pre-run system calibration error
during the two-point system integrity
check, percent of calibration span.
SCEf = Post-run system calibration error
during the two-point system integrity
check, percent of calibration span.
12.2 System Calibration Error. Use
Equation 30A–1 to calculate the system
calibration error. Equation 30A–1 applies to:
3–point system calibration error tests
performed with Hg° standards; and pre- and
post-run two-point system integrity checks
performed with HgCl2.
SCE =
Cs − C v
× 100
CS
Eq. 30A-1
12.3 Drift Assessment. Use Equation
30A–2 to separately calculate the zero and
upscale drift for each test run.
D = SCE f − SCE i
Eq. 30A-2
12.3 Effluent Hg Concentration. For each
test run, calculate Cavg, the arithmetic average
of all valid Hg concentration values recorded
during the run. Then, adjust the value of Cavg
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11.0 Analytical Procedures
Because sample collection and analysis are
performed together (see Section 8), additional
discussion of the analytical procedure is not
necessary.
individual or combined interference
gases, µg/m3.
Cgas = Average Hg concentration in the
effluent gas for the test run, adjusted for
system calibration error, µg/m3.
Cint = Measured Hg concentration of the
reference HgCl2 calibration gas plus the
individual or combined interference
gases, µg/m3.
Cm = Average of pre- and post-run system
integrity check responses for the upscale
(i.e., mid- or high-level) calibration gas,
µg/m3.
Cma = Actual concentration of the upscale
(i.e., mid- or high-level) calibration gas
used for the system integrity checks, µg/
m3.
C0 = Average of pre- and post-run system
integrity check responses from the zero
gas, µg/m3.
Cnative = Vapor phase Hg concentration in the
source effluent, µg/m3.
Cref = Measured Hg concentration of the
reference HgCl2 calibration gas alone, in
the interference test, µg/m3.
Cs = Measured concentration of a calibration
gas (zero-, low-, mid-, or high-level),
when introduced in system calibration
mode, µg/m3.
Cspike = Actual Hg concentration of the spike
gas, µg/m3.
C*spike = Hg concentration of the spike gas
required to achieve a certain target value
for the spiked sample Hg concentration,
µg/m3.
Css = Measured Hg concentration of the
spiked sample at the target level, µg/m3.
C*ss = Expected Hg concentration of the
spiked sample at the target level, µg/m3.
Ctarget = Target Hg concentration of the spiked
sample, µg/m3.
CTnative = Measured tracer gas concentration
present in native effluent gas, ppm.
CTdir = Tracer gas concentration injected with
spike gas, ppm.
CTv = Diluted tracer gas concentration
measured in a spiked sample, ppm.
ER07SE07.005
10.0 Calibration and Standardization
What measurement system calibrations are
required?
Your analyzer must be calibrated with Hg°
standards. The initial 3-point system
calibration error test described in Section
8.2.4 is required before you start the test.
Also, prior to and following test runs, the
two-point system integrity checks described
in Sections 8.2.5 and 8.2.8 are required. On
and after January 1, 2009, the pre-test
dynamic spiking procedure described in
section 8.2.7 is also required to verify that the
accuracy of the measurement system is
suitable and not adversely affected by the
flue gas matrix.
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for system calibration error, using Equation
30A–3.
Cd =
Cw
1 − Bws
Eq. 30A-3
C w = Cd × (1 − Bws )
Eq. 30A-4a
Use Equation 30A–4b if your
measurements need to be corrected to a wet
basis.
C*spike = DF(C target − Cnative ) + Cnative
ER07SE07.017
Eq. 30A-5
(Cspike − C native )
Eq. 30A-6
DF
ER07SE07.015
C*ss = C native +
ER07SE07.016
theoretical Hg concentration of a spiked
sample.
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Cnative
Eq. 30A-10
18:54 Sep 06, 2007
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Q probe
Qspike
=
CTdir − CTnative
CTtv − CTnative
ER07SE07.012
Eq. 30A-9
concentration equals the average baseline
concentration (see Equation 30A–11).
Cnative = Cbaseline
Where, for each interference gas (or
mixture):
3
Eq. 30A-11
12.11 Overall Interference Response. Use
equation 30A–12 to calculate the overall
interference response.
For spiking procedures that halt all
injections between spikes, the native
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Eq. 30A-8
n −1
using either direct flow measurements or
tracer gas measurements.
DF =
12.10 Native Concentration. For spiking
procedures that inject blank or carrier gases
(at the spiking flow rate, Qspike) between
spikes, use Equation 30A–10 to calculate the
native concentration.
− R )2
ER07SE07.010
12.9 Spike Dilution Factor. Use Equation
30A–9 to calculate the spike dilution factor,
i
i =1
ER07SE07.011
100%
RSD =
R
∑ (R
ER07SE07.013
percentage spike recovery values from the
mean.
n
C
DF
= baseline
DF −1
Eq. 30A-7
I=
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difavg
CS
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× 100
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Eq. 30A-12
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Cdifavg =
∑C
dif
1
3
Cdif = Cref − Cint
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Eq. 30A-13
Eq. 30A-14
ER07SE07.009
12.8 Relative Standard Deviation. Use
Equation 30A–8 to calculate the relative
standard deviation of the individual
DF (Css − Cnative ) + Cnative
× 100%
Cspike
ER07SE07.008
R=
ER07SE07.014
12.7 Spike Recovery. Use Equation 30A–
7 to calculate the percentage recovery of each
spike.
ER07SE07.007
12.6 Spiked Sample Concentration. Use
Equation 30A–6 to determine the expected or
Eq. 30A-4b
12.5 Dynamic Spike Gas Concentrations.
Use Equation 30A–5 to determine the spike
gas concentration needed to produce a spiked
sample with a certain ‘‘target’’ Hg
concentration.
ER07SE07.019
12.4 Moisture Correction. Use Equation
30A–4a if your measurements need to be
corrected to a dry basis.
Cma
C m − C0
ER07SE07.018
Cgas = (Cavg − C0 )
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13.0
Method Performance
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13.1 System Calibration Error Test. This
specification applies to the 3-point system
calibration error tests using Hg0. At each
calibration gas level tested (low-, mid-, or
high-level), the calibration error must be
within ±5.0 percent of the calibration span.
Alternatively, the results are acceptable if | Cs
¥ Cv | ≤0.5 µg/m3.
13.2 System Integrity Checks. This
specification applies to all pre- and post-run
2-point system integrity checks using HgCl2
and zero gas. At each calibration gas level
tested (zero and mid- or high-level), the error
must be within ±5.0 percent of the calibration
span. Alternatively, the results are acceptable
if | Cs ¥ Cv | ≤0.5 µg/m3.
13.3 Drift. For each run, the low-level and
upscale drift must be less than or equal to 3.0
percent of the calibration span. The drift is
also acceptable if the pre- and post-run
system integrity check responses do not
differ by more than 0.3 µg/m3 (i.e., | Cs post-run
¥ Cs pre-run | ≤0.3 µg/m3).
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13.4 Interference Test. Summarize the
results following the format contained in
Table 30A–4. For each interference gas (or
mixture), calculate the mean difference
between the measurement system responses
with and without the interference test gas(es).
The overall interference response for the
analyzer that was used for the test (calculated
according to Equation 30A–12), must not be
greater than 3.0 percent of the calibration
span used for the test (see Section 8.6). The
results of the interference test are also
acceptable if the sum of the absolute average
differences for all interference gases (i.e., S
Cdif avg) does not exceed 0.3 µg/m3.
13.5 Dynamic Spiking Test. For the pretest dynamic spiking, the mean value of the
percentage spike recovery must be 100 ±10
percent. In addition, the relative standard
deviation (RSD) of the individual percentage
spike recovery values from the mean must be
≤5.0 percent. Alternatively, if the mean
percentage recovery is not met, the results are
acceptable if the absolute difference between
the theoretical spiked sample concentration
(see Section 12.6) and the actual average
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51511
value of the spiked sample concentration is
≤0.5 µg/m3.
14.0
Pollution Prevention [Reserved]
15.0
Waste Management [Reserved]
16.0
References
1. EPA Traceability Protocol for
Qualification and Certification of Elemental
Mercury Gas Generators, expected
publication date December 2008, see
www.epa.gov/ttn/emc.
2. EPA Traceability Protocol for
Qualification and Certification of Oxidized
Mercury Gas Generators, expected
publication date December 2008, see
www.epa.gov/ttn/emc.
3. EPA Traceability Protocol for Assay and
Certification of Gaseous Calibration
Standards, expected revision publication
date December 2008, see www.epa.gov/ttn/
emc.
17.0
Figures and Tables
BILLING CODE 6560–50–C
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51515
TABLE 30A–3.—INTERFERENCE CHECK TABLE 30A–3.—INTERFERENCE CHECK TABLE 30A–3.—INTERFERENCE CHECK
GAS CONCENTRATIONS
GAS CONCENTRATIONS—Continued
GAS CONCENTRATIONS—Continued
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CO2 ......................
CO ........................
HCl 2 .....................
NO 2 ......................
SO2 .......................
O2 .........................
VerDate Aug<31>2005
Concentration,
tentative—(balance N2)
15% ± 1% CO2
100 ± 20 ppm
100 ± 20 ppm
250 ± 50 ppm
200 ± 20 ppm
3% ± 1% O2
18:54 Sep 06, 2007
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Potential
interferent gas 1
H2O ......................
Nitrogen ................
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Concentration,
tentative—(balance N2)
10% ± 1% H2O
Balance
Fmt 4701
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Potential
interferent gas 1
Concentration,
tentative—(balance N2)
Other.
1 Any of these specific gases can be tested
at a lower level if the manufacturer has provided reliable means for limiting or scrubbing
that gas to a specified level.
2 HCl and NO must be tested as a mixture.
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ER07SE07.023
Potential
interferent gas 1
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Method 30B—Determination of Total Vapor
Phase Mercury Emissions From Coal-Fired
Combustion Sources Using Carbon Sorbent
Traps
1.0 Scope and Application
What is Method 30B?
Method 30B is a procedure for measuring
total vapor phase mercury (Hg) emissions
from coal-fired combustion sources using
sorbent trap sampling and an extractive or
thermal analytical technique. This method is
only intended for use only under relatively
low particulate conditions (e.g., sampling
after all pollution control devices). Quality
assurance and quality control requirements
are included to assure that you, the tester,
collect data of known and acceptable quality
for each testing program. This method does
not completely describe all equipment,
supplies, and sampling and analytical
procedures you will need, but instead refers
to other test methods for some of the details.
Therefore, to obtain reliable results, you
should also have a thorough knowledge of
these additional methods which are found in
Appendices A–1 and A–3 to this part:
(a) Method 1—Sample and Velocity
Traverses for Stationary Sources.
(b) Method 4—Determination of Moisture
Content in Stack Gases.
(c) Method 5—Determination of Particulate
Matter Emissions from Stationary Sources
1.1 Analytes. What does this method
determine? This method is designed to
measure the mass concentration of total
vapor phase Hg in flue gas, including
elemental Hg (Hg0) and oxidized forms of Hg
(Hg∂2), in micrograms per dry standard cubic
meter (µg/dscm).
CAS No.
Elemental Hg
(Hg 0 ).
7439–97–6
Oxidized Hg
(Hg∂2).
jlentini on PROD1PC65 with RULES2
Analyte
....................
Analytical
range and
sensitivity
Typically 0.1
µg/dscm to
>50 µg/
dscm.
(Same)
1.2 Applicability. When is this method
required? Method 30B is a reference method
for relative accuracy test audits (RATAs) of
vapor phase Hg CEMS and sorbent trap
monitoring systems installed at coal-fired
boilers and is also appropriate for Hg
emissions testing at such boilers. It is
intended for use only under relatively low
particulate conditions (i.e., sampling after all
pollution control devices); in cases where
significant amounts of particle-bound Hg
may be present, an isokinetic sampling
method for Hg should be used. Method 30B
may also be specified by New Source
Performance Standards (NSPS), National
Emission Standards for Hazardous Air
Pollutants (NESHAP), emissions trading
programs, State Implementation Plans (SIPs),
and operating permits that require
measurement of Hg concentrations in
stationary source emissions, either to
determine compliance with an applicable
emission standard or limit, or to conduct
RATAs of Hg CEMS and sorbent trap
monitoring systems.
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1.3 Data Quality Objectives (DQO). How
good must my collected data be? Method 30B
has been designed to provide data of high
and known quality for Hg emissions testing
and for RATA testing of Hg monitoring
systems, including CEMS and sorbent trap
monitors. In these and other applications, the
principal objective is to ensure the accuracy
of the data at the actual emissions levels and
in the actual emissions matrix encountered.
To meet this objective, NIST-traceable
calibration standards must be used and
method performance tests are required.
3.8 Test refers to the series of runs
required by the applicable regulation.
3.9 Thermal Analysis means an analytical
technique where the contents of the sorbent
traps are analyzed using a thermal technique
(desorption or combustion) to release the
captured Hg in a detectable form for
quantification.
3.10 Wet Analysis means an analytical
technique where the contents of the sorbent
tube are first leached or digested to
quantitatively transfer the captured Hg to
liquid solution for subsequent analysis.
2.0 Summary of Method
Known volumes of flue gas are extracted
from a stack or duct through paired, in-stack
sorbent media traps at an appropriate flow
rate. Collection of mercury on the sorbent
media in the stack mitigates potential loss of
mercury during transport through a probe/
sample line. For each test run, paired train
sampling is required to determine
measurement precision and verify
acceptability of the measured emissions data.
A field recovery test which assesses recovery
of an elemental Hg spike to determine
measurement bias is also used to verify data
acceptability. The sorbent traps are recovered
from the sampling system, prepared for
analysis as needed, and analyzed by any
suitable determinative technique that can
meet the performance criteria.
4.0 Interferences
Interferences may result from the sorbent
trap material used as well as from the
measurement environment itself. The iodine
present on some sorbent traps may impart a
negative measurement bias. High levels of
sulfur trioxide (SO3) are also suspected to
compromise the performance of sorbent trap
Hg capture. These, and other, potential
interferences are assessed by performing the
analytical matrix interference, Hg0 and HgCl2
analytical bias and field recovery tests.
3.0 Definitions
3.1 Analytical System is the combined
equipment and apparatus used to perform
sample analyses. This includes any
associated sample preparation apparatus e.g.,
digestion equipment, spiking systems,
reduction devices, etc., as well as analytical
instrumentation such as UV AA and UV AF
cold vapor analyzers.
3.2 Calibration Standards are the Hg
containing solutions prepared from NIST
traceable standards and are used to directly
calibrate analytical systems.
3.3 Independent Calibration Standard is
a NIST traceable standard obtained from a
source or supplier independent of that for the
calibration standards and is used to confirm
the integrity of the calibration standards
used.
3.4 Method Detection Limit (MDL) is the
lowest mass of Hg greater than zero that can
be estimated and reported by your candidate
analytical technique. The MDL is statistically
derived from replicate low level
measurements near your analytical
instrument’s detection level.
3.5 NIST means the National Institute of
Standards and Technology, located in
Gaithersburg, Maryland.
3.6 Run means a series of gas samples
taken successively from the stack or duct. A
test normally consists of a specific number of
runs.
3.7 Sorbent Trap means a cartridge or
sleeve containing a sorbent media (typically
activated carbon treated with iodine or some
other halogen) with multiple sections
separated by an inert material such as glass
wool. These sorbent traps are optimized for
the quantitative capture of elemental and
oxidized forms of Hg and can be analyzed by
multiple techniques.
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5.0 Safety
What safety measures should I consider
when using this method? This method may
require you to work with hazardous materials
and in hazardous conditions. You are
encouraged to establish safety procedures
before using the method. Among other
precautions, you should become familiar
with the safety recommendations in the gas
analyzer user’s manual. Occupational Safety
and Health Administration (OSHA)
regulations concerning use of compressed gas
cylinders and noxious gases may apply.
5.1 Site Hazards. Prior to applying these
procedures/specifications in the field, the
potential hazards at the test site should be
considered; advance coordination with the
site is critical to understand the conditions
and applicable safety policies. At a
minimum, portions of the sampling system
will be hot, requiring appropriate gloves,
long sleeves, and caution in handling this
equipment.
5.2 Laboratory Safety. Policies should be
in place to minimize risk of chemical
exposure and to properly handle waste
disposal in the laboratory. Personnel shall
wear appropriate laboratory attire according
to a Chemical Hygiene Plan established by
the laboratory.
5.3 Reagent Toxicity/Carcinogenicity.
The toxicity and carcinogenicity of any
reagents used must be considered. Depending
upon the sampling and analytical
technologies selected, this measurement may
involve hazardous materials, operations, and
equipment and this method does not address
all of the safety problems associated with
implementing this approach. It is the
responsibility of the user to establish
appropriate safety and health practices and
determine the applicable regulatory
limitations prior to performance. Any
chemical should be regarded as a potential
health hazard and exposure to these
compounds should be minimized. Chemists
should refer to the Material Safety Data Sheet
(MSDS) for each chemical used.
5.4 Waste Disposal. Any waste generated
by this procedure must be disposed of
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according to a hazardous materials
management plan that details and tracks
various waste streams and disposal
procedures.
6.0 Equipment and Supplies
The following list is presented as an
example of key equipment and supplies
likely required to measure vapor-phase Hg
using a sorbent trap sampling system. It is
recognized that additional equipment and
supplies may be needed. Collection of paired
samples is required.
6.1 Sorbent Trap Sampling System. A
typical sorbent trap sampling system is
shown in Figure 30B–1 in Section 17.0. The
sorbent trap sampling system shall include
the following components:
6.1.1 Sorbent Traps. The sorbent media
used to collect Hg must be configured in a
trap with at least two distinct segments or
sections, connected in series, that are
amenable to separate analyses. Section 1 is
designated for primary capture of gaseous Hg.
Section 2 is designated as a backup section
for determination of vapor phase Hg
breakthrough. Each sorbent trap must be
inscribed or otherwise permanently marked
with a unique identification number, for
tracking purposes. The sorbent media may be
any collection material (e.g., carbon,
chemically-treated filter, etc.) capable of
quantitatively capturing and recovering for
subsequent analysis, all gaseous forms of Hg
in the emissions from the intended
application. Selection of the sorbent media
shall be based on the material’s ability to
achieve the performance criteria contained in
this method as well as the sorbent’s vapor
phase Hg capture efficiency for the emissions
matrix and the expected sampling duration at
the test site. The sorbent media must be
obtained from a source that can demonstrate
their quality assurance and quality control
(see Section 7.2). The paired sorbent traps are
supported on a probe (or probes) and inserted
directly into the flue gas stream.
6.1.2 Sampling Probe Assembly. Each
probe assembly shall have a leak-free
attachment to the sorbent trap(s). Each
sorbent trap must be mounted at the entrance
of or within the probe such that the gas
sampled enters the trap directly. Each probe/
sorbent trap assembly must be heated to a
temperature sufficient to prevent liquid
condensation in the sorbent trap(s). Auxiliary
heating is required only where the stack
temperature is too low to prevent
condensation. Use a calibrated thermocouple
to monitor the stack temperature. A single
probe capable of operating the paired sorbent
traps may be used. Alternatively, individual
probe/sorbent trap assemblies may be used,
provided that the individual sorbent traps are
co-located to ensure representative Hg
monitoring.
6.1.3 Moisture Removal Device. A
moisture removal device or system shall be
used to remove water vapor from the gas
stream prior to entering dry gas flow
metering devices.
6.1.4 Vacuum Pump. Use a leak-tight,
vacuum pump capable of operating within
the system’s flow range.
6.1.5 Gas Flow Meter. A gas flow meter
(such as a dry gas meter, thermal mass flow
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meter, or other suitable measurement device)
shall be used to determine the total sample
volume on a dry basis, in units of standard
cubic meters. The meter must be sufficiently
accurate to measure the total sample volume
to within 2 percent and must be calibrated
at selected flow rates across the range of
sample flow rates at which the sampling train
will be operated. The gas flow meter shall be
equipped with any necessary auxiliary
measurement devices (e.g., temperature
sensors, pressure measurement devices)
needed to correct the sample volume to
standard conditions.
6.1.6 Sample Flow Rate Meter and
Controller. Use a flow rate indicator and
controller for maintaining necessary
sampling flow rates.
6.1.7 Temperature Sensor. Same as
Section 6.1.1.7 of Method 5 in Appendix A–
3 to this part.
6.1.8 Barometer. Same as Section 6.1.2 of
Method 5 in Appendix A–3 to this part.
6.1.9 Data Logger (optional). Device for
recording associated and necessary ancillary
information (e.g., temperatures, pressures,
flow, time, etc.).
6.2 Gaseous Hg0 Sorbent Trap Spiking
System. A known mass of gaseous Hg0 must
be either present on or spiked onto the first
section of sorbent traps in order to perform
the Hg0 and HgCl2 analytical bias test and the
field recovery study. Any approach capable
of quantitatively delivering known masses of
Hg0 onto sorbent traps is acceptable. Several
spiking technologies or devices are available
to meet this objective. Their practicality is a
function of Hg mass spike levels. For low
levels, NIST-certified or NIST-traceable gas
generators or tanks may be suitable. An
alternative system, capable of delivering
almost any mass required, makes use of
NIST-certified or NIST-traceable Hg salt
solutions (e.g., HgCl2, Hg(NO3)2). With this
system, an aliquot of known volume and
concentration is added to a reaction vessel
containing a reducing agent (e.g., stannous
chloride); the Hg salt solution is reduced to
Hg0 and purged onto the sorbent trap using
an impinger sparging system. When
available, information on example spiking
systems will be posted at https://
www.epa.gov/ttn/emc.
6.3 Sample Analysis Equipment. Any
analytical system capable of quantitatively
recovering and quantifying total Hg from the
sorbent media selected is acceptable
provided that the analysis can meet the
performance criteria described in this
method. Example recovery techniques
include acid leaching, digestion, and thermal
desorption/direct combustion. Example
analytical techniques include, but are not
limited to, ultraviolet atomic fluorescence
(UV AF), ultraviolet atomic absorption (UV
AA) with and without gold trapping, and Xray fluorescence (XRF) analysis.
6.3 Moisture Measurement System. If
correction of the measured Hg emissions for
moisture is required (see Section 8.3.3.7),
either Method 4 in Appendix A–3 to this part
or other moisture measurement methods
approved by the Administrator will be
needed to measure stack gas moisture
content.
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7.0 Reagents and Standards
7.1 Reagents and Standards. Only NISTcertified or NIST-traceable calibration
standards, standard reference materials, and
reagents shall be used for the tests and
procedures required by this method.
7.2 Sorbent Trap Media. The sorbent trap
media shall be prepared such that the
material used for testing is of known and
acceptable quality. Sorbent supplier quality
assurance/quality control measures to ensure
appropriate and consistent performance such
as sorptive capacity, uniformity of
preparation treatments, and background
levels shall be considered.
8.0 Sample Collection and Handling
This section presents the sample collection
and handling procedures along with the
pretest and on-site performance tests
required by this method. Since you may
choose different options to comply with
certain performance criteria, each test report
must identify the specific options selected
and document the results with respect to the
performance criteria of this method.
8.1 Sample Point Selection. What
sampling site and sampling points do I
select? Same as Section 8.1 of Method 30A
of this appendix.
8.2 Measurement System Performance
Tests. What performance criteria must my
measurement system meet? The following
laboratory and field procedures and
associated criteria of this section are
designed to ensure (1) selection of a sorbent
and analytical technique combination
capable of quantitative collection and
analysis of gaseous Hg, (2) collection of an
adequate amount of Hg on each sorbent trap
during field tests, and (3) adequate
performance of the method for each test
program: The primary objectives of these
performance tests are to characterize and
verify the performance of your intended
analytical system and associated sampling
and analytical procedures, and to define the
minimum amount of Hg (as the sample
collection target) that can be quantified
reliably.
(a) Analytical Matrix Interference Test;
(b) Determination of Minimum Sample
Mass;
(c) Hg0 and HgCl2 Analytical Bias Test;
(d) Determination of Nominal Sample
Volume;
(e) Field Recovery Test.
8.2.1 Analytical Matrix Interference Test
and Minimum Sample Dilution.
(a) The analytical matrix interference test
is a laboratory procedure. It is required only
if you elect to use a liquid digestion
analytical approach and needs to be
performed only once for each sorbent
material used. The purpose of the test is to
verify the presence or absence of known and
potential analytical matrix interferences,
including the potential negative bias
associated with iodine common to many
sorbent trap materials. The analytical matrix
interference test determines the minimum
dilution (if any) necessary to mitigate matrix
effects on the sample digestate solutions.
(b) The result of the analytical matrix
interference test, i.e., the minimum sample
dilution required (if any) for all sample
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analyses, is used to establish the minimum
sample mass needed for the Hg0 and HgCl2
analytical bias test and to determine the
nominal sample volume for a test run. The
analytical matrix interference test is sorbent
material-specific and shall be performed for
each sorbent material you intend to use for
field sampling and analysis. The test shall be
performed using a mass of sorbent material
comparable to the sorbent mass typically
used in the first section of the trap for
sampling. Similar sorbent materials from
different sources of supply are considered to
be different materials and must be tested
individually. You must conduct the
analytical matrix interference test for each
sorbent material prior to the analysis of field
samples.
8.2.1.1 Analytical Matrix Interference
Test Procedures. Digest and prepare for
analysis a representative mass of sorbent
material (unsampled) according to your
intended laboratory techniques for field
samples. Analyze the digestate according to
your intended analytical conditions at the
least diluted level you intend to use for
sample analysis (e.g., undiluted, 1 in 10
dilution, etc.). Determine the Hg
concentration of the undiluted digestate
solution. Prepare a series of solutions with a
fixed final volume containing graduated
aliquots of the sample digestate and, a fixed
aliquot of a calibration standard (with the
balance being Hg-free reagent or H20) to
establish solutions of varied digestate
dilution ratio (e.g., 1:2, 1:5, 1:10, 1:100, etc.—
see example in Section 8.2.1.3, below). One
of these solutions should contain only the
aliquot of the calibration standard in Hg-free
reagent or H2O. This will result in a series
of solutions where the amount of Hg is held
relatively constant and only the volume of
digestate diluted is varied. Analyze each of
these solutions following intended sample
analytical procedures and conditions,
determining the concentration for each
solution.
8.2.1.2 Analytical Matrix Interference
Test Acceptance Criteria. Compare the
measured concentration of each solution
containing digestate to the measured
concentration of the digestate-free solution.
The lowest dilution ratio of any solution
having a Hg concentration within ±5 percent
of the digestate-free solution is the minimum
dilution ratio required for analysis of all
samples. If you desire to measure the
digestate without dilution, the ± 5 percent
criterion must be met at a dilution ratio of
at least 9:10 (i.e., ≥90% digestate).
8.2.1.3 Example Analytical Matrix
Interference Test. An example analytical
matrix interference test is presented below.
Additional information on the conduct of the
analytical matrix interference test will be
posted at https://www.epa.gov/ttn/emc.
Determine the most sensitive working range
for the analyzer to be used. This will be a
narrow range of concentrations. Digest and
prepare for analysis a representative mass of
sorbent material (unsampled) according to
your intended laboratory techniques for
sample preparation and analysis. Prepare a
calibration curve for the most sensitive
analytical region, e.g., 0.0, 0.5, 1.0, 3.0, 5.0,
10 ppb. Using the highest calibration
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standard, e.g., 10.0 ppb, prepare a series of
solutions by adding successively smaller
increments of the digestate to a fixed volume
of the calibration standard and bringing each
solution to a final fixed volume with
mercury-free deionized water (diH2O). To 2.0
ml of the calibration standard add 18.0, 10.0,
4.0, 2.0, 1.0, 0.2, and 0.0 ml of the digestate.
Bring the final volume of each solution to a
total volume of 20 ml by adding 0.0, 8.0,
14.0, 16.0, 17.0, 17.8, and 18.0 ml of diH2O.
This will yield solutions with dilution ratios
of 9:10, 1:2, 1:5, 1:10, 1:20, 1:100, and 0:10,
respectively. Determine the Hg concentration
of each solution. The dilution ratio of any
solution having a concentration that is within
±5 percent of the concentration of the
solution containing 0.0 ml of digestate is an
acceptable dilution ratio for analyzing field
samples. If more than one solution meets this
criterion, the one with the lowest dilution
ratio is the minimum dilution required for
analysis of field samples. If the 9:10 dilution
meets this criterion, then no sample dilution
is required.
8.2.2 Determination of Minimum Sample
Mass. The minimum mass of Hg that must be
collected per sample must be determined.
This information is necessary in order to
effectively perform the Hg0 and HgCl2
Analytical Bias Test, to estimate target
sample volumes/sample times for test runs,
and to ensure the quality of the
measurements. The determination of
minimum sample mass is a direct function of
analytical technique, measurement
sensitivity, dilutions, etc. This determination
is required for all analytical techniques.
Based on the analytical approach you
employ, you should determine the most
sensitive calibration range. Based on a
calibration point within that range, you must
consider all sample treatments (e.g.,
dilutions) to determine the mass of sample
that needs to be collected to ensure that all
sample analyses fall within your calibration
curve.
8.2.2.1 Determination of Minimum
Calibration Concentration or Mass. Based on
your instrument’s sensitivity and linearity,
determine the calibration concentrations or
masses that make up a representative low
level calibration range. Verify that you are
able to meet the multipoint calibration
performance criteria in section 11.0 of this
method. Select a calibration concentration or
mass that is no less than 2 times the lowest
concentration or mass in your calibration
curve. The lowest point in your calibration
curve must be at least 5, and preferably 10,
times the Method Detection Limit (MDL),
which is the minimum amount of the analyte
that can be detected and reported. The MDL
must be determined at least once for the
analytical system using an MDL study such
as that found in section 17.0 of the proposed
amendments to EPA Method 301 (69 FR
76642, 12/22/2004).
Note to Section 8.2.2.1: While it might be
desirable to base the minimum calibration
concentration or mass on the lowest point in
the calibration curve, selecting a higher
concentration or mass is necessary to ensure
that all analyses of the field samples will fall
within the calibration curve. Therefore, it is
strongly recommended that you select a
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minimum calibration concentration or mass
that is sufficiently above the lowest point of
the calibration curve (see examples in
sections 8.2.2.2.1 and 8.2.2.2.2 below).
8.2.2.2 Determination of Minimum
Sample Mass. Based on your minimum
calibration concentration or mass and other
sample treatments including, but not limited
to, final digestate volume and minimum
sample dilution, determine the minimum
sample mass. Consideration should also be
given to the Hg levels expected to be
measured in Section 2 of the sorbent traps
and to the breakthrough criteria presented in
Table 9–1.
8.2.2.2.1 Example Determination of
Minimum Sample Mass for Thermal
Desorption Analysis. A thermal analysis
system has been calibrated at five Hg mass
levels: 10 ng, 20 ng, 50 ng, 100 ng, 200 ng,
and shown to meet the calibration
performance criteria in this method. Based
on 2 times the lowest point in the calibration
curve, 20 ng is selected as the minimum
calibration mass. Because the entire sample
is analyzed and there are no dilutions
involved, the minimum sample mass is also
20 ng.
Note: In this example, if the typical
background (blank) Hg levels in section 2
were relatively high (e.g., 3 to 5 ng), a sample
mass of 20 ng might not have been sufficient
to ensure that the breakthrough criteria in
Table 9–1 would be met, thereby
necessitating the use of a higher point on the
calibration curve (e.g., 50 ng) as the
minimum calibration and sample mass.
8.2.2.2.2 Example Determination of
Minimum Sample Mass for Acid Leachate/
Digestate Analysis. A cold vapor analysis
system has been calibrated at four Hg
concentration levels: 2 ng/L, 5 ng, 10 ng/L,
20 ng/L, and shown to meet the calibration
performance criteria in this method. Based
on 2 times the lowest point in the calibration
curve, 4 ng/L was selected as the minimum
calibration concentration. The final sample
volume of a digestate is nominally 50 ml
(0.05 L) and the minimum dilution necessary
was determined to be 1:100 by the Analytical
Matrix Interference Test of Section 8.2.1. The
following calculation would be used to
determine the minimum sample mass.
Minimum sample mass = (4 ng/L) × (0.05 L)
× (100) = 20 ng
Note: In this example, if the typical
background (blank) Hg levels in section 2
were relatively high (e.g., 3 to 5 ng), a sample
mass of 20 ng might not have been sufficient
to ensure that the breakthrough criterion in
Table 9–1 would be met, thereby
necessitating the use of a higher point on the
calibration curve (e.g., 10 ng/L) as the
minimum calibration concentration.
8.2.3 Hg0 and HgCl2 Analytical Bias Test.
Before analyzing any field samples, the
laboratory must demonstrate the ability to
recover and accurately quantify Hg0 and
HgCl2 from the chosen sorbent media by
performing the following analytical bias test
for sorbent traps spiked with Hg0 and HgCl2.
The analytical bias test is performed at a
minimum of two distinct sorbent trap Hg
loadings that will: (1) Represent the lower
and upper bound of sample Hg loadings for
application of the analytical technique to the
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field samples, and (2) be used for data
validation.
8.2.3.1 Hg0 and HgCl2 Analytical Bias
Test Procedures. Determine the lower and
upper bound mass loadings. The minimum
sample mass established in Section 8.2.2.2
can be used for the lower bound Hg mass
loading although lower Hg loading levels are
acceptable. The upper bound Hg loading
level should be an estimate of the greatest
mass loading that may result as a function of
stack concentration and volume sampled. As
previously noted, this test defines the bounds
that actual field samples must be within in
order to be valid.
8.2.3.1.1 Hg0 Analytical Bias Test.
Analyze the front section of three sorbent
traps containing Hg0 at the lower bound mass
loading level and the front section of three
sorbent traps containing Hg0 at the upper
bound mass loading level. In other words,
analyze each mass loading level in triplicate.
You may refer to Section 6.2 for spiking
guidance. Prepare and analyze each spiked
trap, using the same techniques that will be
used to prepare and analyze the field
samples. The average recovery for the three
traps at each mass loading level must be
between 90 and 110 percent. If multiple
types of sorbent media are to be analyzed, a
separate analytical bias test is required for
each sorbent material.
8.2.3.1.2 HgCl2 Analytical Bias Test.
Analyze the front section of three sorbent
traps containing HgCl2 at the lower bound
mass loading level and the front section of
three traps containing HgCl2 at the upper
bound mass loading level. HgCl2 can be
spiked as a gas, or as a liquid solution
containing HgCl2. However the liquid volume
spiked must be <100 µL. Prepare and analyze
each spiked trap, using the techniques that
will be used to prepare and analyze the field
samples. The average recovery for three traps
at each spike concentration must be between
90 and 110 percent. Again, if multiple types
of sorbent media are to be analyzed, a
separate analytical bias test is required for
each sorbent material.
8.2.4 Determination of Target Sample
Volume. The target sample volume is an
estimate of the sample volume needed to
ensure that valid emissions data are collected
(i.e., that sample mass Hg loadings fall within
the analytical calibration curve and are
within the upper and lower bounds set by the
analytical bias tests). The target sample
volume and minimum sample mass can also
be determined by performing a diagnostic
test run prior to initiation of formal testing.
Example: If the minimum sample mass is
50 ng and the concentration of mercury in
the stack gas is estimated to be 2 µg/m3 (ng/
L) then the following calculation would be
used to determine the target sample volume:
Target Sample Volume = (50 ng)/(2 ng/L) =
25 L
Note: For the purposes of relative accuracy
testing of Hg monitoring systems under part
75 of this chapter and Performance
Specification 12A in appendix B to this part,
when the stack gas Hg concentration is
expected to be very low (<0.5 µg/dscm) you
may estimate the Hg concentration at 0.5 µg/
dscm.
8.2.5 Determination of Sample Run Time.
Sample run time will be a function of
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minimum sample mass (see Section 8.2.2),
target sample volume and nominal
equipment sample flow rate. The minimum
sample run time for conducting relative
accuracy test audits of Hg monitoring
systems is 30 minutes and for emissions
testing to characterize an emission source is
1 hour. The target sample run time can be
calculated using the following example.
Example: If the target sample volume has
been determined to be 25 L, then the
following formula would be used to
determine the sampling time necessary to
acquire 25 L of gas when sampling at a rate
of 0.4 L/min.
Sampling time (min) = 25 L / 0.4 L/min = 63
minutes
8.2.6 Field Recovery Test. The field
recovery test provides a test program-specific
verification of the performance of the
combined sampling and analytical approach.
Three sets of paired samples, one of each pair
which is spiked with a known level of Hg,
are collected and analyzed and the average
recovery of the spiked samples is used to
verify performance of the measurement
system under field conditions during that test
program. The conduct of this test requires an
estimate or confirmation of the stack Hg
concentrations at the time of testing.
8.2.6.1 Calculation of Pre-sampling
Spiking Level. Determine the sorbent trap
spiking level for the field recovery test using
estimates of the stack Hg concentration, the
target sample flow rate, and the planned
sample duration. First, determine the Hg
mass expected to be collected in section 1 of
the sorbent trap. The pre-sampling spike
must be within 50 to 150 percent of this
expected mass.
Example calculation: For an expected stack
Hg concentration of 5 ug/m3 (ng/L) a target
sample rate of 0.40 liters/min, and a sample
duration of 1 hour:
(0.40 L/min)*(60 min)*(5ng/L) = 120 ng
A Hg spike of 60 to 180 ng (50–150% of
120 ng) would be appropriate.
8.2.6.2 Procedures. Set up two identical
sampling trains. One of the sampling trains
shall be designated the spiked train and the
other the unspiked train. Spike Hg0 onto the
front section of the sorbent trap in the spiked
train before sampling. The mass of Hg spiked
shall be 50 to 150 percent of the mass
expected to be collected with the unspiked
train. Sample the stack gas with the two
trains simultaneously using the same
procedures as for the field samples (see
Section 8.3). The total sample volume must
be within ±20 percent of the target sample
volume for the field sample test runs.
Analyze the sorbent traps from the two trains
utilizing the same analytical procedures and
instrumentation as for the field samples (see
Section 11.0). Determine the fraction of
spiked Hg recovered (R) using the equations
in Section 12.7. Repeat this procedure for a
total of three runs. Report the individual R
values in the test report; the average of the
three R values must be between 85 and 115
percent.
Note to section 8.2.6.2: It is acceptable to
perform the field recovery test concurrent
with actual test runs (e.g., through the use of
a quad probe). It is also acceptable to use the
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field recovery test runs as test runs for
emissions testing or for the RATA of a Hg
monitoring system under part 75 of this
chapter and Performance Specification 12A
in appendix B to this part, if certain
conditions are met. To determine whether a
particular field recovery test run may be used
as a RATA run, subtract the mass of the Hg0
spike from the total Hg mass collected in
sections 1 and 2 of the spiked trap. The
difference represents the mass of Hg in the
stack gas sample. Divide this mass by the
sample volume to obtain the Hg
concentration in the effluent gas stream, as
measured with the spiked trap. Compare this
concentration to the corresponding Hg
concentration measured with the unspiked
trap. If the paired trains meet the relative
deviation and other applicable data
validation criteria in Table 9–1, then the
average of the two Hg concentrations may be
used as an emissions test run value or as the
reference method value for a RATA run.
8.3 Sampling. This section describes the
procedures and criteria for collecting the
field samples for analysis. As noted in
Section 8.2.6, the field recovery test samples
are also collected using these procedures.
8.3.1 Pre-test leak check. Perform a leak
check of the sampling system with the
sorbent traps in place. For each of the paired
sampling trains, draw a vacuum in the train,
and adjust the vacuum to ∼15″ Hg; and, using
the gas flow meter, determine leak rate. The
leak rate for an individual train must not
exceed 4 percent of the target sampling rate.
Once the leak check passes this criterion,
carefully release the vacuum in the sample
train, then seal the sorbent trap inlet until the
probe is ready for insertion into the stack or
duct.
8.3.2 Determination of Flue Gas
Characteristics. Determine or measure the
flue gas measurement environment
characteristics (gas temperature, static
pressure, gas velocity, stack moisture, etc.) in
order to determine ancillary requirements
such as probe heating requirements (if any),
initial sampling rate, moisture management,
etc.
8.3.3 Sample Collection
8.3.3.1 Remove the plug from the end of
each sorbent trap and store each plug in a
clean sorbent trap storage container. Remove
the stack or duct port cap and insert the
probe(s). Secure the probe(s) and ensure that
no leakage occurs between the duct and
environment.
8.3.3.2 Record initial data including the
sorbent trap ID, date, and the run start time.
8.3.3.3 Record the initial gas flow meter
reading, stack temperature, meter
temperatures (if needed), and any other
appropriate information, before beginning
sampling. Begin sampling and target a
sampling flow rate similar to that for the field
recovery test. Then, at regular intervals (≤5
minutes) during the sampling period, record
the date and time, the sample flow rate, the
gas meter reading, the stack temperature, the
flow meter temperatures (if using a dry gas
meter), temperatures of heated equipment
such as the vacuum lines and the probes (if
heated), and the sampling system vacuum
readings. Adjust the sampling flow rate as
necessary to maintain the initial sample flow
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rate. Ensure that the total volume sampled for
each run is within 20 percent of the total
volume sampled for the field recovery test.
8.3.3.4 Data Recording. Obtain and record
any essential operating data for the facility
during the test period, e.g., the barometric
pressure must be obtained for correcting
sample volume to standard conditions when
using a dry gas meter. At the end of the data
collection period, record the final gas flow
meter reading and the final values of all other
essential parameters.
8.3.3.5 Post-Test Leak Check. When
sampling is completed, turn off the sample
pump, remove the probe(s) with sorbent traps
from the port, and carefully seal the end of
each sorbent trap. Perform another leak check
of each sampling train with the sorbent trap
in place, at the maximum vacuum reached
during the sampling period. Record the
leakage rates and vacuums. The leakage rate
for each train must not exceed 4 percent of
the average sampling rate for the data
collection period. Following each leak check,
carefully release the vacuum in the sample
train.
8.3.3.6 Sample Recovery. Recover each
sampled sorbent trap by removing it from the
probe and sealing both ends. Wipe any
deposited material from the outside of the
sorbent trap. Place the sorbent trap into an
appropriate sample storage container and
store/preserve in appropriate manner (see
Section 8.3.3.8).
8.3.3.7 Stack Gas Moisture
Determination. If the moisture basis of the
measurements made with this method (dry)
is different from the moisture basis of either:
(1) the applicable emission limit; or (2) a Hg
CEMS being evaluated for relative accuracy,
you must determine the moisture content of
the flue gas and correct for moisture using
Method 4 in appendix A–3 to this part. If
correction of the measured Hg concentrations
for moisture is required, at least one Method
4 moisture determination shall be made
during each test run.
8.3.3.8 Sample Handling, Preservation,
Storage, and Transport. While the
performance criteria of this approach provide
for verification of appropriate sample
handling, it is still important that the user
consider, determine, and plan for suitable
sample preservation, storage, transport, and
holding times for these measurements.
Therefore, procedures in ASTM WK223
‘‘Guide for Packaging and Shipping
Environmental Samples for Laboratory
Analysis’’ shall be followed for all samples,
where appropriate. To avoid Hg
contamination of the samples, special
attention should be paid to cleanliness
during transport, field handling, sampling,
recovery, and laboratory analysis, as well as
during preparation of the sorbent cartridges.
Collection and analysis of blank samples
(e.g., reagent, sorbent, field, etc.,) is useful in
verifying the absence or source of
contaminant Hg.
8.3.3.9 Sample Custody. Proper
procedures and documentation for sample
chain of custody are critical to ensuring data
integrity. The chain of custody procedures in
ASTM D4840–99 ‘‘Standard Guide for
Sampling Chain-of-Custody Procedures’’
shall be followed for all samples (including
field samples and blanks).
9.0
Quality Assurance and Quality Control
Table 9–1 summarizes the QA/QC
performance criteria that are used to validate
the Hg emissions data from Method 30B
sorbent trap measurement systems.
TABLE 9–1.—QUALITY ASSURANCE/QUALITY CONTROL CRITERIA FOR METHOD 30B
QA/QC test or specification
Acceptance criteria
Frequency
Consequences if not met
Gas flow meter calibration (At 3
settings or points).
Calibration factor (Yi) at each flow
rate must be within ± 2% of the
average value (Y).
Calibration factor (Yi) must be
within ± 5% of the Y value from
the most recent 3-point calibration.
Prior to initial use and when posttest check is not within ± 5% of
Y.
After each field test. For mass
flow meters, must be done onsite, using stack gas.
Recalibrate at 3 points until the
acceptance criteria are met.
Absolute temperature measures
by sensor within ± 1.5% of a
reference sensor.
Absolute pressure measured by
instrument within ± 10 mm Hg
of reading with a mercury barometer.
≤ 4% of target sampling rate ........
Prior to initial use and before
each test thereafter.
≤ 4% of average sampling rate .....
Establish minimum dilution (if any)
needed to eliminate sorbent
matrix interferences.
Average recovery between 90%
and 110% for Hg0 and HgCl2 at
each of the 2 spike concentration levels.
Each analyzer reading withini
± 10% of true value and r2
≥ 0.99.
Within ± 10% of true value ...........
After sampling ...............................
Prior to analyzing any field samples; repeat for each type of
sorbent used.
Prior to analyzing field samples
and prior to use of new sorbent
media.
Analysis of continuing calibration
verification standard (CCVS).
Within ± 10% of true value ...........
Following daily calibration, after
analyzing ≤10 field samples,
and at end of each set of analyses.
Test run total sample volume ........
Within ± 20% of total volume sampled during field recovery test.
<10% of section 1 Hg mass for
Hg concentrations > 1 µg/dscm;.
Gas flow meter post-test calibration check (Single-point).
Temperature sensor calibration .....
Barometer calibration .....................
Pre-test leak check ........................
Post-test leak check ......................
Analytical matrix interference test
(wet chemical analysis, only).
Analytical bias test .........................
Multipoint analyzer calibration .......
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Analysis of independent calibration
standard.
Sorbent trap
through.
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Recalibrate gas flow meter at 3
points to determine a new value
of Y. For mass flow meters,
must be done on-site, using
stack gas. Apply the new Y
value to the field test data.
Recalibrate; sensor may not be
used until specification is met.
Prior to initial use and before
each test thereafter.
Recalibrate; instrument may not
be used until specification is
met.
Prior to sampling ..........................
Sampling shall not commence
until the leak check is passed.
Sample invalidated.*
Field sample results not validated.
Field samples shall not be analyzed until the percent recovery
criteria has been met.
On the day of analysis, before
analyzing any samples.
Recalibrate until successful.
Following daily calibration, prior to
analyzing field samples.
Each individual sample .................
Recalibrate and repeat independent standard analysis until
successful.
Recalibrate and repeat independent standard analysis, reanalyze samples until successful, if possible; for destructive
techniques, samples invalidated.
Sample invalidated.
Every sample ................................
Sample invalidated.*
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51523
TABLE 9–1.—QUALITY ASSURANCE/QUALITY CONTROL CRITERIA FOR METHOD 30B—Continued
QA/QC test or specification
Acceptance criteria
Paired sorbent trap agreement ......
Sample analysis .............................
Frequency
≤ 20% of section 1 Hg mass for
Hg concentrations ≤ 1 µg/dscm.
≤ 10% Relative Deviation (RD)
mass for Hg concentrations > 1
µg/dscm;
≤ 20% RD or ≤ 0.2 µg/dscm absolute difference for Hg concentrations ≤ 1 µg/dscm.
Within valid calibration range
(within calibration curve).
Sample analysis .............................
Within bounds of Hg0 and HgCl2
Analytical Bias Test.
Field recovery test .........................
Average recovery between 85%
and 115% for Hg0.
Consequences if not met
Every run ......................................
Run invalidated.*
All Section 1 samples where
stack Hg concentation is ≥ 0.5
µg/dscm.
Reanalyze at more concentrated
level if possible, samples invalidated if not within calibrated
range.
Expand bounds of Hg0 and HgCl2
Analytical Bias Test; if not successful, samples invalidated.
Field sample runs not validated
without successful field recovery test.
All Section 1 samples where
stack Hg concentration is ≥ 0.5
µg/dscm.
Once per field test ........................
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* And data from the pair of sorbent traps are also invalidated.
10.0 Calibration and Standardization
10.1 Only NIST-certified and NISTtraceable calibration standards (i.e.,
calibration gases, solutions, etc.) shall be
used for the spiking and analytical
procedures in this method.
10.2 Gas Flow Meter Calibration.
10.2.1 Preliminaries. The manufacturer or
equipment supplier of the gas flow meter
should perform all necessary set-up, testing,
programming, etc., and should provide the
end user with any necessary instructions, to
ensure that the meter will give an accurate
readout of dry gas volume in standard cubic
meters for this method.
10.2.2 Initial Calibration. Prior to its
initial use, a calibration of the gas flow meter
shall be performed. The initial calibration
may be done by the manufacturer, by the
equipment supplier, or by the end user. If the
flow meter is volumetric in nature (e.g., a dry
gas meter), the manufacturer or end user may
perform a direct volumetric calibration using
any gas. For a mass flow meter, the
manufacturer, equipment supplier, or end
user may calibrate the meter using either: (1)
A bottled gas mixture containing 12 ±0.5%
CO2, 7 ±0.5% O2, and balance N2 (when this
method is applied to coal-fired boilers); (2) a
bottled gas mixture containing CO2, O2, and
N2 in proportions representative of the
expected stack gas composition; or (3) the
actual stack gas.
10.2.2.1 Initial Calibration Procedures.
Determine an average calibration factor (Y)
for the gas flow meter by calibrating it at
three sample flow rate settings covering the
range of sample flow rates at which the
sampling system will be operated. You may
either follow the procedures in section 10.3.1
of Method 5 in appendix A–3 to this part or
in section 16 of Method 5 in appendix A–3
to this part. If a dry gas meter is being
calibrated, use at least five revolutions of the
meter at each flow rate.
10.2.2.2 Alternative Initial Calibration
Procedures. Alternatively, you may perform
the initial calibration of the gas flow meter
using a reference gas flow meter (RGFM). The
RGFM may be: (1) A wet test meter calibrated
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according to section 10.3.1 of Method 5 in
appendix A–3 to this part; (2) a gas flow
metering device calibrated at multiple flow
rates using the procedures in section 16 of
Method 5 in appendix A–3 to this part; or (3)
a NIST-traceable calibration device capable
of measuring volumetric flow to an accuracy
of 1 percent. To calibrate the gas flow meter
using the RGFM, proceed as follows: While
the Method 30B sampling system is sampling
the actual stack gas or a compressed gas
mixture that simulates the stack gas
composition (as applicable), connect the
RGFM to the discharge of the system. Care
should be taken to minimize the dead
volume between the gas flow meter being
tested and the RGFM. Concurrently measure
dry stack gas volume with the RGFM and the
flow meter being calibrated for at least 10
minutes at each of three flow rates covering
the typical range of operation of the sampling
system. For each set of concurrent
measurements, record the total sample
volume, in units of dry standard cubic meters
(dscm), measured by the RGFM and the gas
flow meter being tested.
10.2.2.3 Initial Calibration Factor.
Calculate an individual calibration factor Yi
at each tested flow rate from section 10.2.2.1
or 10.2.2.2 of this method (as applicable) by
taking the ratio of the reference sample
volume to the sample volume recorded by
the gas flow meter. Average the three Yi
values, to determine Y, the calibration factor
for the flow meter. Each of the three
individual values of Yi must be within ±0.02
of Y. Except as otherwise provided in
sections 10.2.2.4 and 10.2.2.5 of this method,
use the average Y value from the initial 3point calibration to adjust subsequent gas
volume measurements made with the gas
flow meter.
10.2.2.4 Pretest On-Site Calibration Check
(Optional). For a mass flow meter, if the most
recent 3-point calibration of the flow meter
was performed using a compressed gas
mixture, you may want to conduct the
following on-site calibration check prior to
testing, to ensure that the flow meter will
accurately measure the volume of the stack
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gas: While sampling stack gas, check the
calibration of the flow meter at one
intermediate flow rate setting representative
of normal operation of the sampling system.
If the pretest calibration check shows that the
value of Yi, the calibration factor at the tested
flow rate, differs from the current value of Y
by more than 5 percent, perform a full 3point recalibration of the meter using stack
gas to determine a new value of Y, and
(except as otherwise provided in section
10.2.2.5 of this method) apply the new Y
value to the data recorded during the field
test.
10.2.2.5 Post-Test Calibration Check.
Check the calibration of the gas flow meter
following each field test at one intermediate
flow rate setting, either at, or in close
proximity to, the average sample flow rate
during the field test. For dry gas meters,
ensure at least three revolutions of the meter
during the calibration check. For mass flow
meters, this check must be performed before
leaving the test site, while sampling stack
gas. If a one-point calibration check shows
that the value of Yi at the tested flow rate
differs by more than 5 percent from the
current value of Y, repeat the full 3-point
calibration procedure to determine a new
value of Y, and apply the new Y value to the
gas volume measurements made with the gas
flow meter during the field test that was just
completed. For mass flow meters, perform
the 3-point recalibration while sampling
stack gas.
10.3 Thermocouples and Other
Temperature Sensors. Use the procedures
and criteria in Section 10.3 of Method 2 in
Appendix A–1 to this part to calibrate instack temperature sensors and
thermocouples. Dial thermometers shall be
calibrated against mercury-in-glass
thermometers. Calibrations must be
performed prior to initial use and before each
field test thereafter. At each calibration point,
the absolute temperature measured by the
temperature sensor must agree to within ±1.5
percent of the temperature measured with the
reference sensor, otherwise the sensor may
not continue to be used.
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11.0 Analytical Procedures
The analysis of Hg in the field and quality
control samples may be conducted using any
instrument or technology capable of
quantifying total Hg from the sorbent media
and meeting the performance criteria in this
method. Because multiple analytical
approaches, equipment and techniques are
appropriate for the analysis of sorbent traps,
it is not possible to provide detailed,
technique-specific analytical procedures. As
they become available, detailed procedures
for a variety of candidate analytical
approaches will be posted at https://
www.epa.gov/ttn/emc.
11.1 Analytical System Calibration.
Perform a multipoint calibration of the
analyzer at three or more upscale points over
the desired quantitative range (multiple
calibration ranges shall be calibrated, if
necessary). The field samples analyzed must
fall within a calibrated, quantitative range
and meet the performance criteria specified
below. For samples suitable for aliquotting, a
series of dilutions may be needed to ensure
that the samples fall within a calibrated
range. However, for sorbent media samples
consumed during analysis (e.g., when using
thermal desorption techniques), extra care
must be taken to ensure that the analytical
system is appropriately calibrated prior to
sample analysis. The calibration curve
range(s) should be determined such that the
levels of Hg mass expected to be collected
and measured will fall within the calibrated
range. The calibration curve may be
generated by directly introducing standard
solutions into the analyzer or by spiking the
standards onto the sorbent media and then
introducing into the analyzer after preparing
the sorbent/standard according to the
particular analytical technique. For each
calibration curve, the value of the square of
the linear correlation coefficient, i.e., r2, must
be ≥0.99, and the analyzer response must be
within ±10 percent of the reference value at
each upscale calibration point. Calibrations
must be performed on the day of the analysis,
before analyzing any of the samples.
Following calibration, an independent
standard shall be analyzed. The measured
value of the independently prepared
standard must be within ±10 percent of the
expected value.
11.2 Sample Preparation. Carefully
separate the sections of each sorbent trap.
Combine for analysis all materials associated
with each section; any supporting substrate
that the sample gas passes through prior to
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entering a media section (e.g., glass wool
separators, acid gas traps, etc.) must be
analyzed with that segment.
11.3 Field Sample Analyses. Analyze the
sorbent trap samples following the same
procedures that were used for conducting the
Hg0 and HgCl2 analytical bias tests. The
individual sections of the sorbent trap and
their respective components must be
analyzed separately (i.e., section 1 and its
components, then section 2 and its
components). All sorbent trap section 1
sample analyses must be within the
calibrated range of the analytical system. For
wet analyses, the sample can simply be
diluted to fall within the calibrated range.
However, for the destructive thermal
analyses, samples that are not within the
calibrated range cannot be re-analyzed. As a
result, the sample cannot be validated, and
another sample must be collected. It is
strongly suggested that the analytical system
be calibrated over multiple ranges so that
thermally analyzed samples do fall within
the calibrated range. The total mass of Hg
measured in each sorbent trap section 1 must
also fall within the lower and upper mass
limits established during the initial Hg0 and
HgCl2 analytical bias test. If a sample is
analyzed and found to fall outside of these
limits, it is acceptable for an additional Hg0
and HgCl2 analytical bias test to be performed
that now includes this level. However, some
samples (e.g., the mass collected in trap
section 2 or the mass collected in trap section
1 when the stack gas concentration is <0.5
µg/m3), may have Hg levels so low that it
may not be possible to quantify them in the
analytical system’s calibrated range. Because
a reliable estimate of these low-level Hg
measurements is necessary to fully validate
the emissions data, the MDL (see section
8.2.2.1 of this method) is used to establish
the minimum amount that can be detected
and reported. If the measured mass or
concentration is below the lowest point in
the calibration curve and above the MDL, the
analyst must do the following: estimate the
mass or concentration of the sample based on
the analytical instrument response relative to
an additional calibration standard at a
concentration or mass between the MDL and
the lowest point in the calibration curve.
This is accomplished by establishing a
response factor (e.g., area counts per Hg mass
or concentration) and estimating the amount
of Hg present in the sample based on the
analytical response and this response factor.
Example: The analysis of a particular
sample results in a measured mass above the
MDL, but below the lowest point in the
calibration curve which is 10 ng. An MDL of
1.3 ng Hg has been established by the MDL
study. A calibration standard containing 5 ng
of Hg is analyzed and gives an analytical
response of 6,170 area counts, which equates
to a response factor of 1,234 area counts/ng
Hg. The analytical response for the sample is
4,840 area counts. Dividing the analytical
response for the sample (4,840 area counts)
by the response factor gives 3.9 ng Hg, which
is the estimated mass of Hg in the sample.
11.4 Analysis of Continuing Calibration
Verification Standard (CCVS). After no more
than 10 samples and at the end of each set
of analyses, a continuing calibration
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verification standard must be analyzed. The
measured value of the continuing calibration
standard must be within ±10 percent of the
expected value.
11.5 Blanks. The analysis of blanks is
optional. The analysis of blanks is useful to
verify the absence of, or an acceptable level
of, Hg contamination. Blank levels should be
considered when quantifying low Hg levels
and their potential contribution to meeting
the sorbent trap section 2 breakthrough
requirements; however, correcting sorbent
trap results for blank levels is prohibited.
12.0 Calculations and Data Analysis
You must follow the procedures for
calculation and data analysis listed in this
section.
12.1 Nomenclature. The terms used in the
equations are defined as follows:
B = Breakthrough (%).
Bws = Moisture content of sample gas as
measured by Method 4, percent/100.
Ca = Concentration of Hg for the sample
collection period, for sorbent trap ‘‘a’’
(µg/dscm).
Cb = Concentration of Hg for the sample
collection period, for sorbent trap ‘‘b’’
(µg/dscm).
Cd = Hg concentration, dry basis (µg/dscm).
Crec = Concentration of spiked compound
measured (µg/m3).
Cw = Hg concentration, wet basis (µg/m3).
m1 = Mass of Hg measured on sorbent trap
section 1 (µg).
m2 = Mass of Hg measured on sorbent trap
section 2 (µg).
mrecovered = Mass of spiked Hg recovered in
Analytical Bias or Field Recovery Test
(µg).
ms = Total mass of Hg measured on spiked
trap in Field Recovery Test (µg).
mspiked = Mass of Hg spiked in Analytical Bias
or Field Recovery Test (µg).
mu = Total mass of Hg measured on unspiked
trap in Field Recovery Test (µg).
R = Percentage of spiked mass recovered (%).
RD = Relative deviation between the Hg
concentrations from traps ‘‘a’’ and ‘‘b’’
(%).
vs = Volume of gas sampled, spiked trap in
Field Recovery Test (dscm).
Vt = Total volume of dry gas metered during
the collection period (dscm); for the
purposes of this method, standard
temperature and pressure are defined as
20 °C and 760 mm Hg, respectively.
vu = Volume of gas sampled, unspiked trap
in Field Recovery Test (dscm).
12.2 Calculation of Spike Recovery
(Analytical Bias Test). Calculate the percent
recovery of Hg0 and HgCl2 using Equation
30B–1.
R=
m recovered
× 100
mspiked
Eq. 30B-1
12.3 Calculation of Breakthrough. Use
Equation 30B–2 to calculate the percent
breakthrough to the second section of the
sorbent trap.
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B=
m2
× 100
m1
07SER2
Eq. 30B-2
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10.4 Barometer. Calibrate against a
mercury barometer as per Section 10.6 of
Method 5 in appendix A–3 to this part.
Calibration must be performed prior to initial
use and before each test program, and the
absolute pressure measured by the barometer
must agree to within +10 mm Hg of the
pressure measured by the mercury barometer,
otherwise the barometer may not continue to
be used.
10.5 Other Sensors and Gauges. Calibrate
all other sensors and gauges according to the
procedures specified by the instrument
manufacturer(s).
10.6 Analytical System Calibration. See
Section 11.1 of this method.
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12.4 Calculation of Hg Concentration.
Calculate the Hg concentration measured
with sorbent trap ‘‘a’’, using Equation 30B–
3.
Ca =
(m1 + m 2 )
Vt
C w = Cd × (1 − Bws )
Eq. 30B-4
12.6 Calculation of Paired Trap
Agreement. Calculate the relative deviation
(RD) between the Hg concentrations
measured with the paired sorbent traps using
Equation 30B–5.
Ca − C b
Ca + C b
× 100
Eq. 30B-5
Eq. 30B-6
R=
Crec × vs
× 100
mspiked
calibration curve, continuing calibration
performance, sample results within
calibration curve and bounds of Hg0 and
HgCl2 analytical bias test). Complete data
validation requirements are summarized in
Table 9–1.
13.0 Method Performance
How do I validate my data? Measurement
data are validated using initial, one-time
laboratory tests coupled with test programspecific tests and procedures. The analytical
matrix interference test and the Hg0 and
HgCl2 analytical bias test described in
Section 8.2 are used to verify the
appropriateness of the selected analytical
approach(es) as well as define the valid
working ranges for sample analysis. The field
recovery test serves to verify the performance
of the combined sampling and analysis as
applied for each test program. Field test
samples are validated by meeting the above
requirements as well as meeting specific
sampling requirements (i.e., leak checks,
paired train agreement, total sample volume
agreement with field recovery test samples)
and analytical requirements (i.e., valid
14.0
Pollution Prevention [Reserved]
15.0
Eq. 30B-7
Waste Management [Reserved]
16.0
References
1. EPA Traceability Protocol for
Qualification and Certification of Elemental
Mercury Gas Generators, expected
publication date December 2008, see
www.epa.gov/ttn/emc.
2. EPA Traceability Protocol for
Qualification and Certification of Oxidized
Mercury Gas Generators, expected
publication date December 2008, see
www.epa.gov/ttn/emc.
3. EPA Traceability Protocol for Assay and
Certification of Gaseous Calibration
Standards, expected revision publication
date December 2008, see www.epa.gov/ttn/
emc.
17.0
Figures and Tables
BILLING CODE 6560–50–C
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12.7 Calculation of Measured Spike Hg
Concentration (Field Recovery Test).
Calculate the measured spike concentration
using Equation 30B–6.
ms m u
−
vs
vu
Then calculate the spiked Hg recovery, R,
using Equation 30B–7.
Eq. 30B-3
For sorbent trap ‘‘b’’, replace ‘‘Ca ’’ with
‘‘Cb ’’ in Equation 30B–3. Report the average
concentration, i.e., 1⁄2 (Ca + Cb).
12.5 Moisture Correction. Use Equation
30B–4 if your measurements need to be
corrected to a wet basis.
RD =
Crec =
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3. Amend Performance Specification
12A in Appendix B to part 60 by
revising sections 8.6.2, 8.6.4, 8.6.5, and
8.6.6.1 to read as follows:
I
Performance Specification 12A—
Specifications and Test Procedures for Total
Vapor Phase Mercury Continuous Emission
Monitoring Systems in Stationary Sources
*
*
*
*
*
8.6.2 RM. Unless otherwise specified in
an applicable subpart of the regulations, use
Method 29, Method 30A, or Method 30B in
appendix A to this part or American Society
of Testing and Materials (ASTM) Method
D6784–02 (incorporated by reference, see
§ 60.17) as the RM for Hg concentration. Do
not include the filterable portion of the
sample when making comparisons to the
CEMS results. When Method 29, Method
30B, or ASTM D6784–02 is used, conduct the
RM test runs with paired or duplicate
sampling systems. When Method 30A is
used, paired sampling systems are not
required. If the RM and CEMS measure on a
different moisture basis, data derived with
Method 4 in appendix A to this part shall
also be obtained during the RA test.
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*
*
*
*
*
8.6.4 Number and Length of RM and
Tests. Conduct a minimum of nine RM test
runs. When Method 29, Method 30B, or
ASTM D6784–02 is used, only test runs for
which the paired RM trains meet the relative
deviation criteria (RD) of this PS shall be
used in the RA calculations. In addition, for
Method 29 and ASTM D6784–02, use a
minimum sample time of 2 hours and for
Method 30A use a minimum sample time of
30 minutes.
Note: More than nine sets of RM tests may
be performed. If this option is chosen, paired
RM test results may be excluded so long as
the total number of paired RM test results
used to determine the CEMS RA is greater
than or equal to nine. However, all data must
be reported including the excluded data.
8.6.5 Correlation of RM and CEMS Data.
Correlate the CEMS and the RM test data as
to the time and duration by first determining
from the CEMS final output (the one used for
reporting) the integrated average pollutant
concentration for each RM test period.
Consider system response time, if important,
and confirm that the results are on a
consistent moisture basis with the RM test.
Then, compare each integrated CEMS value
against the corresponding RM value. When
Method 29, Method 30A, Method 30B, or
ASTM D6784–02 is used, compare each
CEMS value against the corresponding
average of the paired RM values.
8.6.6 * * *
8.6.6.1 When Method 29, Method 30B, or
ASTM D6784–02 is used, outliers are
identified through the determination of
relative deviation (RD) of the paired RM tests.
Data that do not meet the criteria should be
flagged as a data quality problem. The
primary reason for performing paired RM
sampling is to ensure the quality of the RM
data. The percent RD of paired data is the
parameter used to quantify data quality.
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Determine RD for two paired data points as
follows:
RD =
Ca − C b
Ca + C b
× 100
Eq. 12A-1
where Ca and Cb are concentration values
determined from each of the two samples,
respectively.
*
*
*
*
*
PART 72—PERMITS REGULATION
4. The authority citation for part 72
continues to read as follows:
I
Authority: 42 U.S.C. 7601 and 7651, et seq.
5. Revise the definition of ‘‘sorbent
trap monitoring system’’ in § 72.2 as
follows:
I
§ 72.2
Definitions.
*
*
*
*
*
Sorbent trap monitoring system
means the equipment required by part
75 of this chapter for the continuous
monitoring of Hg emissions, using
paired sorbent traps containing iodated
charcoal (IC) or other suitable reagents.
This excepted monitoring system
consists of a probe, the paired sorbent
traps, an umbilical line, moisture
removal components, an air tight
sample pump, a gas flow meter, and an
automated data acquisition and
handling system. The monitoring
system samples the stack gas at a rate
proportional to the stack gas volumetric
flowrate. The sampling is a batch
process. Using the sample volume
measured by the gas flow meter and the
results of the analyses of the sorbent
traps, the average mercury
concentration in the stack gas for the
sampling period is determined, in units
of micrograms per dry standard cubic
meter (µg/dscm). Mercury mass
emissions for each hour in the sampling
period are calculated using the average
Hg concentration for that period, in
conjunction with contemporaneous
hourly measurements of the stack gas
flow rate, corrected for the stack
moisture content.
*
*
*
*
*
PART 75—CONTINUOUS EMISSION
MONITORING
6. The authority citation for part 75
continues to read as follows:
I
Authority: 42 U.S.C. 7601, 7651k, and
7651k note.
7. Amend § 75.15 as follows:
a. Revise paragraph (f);
b. Revise paragraph (i); and
c. Add new paragraph (k).
The revisions and additions read as
follows:
I
I
I
I
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§ 75.15 Special provisions for measuring
Hg mass emissions using the excepted
sorbent trap monitoring methodology.
*
*
*
*
*
(f) At the beginning and end of each
sample collection period, and at least
once in each unit operating hour during
the collection period, the gas flow meter
reading shall be recorded.
*
*
*
*
*
(i) All unit operating hours for which
valid Hg concentration data are obtained
with the primary sorbent trap
monitoring system (as verified using the
quality assurance procedures in
appendix K to this part) shall be
reported in the electronic quarterly
report under § 75.84(f). For hours in
which data from the primary monitoring
system are invalid, the owner or
operator may, in accordance with
§ 75.20(d), report valid Hg concentration
data from: A certified redundant backup
CEMS or sorbent trap monitoring
system; a certified non-redundant
backup CEMS or sorbent trap
monitoring system; or an applicable
reference method under § 75.22. If no
quality-assured Hg concentration are
available for a particular hour, the
owner or operator shall report the
appropriate substitute data value in
accordance with § 75.39.
*
*
*
*
*
(k) During each RATA of a sorbent
trap monitoring system, the type of
sorbent material used by the traps shall
be the same as for daily operation of the
monitoring system. A new pair of traps
shall be used for each RATA run.
However, the size of the traps used for
the RATA may be smaller than the traps
used for daily operation of the system.
*
*
*
*
*
I 8. Amend § 75.20 by adding new
paragraph (d)(2)(ix) to read as follows:
§ 75.20 Initial certification and
recertification procedures.
*
*
*
*
*
(d)* * *
(2)* * *
(ix) For non-redundant backup Hg
CEMS and sorbent trap monitoring
systems, and for like-kind replacement
Hg analyzers, the following provisions
apply in addition to, or, in some cases,
in lieu of, the general requirements in
paragraphs (d)(2)(i) through (d)(2)(viii)
of this section:
(A) When a certified sorbent trap
monitoring system is brought into
service as a regular non-redundant
backup monitoring system, the system
shall be operated according to the
procedures in § 75.15 and appendix K of
this part;
(B) When a regular non-redundant
backup Hg CEMS or a like-kind
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replacement Hg analyzer is brought into
service, a linearity check with elemental
Hg standards, as described in paragraph
(c)(1)(ii) of this section and section 6.2
of appendix A of this part, and a singlepoint system integrity check, as
described in section 2.6 of appendix B
of this part, shall be performed.
Alternatively, a 3-level system integrity
check, as described in paragraph
(c)(1)(vi) of this section and paragraph
(g) of section 6.2 in appendix A of this
part, may be performed in lieu of these
two tests.
(C) The weekly single-point system
integrity checks described in section 2.6
of appendix B of this part are required
as long as a non-redundant backup Hg
CEMS or like-kind replacement Hg
analyzer remains in service, unless the
daily calibrations of the Hg analyzer are
done using a NIST-traceable source of
oxidized Hg.
*
*
*
*
*
I 9. Amend § 75.57 by revising
paragraph (j)(7) to read as follows:
§ 75.57
General recordkeeping provisions.
*
*
*
*
*
(j) * * *
(7) Record the gas flow meter reading
(in dscm, rounded to the nearest
hundreth) at the beginning and end of
the collection period and at least once
in each unit operating hour during the
collection period.
*
*
*
*
*
I 10. Amend § 75.81 by revising
paragraph (a)(1) to read as follows:
§ 75.81 Monitoring of Hg mass emissions
and heat input at the unit level.
*
*
*
*
(a) * * *
(1) A Hg concentration monitoring
system (as defined in § 72.2 of this
chapter) or a sorbent trap monitoring
system (as defined in § 72.2 of this
chapter), to measure the mass
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*
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concentration of total vapor phase Hg in
the flue gas, including the elemental
and oxidized forms of Hg, in
micrograms per standard cubic meter
(µg/scm); and
*
*
*
*
*
I 11. Amend § 75.84 by revising
paragraph (f)(1)(ii)(J) to read as follows:
§ 75.84
Recordkeeping and Reporting.
*
*
*
*
*
(f) * * *
(1) * * *
(ii) * * *
(J) For units using sorbent trap
monitoring systems, the hourly gas flow
meter readings taken between the initial
and final meter readings for the data
collection period; and
*
*
*
*
*
Appendix A to Part 75—[Amended]
12. Amend Appendix A to part 75 by
removing the twentieth sentence in
paragraph (a) of section 6.5.7 which
currently reads ‘‘For the RATA of a
sorbent trap monitoring system, use the
same size trap that is used for daily
operation of the monitoring system.’’
and adding in its place ‘‘For the RATA
of a sorbent trap monitoring system, the
type of sorbent material used by the
traps shall be the same as for daily
operation of the monitoring system;
however, the size of the traps used for
the RATA may be smaller than the traps
used for daily operation of the system.’’.
I 13. Amend Appendix B to part 75 by
revising section 1.5.2 to read as follows:
I
Appendix B to Part 75—Quality
Assurance and Quality Control
Procedures
*
*
*
*
*
1.5.2 Monitoring System Integrity and Data
Quality
Explain the procedures used to perform the
leak checks when sorbent traps are placed in
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service and removed from service. Also
explain the other QA procedures used to
ensure system integrity and data quality,
including, but not limited to, gas flow meter
calibrations, verification of moisture removal,
and ensuring air-tight pump operation. In
addition, the QA plan must include the data
acceptance and quality control criteria in
section 8 of appendix K to this part. All
reference meters used to calibrate the gas
flow meters (e.g., wet test meters) shall be
periodically recalibrated. Annual, or more
frequent, recalibration is recommended. If a
NIST–traceable calibration device is used as
a reference flow meter, the QA plan must
include a protocol for ongoing maintenance
and periodic recalibration to maintain the
accuracy and NIST–traceability of the
calibrator.
*
*
*
*
*
14. Amend Appendix K to part 75 as
follows:
I a. Amend section 5.1 by revising
Figure K–1;
I b. Revise section 5.1.3;
I c. Revise section 5.1.5;
I d. Revise section 7.1.3;
I e. Revise section 7.2.3;
I f. Revise section 7.2.5;
I g. Amend section 8.0 by revising
Table K–1;
I h. Revise section 9.2;
I i. Revise section 10.4;
I j. Remove and reserve section 11.5;
I k. Revise section 11.6; and
I l. Revise section 11.7.
The revisions and additions read as
follows:
I
Appendix K to Part 75—Quality
Assurance and Operating Procedures
for Sorbent Trap Monitoring Systems
*
5.1
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5.1.3 Moisture Removal Device
A robust moisture removal device or
system, suitable for continuous duty (such as
a Peltier cooler), shall be used to remove
water vapor from the gas stream prior to
entering the gas flow meter.
*
*
*
*
*
5.1.5 Gas Flow Meter
A gas flow meter (such as a dry gas meter,
thermal mass flow meter, or other suitable
measurement device) shall be used to
determine the total sample volume on a dry
basis, in units of standard cubic meters. The
meter must be sufficiently accurate to
measure the total sample volume to within 2
percent and must be calibrated at selected
flow rates across the range of sample flow
rates at which the sorbent trap monitoring
system typically operates. The gas flow meter
shall be equipped with any necessary
auxiliary measurement devices (e.g.,
temperature sensors, pressure measurement
devices) needed to correct the sample volume
to standard conditions.
*
*
*
*
*
7.1.3 Pre-test Leak Check
Perform a leak check with the sorbent traps
in place. Draw a vacuum in each sample
train. Adjust the vacuum in the sample train
to ∼15″ Hg. Using the gas flow meter,
determine leak rate. The leakage rate must
not exceed 4 percent of the target sampling
rate. Once the leak check passes this
criterion, carefully release the vacuum in the
sample train then seal the sorbent trap inlet
until the probe is ready for insertion into the
stack or duct.
readings. Also, record the stack gas flow rate,
as measured by the certified flow monitor,
and the ratio of the stack gas flow rate to the
sample flow rate. Adjust the sampling flow
rate to maintain proportional sampling, i.e.,
keep the ratio of the stack gas flow rate to
sample flow rate constant, to within ±25
percent of the reference ratio from the first
hour of the data collection period (see section
11 of this appendix).
*
*
*
7.2.5
Essential Operating Data
*
*
*
*
7.2.3 Flow Rate Control
Set the initial sample flow rate at the target
value from section 7.1.1 of this appendix.
Record the initial gas flow meter reading,
stack temperature (if needed to convert to
standard conditions), meter temperatures (if
needed), etc. Then, for every operating hour
during the sampling period, record the date
and time, the sample flow rate, the gas flow
meter reading, the stack temperature (if
needed), the flow meter temperatures (if
needed), temperatures of heated equipment
such as the vacuum lines and the probes (if
heated), and the sampling system vacuum
*
*
*
Obtain and record any essential operating
data for the facility during the test period,
e.g., the barometric pressure for correcting
the sample volume measured by a dry gas
meter to standard conditions. At the end of
the data collection period, record the final
gas flow meter reading and the final values
of all other essential parameters.
*
8.0
*
*
*
*
* * *
TABLE K–1.—QUALITY ASSURANCE/QUALITY CONTROL CRITERIA FOR SORBENT TRAP MONITORING SYSTEMS
QA/QC test or specification
Acceptance criteria
Frequency
Consequences if not met
Pre-test leak check ........................
≤4% of target sampling rate .........
Prior to Sampling ..........................
Post-test leak check ......................
Ratio of stack gas flow rate to
sample flow rate.
≤4% of average sampling rate .....
Maintain within ±25% of initial
ratio from first hour of data collection period.
≤5% of Section 1 Hg mass ..........
After sampling ...............................
Every hour throughout data collection period.
Sampling shall not commence
until the leak check is passed.
Sample check invalidated.**
Case-by-case evaluation.
Every sample ................................
Sample invalidated.**
≤10% Relative Deviation (RD) .....
Average recovery between 85%
and 115% for each of the 3
spike concentration levels.
Each analyzer reading within
±10% of true value and r2 ≥0.99.
Within ±10% of true value ............
Every sample ................................
Prior to analyzing field samples
and prior to use of new sorbent
media.
On the day of analysis, before
analyzing any samples.
Following daily calibration, prior to
analyzing field.
Sample invalidated.**
Field samples shall not be analyzed until the percent recovery
criterion has been met.
Recalibrate until successful.
75–125% of spike amount ............
Every sample ................................
RA ≤20.0% or Mean difference
≤1.0 µgm/dscm for low emitters.
Calibration factor (Y) within ±5%
of average value from the initial
(3-point) calibration.
Absolute temperature measured
by sensor within ±1.5% of a reference sensor.
Absolute pressure measured by
instrument within ±10 mm Hg of
reading with a mercury barometer.
For initial certification and annually thereafter.
Prior to initial use and at least
quarterly thereafter.
Sorbent trap section 2 breakthrough.
Paired sorbent trap agreement ......
Spike recovery study .....................
Multipoint analyzer calibration .......
Analysis of independent calibration
standard.
Spike recovery from section 3 of
sorbent trap.
RATA .............................................
Gas flow meter calibration (At 3
settings initially, and 1 setting
thereafter).
Temperature sensor calibration .....
Barometer calibration .....................
Prior to initial use and at least
quarterly thereafter.
Prior to initial use and at least
quarterly thereafter.
Recalibrate and repeat independent standard analysis samples until successful.
Sample invalidated.**
Data from the system are invalidated until a RATA is passed.
Recalibrate the meter at three
settings to determine a new
value of Y.
Recalibrate. Sensor may not be
used until specification is met.
Recalibrate. Instrument may not
be used until specification is
met.
** And data from the pair of sorbent traps are also invalidated.
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9.2
*
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Gas Flow Meter Calibration
9.2.1 Preliminaries. The manufacturer or
supplier of the gas flow meter should
perform all necessary set-up, testing,
programming, etc., and should provide the
end user with any necessary instructions, to
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ensure that the meter will give an accurate
readout of dry gas volume in standard cubic
meters for the particular field application.
9.2.2 Initial Calibration. Prior to its initial
use, a calibration of the flow meter shall be
performed. The initial calibration may be
done by the manufacturer, by the equipment
supplier, or by the end user. If the flow meter
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is volumetric in nature (e.g., a dry gas meter),
the manufacturer, equipment supplier, or end
user may perform a direct volumetric
calibration using any gas. For a mass flow
meter, the manufacturer, equipment supplier,
or end user may calibrate the meter using a
bottled gas mixture containing 12 ± 0.5%
CO2, 7 ± 0.5% O2, and balance N2, or these
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or 9.2.2.2 of this appendix (as applicable), by
taking the ratio of the reference sample
volume to the sample volume recorded by
the gas flow meter. Average the three Yi
values, to determine Y, the calibration factor
for the flow meter. Each of the three
individual values of Yi must be within ±0.02
of Y. Except as otherwise provided in
sections 9.2.2.4 and 9.2.2.5 of this appendix,
use the average Y value from the three level
calibration to adjust all subsequent gas
volume measurements made with the gas
flow meter.
9.2.2.4 Initial On-Site Calibration Check.
For a mass flow meter that was initially
calibrated using a compressed gas mixture,
an on-site calibration check shall be
performed before using the flow meter to
provide data for this part. While sampling
stack gas, check the calibration of the flow
meter at one intermediate flow rate typical of
normal operation of the monitoring system.
Follow the basic procedures in section
9.2.2.1 or 9.2.2.2 of this appendix. If the onsite calibration check shows that the value of
Yi, the calibration factor at the tested flow
rate, differs by more than 5 percent from the
value of Y obtained in the initial calibration
of the meter, repeat the full 3-level
calibration of the meter using stack gas to
determine a new value of Y, and apply the
new Y value to all subsequent gas volume
measurements made with the gas flow meter.
9.2.2.5 Ongoing Quality Assurance.
Recalibrate the gas flow meter quarterly at
one intermediate flow rate setting
representative of normal operation of the
monitoring system. Follow the basic
procedures in section 9.2.2.1 or 9.2.2.2 of this
appendix. If a quarterly recalibration shows
that the value of Yi, the calibration factor at
the tested flow rate, differs from the current
value of Y by more than 5 percent, repeat the
full 3-level calibration of the meter to
determine a new value of Y, and apply the
new Y value to all subsequent gas volume
measurements made with the gas flow meter.
*
*
*
*
*
*
*
*
*
11.5
*
[Reserved]
11.6 Calculation of Hg Concentration
Calculate the Hg concentration for each
sorbent trap, using the following equation:
C=
M*
Vt
(Eq. K-5)
Where:
C = Concentration of Hg for the collection
period, (µgm/dscm)
M* = Total mass of Hg recovered from
sections 1 and 2 of the sorbent trap, (µg)
Vt = Total volume of dry gas metered during
the collection period, (dscm). For the
purposes of this appendix, standard
temperature and pressure are defined as
20 °C and 760 mm Hg, respectively.
11.7 Calculation of Paired Trap Agreeement
Calculate the relative deviation (RD)
between the Hg concentrations measured
with the paired sorbent traps:
RD =
Ca − C b
Ca + C b
× 100
(Eq. K-6)
Where:
RD = Relative deviation between the Hg
concentrations from traps ‘‘a’’ and ‘‘b’’
(percent)
Ca = Concentration of Hg for the collection
period, for sorbent trap ‘‘a’’ (µgm/dscm)
Cb = Concentration of Hg for the collection
period, for sorbent trap ‘‘b’’ (µgm/dscm)
*
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*
[FR Doc. 07–4147 Filed 9–6–07; 8:45 am]
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10.4 Field Sample Analysis
Analyze the sorbent trap samples following
the same procedures that were used for
conducting the spike recovery study. The
three sections of each sorbent trap must be
analyzed separately (i.e., section 1, then
section 2, then section 3). Quantify the total
mass of Hg for each section based on
analytical system response and the
calibration curve from section 10.1 of this
appendix. Determine the spike recovery from
sorbent trap section 3. The spike recovery
must be no less than 75 percent and no
greater than 125 percent. To report the final
Hg mass for each trap, add together the Hg
masses collected in trap sections 1 and 2.
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same gases in proportions more
representative of the expected stack gas
composition. Mass flow meters may also be
initially calibrated on-site, using actual stack
gas.
9.2.2.1 Initial Calibration Procedures.
Determine an average calibration factor (Y)
for the gas flow meter, by calibrating it at
three sample flow rate settings covering the
range of sample flow rates at which the
sorbent trap monitoring system typically
operates. You may either follow the
procedures in section 10.3.1 of Method 5 in
appendix A–3 to part 60 of this chapter or
the procedures in section 16 of Method 5 in
appendix A–3 to part 60 of this chapter. If
a dry gas meter is being calibrated, use at
least five revolutions of the meter at each
flow rate.
9.2.2.2 Alternative Initial Calibration
Procedures. Alternatively, you may perform
the initial calibration of the gas flow meter
using a reference gas flow meter (RGFM). The
RGFM may either be: (1) A wet test meter
calibrated according to section 10.3.1 of
Method 5 in appendix A–3 to part 60; (2) a
gas flow metering device calibrated at
multiple flow rates using the procedures in
section 16 of Method 5 in appendix A–3 to
part 60; or (3) a NIST–traceable calibration
device capable of measuring volumetric flow
to an accuracy of 1 percent. To calibrate the
gas flow meter using the RGFM, proceed as
follows: While the sorbent trap monitoring
system is sampling the actual stack gas or a
compressed gas mixture that simulates the
stack gas composition (as applicable),
connect the RGFM to the discharge of the
system. Care should be taken to minimize the
dead volume between the sample flow meter
being tested and the RGFM. Concurrently
measure dry gas volume with the RGFM and
the flow meter being calibrated the for a
minimum of 10 minutes at each of three flow
rates covering the typical range of operation
of the sorbent trap monitoring system. For
each 10-minute (or longer) data collection
period, record the total sample volume, in
units of dry standard cubic meters (dscm),
measured by the RGFM and the gas flow
meter being tested.
9.2.2.3 Initial Calibration Factor.
Calculate an individual calibration factor Yi
at each tested flow rate from section 9.2.2.1
Agencies
[Federal Register Volume 72, Number 173 (Friday, September 7, 2007)]
[Rules and Regulations]
[Pages 51494-51531]
From the Federal Register Online via the Government Printing Office [www.gpo.gov]
[FR Doc No: 07-4147]
[[Page 51493]]
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Part II
Environmental Protection Agency
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40 CFR Parts 60, 72 and 75
Two Optional Methods for Relative Accuracy Test Audits of Mercury
Monitoring Systems Installed on Combustion Flue Gas Streams and Several
Amendments to Related Mercury Monitoring Provisions; Final Rule
Federal Register / Vol. 72, No. 173 / Friday, September 7, 2007 /
Rules and Regulations
[[Page 51494]]
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ENVIRONMENTAL PROTECTION AGENCY
40 CFR Parts 60, 72 and 75
[EPA-HQ-OAR-2007-0164, FRL-8459-8]
RIN 2060-AO01
Two Optional Methods for Relative Accuracy Test Audits of Mercury
Monitoring Systems Installed on Combustion Flue Gas Streams and Several
Amendments to Related Mercury Monitoring Provisions
AGENCY: Environmental Protection Agency (EPA).
ACTION: Direct final rule.
-----------------------------------------------------------------------
SUMMARY: EPA is taking direct final action on two optional methods for
relative accuracy audits of mercury monitoring systems installed on
combustion flue gas streams and several amendments to related mercury
monitoring provisions. This action approves two optional mercury (Hg)
emissions test methods for potential use in conjunction with an
existing regulatory requirement for Hg emissions monitoring, as well as
several revisions to the mercury monitoring provisions themselves. This
action is in regard to the testing and monitoring requirements for
mercury specified in the Federal Register on May 18, 2005. Since that
publication, EPA has received numerous comments concerning the
desirability of EPA evaluating and allowing use of the measurement
techniques addressed in the two optional methods in lieu of the methods
identified in the cited Federal Register publication, as they can
produce equally acceptable measures of the relative accuracy achieved
by Hg monitoring systems. This action allows use of these two optional
methods entirely at the discretion of the owner or operator of an
affected emission source in place of the two currently specified
methods. This direct final rule also amends Performance Specification
12A by adding Methods 30A and 30B to the list of reference methods
acceptable for measuring Hg concentration and the Hg monitoring
provisions of May 18, 2005, to reflect technical insights since gained
by EPA which will help to facilitate implementation including
clarification and increased regulatory flexibility for affected
sources.
DATES: This rule is effective on November 6, 2007 without further
notice, unless EPA receives adverse comment by October 9, 2007. If EPA
receives adverse comment, EPA will publish a timely withdrawal in the
Federal Register informing the public that some or all of the
amendments in this rule will not take effect.
ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-
OAR-2007-0164, by one of the following methods:
www.regulations.gov. Follow the on-line instructions for
submitting comments.
E-mail: a-and-r-docket@epa.gov.
Fax: (202) 566-9744.
Mail: Two Optional Methods for Relative Accuracy Test
Audits of Mercury Monitoring Systems Installed on Combustion Flue Gas
Streams and Several Amendments to the Related Mercury Monitoring
Provisions, Environmental Protection Agency, Mailcode: 2822T, 1200
Pennsylvania Avenue, NW., Washington, DC 20460. Please include a total
of two copies.
Hand Delivery: EPA Docket Center, 1301 Constitution
Avenue, NW., EPA Headquarters Library, Room 3334, EPA West Building,
Washington, DC 20460. Such deliveries are only accepted during the
Docket's normal hours of operation, and special arrangements should be
made for deliveries of boxed information.
Instructions: Direct your comments to Docket ID No. EPA-HQ-OAR-
2007-0164. EPA's policy is that all comments received will be included
in the public docket without change and may be made available online at
www.regulations.gov, including any personal information provided,
unless the comment includes information claimed to be Confidential
Business Information (CBI) or other information whose disclosure is
restricted by statute. Do not submit information that you consider to
be CBI or otherwise protected through www.regulations.gov or e-mail.
The www.regulations.gov Web site is an ``anonymous access'' system,
which means EPA will not know your identity or contact information
unless you provide it in the body of your comment. If you send an e-
mail comment directly to EPA without going through www.regulations.gov,
your e-mail address will be automatically captured and included as part
of the comment that is placed in the public docket and made available
on the Internet. If you submit an electronic comment, EPA recommends
that you include your name and other contact information in the body of
your comment and with any disk or CD-ROM you submit. If EPA cannot read
your comment due to technical difficulties and cannot contact you for
clarification, EPA may not be able to consider your comment. Electronic
files should avoid the use of special characters, any form of
encryption, and be free of any defects or viruses. For additional
information about EPA's public docket, visit the EPA Docket Center
homepage at https://www.epa.gov/epahome/dockets.htm.
Docket: All documents in the docket are listed in the
www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., CBI or other information
whose disclosure is restricted by statute. Certain other material, such
as copyrighted material, will be publicly available only in hard copy.
Publicly available docket materials are available either electronically
in www.regulations.gov or in hard copy at the Two Optional Methods for
Relative Accuracy Audits of Mercury Monitoring Systems Installed on
Combustion Flue Gas Streams Air and Radiation Docket, EPA/DC, EPA West
Building, EPA Headquaters Library, Room 3334, 1301 Constitution Avenue,
NW., Washington, DC. The Public Reading Room is open from 8:30 a.m. to
4:30 p.m., Monday through Friday, excluding legal holidays. The
telephone number for the Public Reading Room is (202) 566-1744, and the
telephone number for the Air and Radiation Docket is (202) 566-1742.
FOR FURTHER INFORMATION CONTACT: Either Mr. William Grimley, Office of
Air Quality Planning and Standards, Air Quality Assessment Division,
Measurement Technology Group (E143-02), EPA, Research Triangle Park, NC
27711, telephone (919) 541-1065, facsimile number (919) 541-0516, e-
mail address: grimley.william@epa.gov or Ms. Robin Segall, Office of
Air Quality Planning and Standards, Air Quality Assessment Division,
Measurement Technology Group (E143-02), EPA, Research Triangle Park, NC
27711, telephone (919) 541-0893, facsimile number (919) 541-0516, e-
mail address: segall.robin@epa.gov.
SUPPLEMENTARY INFORMATION:
I. Why is EPA using a Direct Final Rule?
EPA is publishing this rule without a prior proposed rule because
we view this as a noncontroversial action and anticipate no adverse
comment. The most important benefit of direct final rulemaking for this
action is to provide: (1) Additional reference method options, and (2)
judicious revisions to mercury monitoring provisions specified in the
Federal Register on May 18, 2005 that, if successful, relieve affected
facilities of uncertainty regarding final emission monitoring
requirements and certification details as opposed to waiting through a
potentially protracted proposal/final
[[Page 51495]]
rulemaking process. Insofar as the two methods are concerned, EPA
believes that they contain the necessary elements to generate
acceptable data quality without being unduly burdensome. Through
experience gained from developing existing performance based methods
and trading rules, EPA has learned to identify test method criteria
significant to effective rule implementation. EPA believes each of the
two methods adopted in this action contain adequate specific criteria
and procedures essential to the accurate measurement of Hg emissions,
without adversely compromising the goals of performance-based
methodology. EPA will continue to support and advance the principles
and practicality of these methods by adding detailed method application
information to facilitate their use to the Web site www.epa.gov/
airmarkets/ as it becomes available. Since use of either of these
methods is not mandatory, but optional, there should be no objection to
their availability. Regarding the amendments to the Hg emission
monitoring provisions of 40 CFR parts 72 and 75, these amendments
reflect EPA's increased technical understanding since the May 18, 2005
rulemaking. However, in the ``Proposed Rules'' section of today's
Federal Register, we are publishing a separate document that will serve
as the proposed rule to approve provisions, if any, of this direct
final rule that receive relevant adverse comments on this direct final
rule. We will not institute a second comment period on this action. Any
parties interested in commenting must do so at this time. For further
information about commenting on this rule, see the ADDRESSES section of
this document.
If EPA receives adverse comment on one or more distinct provisions
of this rulemaking, we will publish a timely withdrawal in the Federal
Register indicating which provisions we are withdrawing and informing
the public that those provisions will not take effect. The provisions
that are not withdrawn will become effective on the date set out above,
notwithstanding adverse comment on any other provision. We would
address all public comments in a subsequent final rule based on the
proposed rule.
II. Does This Action Apply to Me?
Regulated Entities. The regulated categories and entities affected
by this direct final rule include:
------------------------------------------------------------------------
Examples of regulated
Category NAICS \a\ entities
------------------------------------------------------------------------
Industry....................... 221112 Fossil fuel-fired
electric utility steam
generating units.
Federal government............. \b\ 221122 Fossil fuel-fired
electric utility steam
generating units owned
by the Federal
government.
State/local governments........ \b\ 221122 Fossil fuel-fired
electric utility steam
generating units owned
by municipalities.
Tribal governments............. 921150 Fossil fuel-fired
electric utility steam
generating units in
Indian country.
------------------------------------------------------------------------
\a\ North American Industry Classification System.
\b\ Federal, State, or local government-owned and operated
establishments are classified according to the activity in which they
are engaged.
This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be affected by this
direct final rule. If you have any questions regarding the
applicability of this direct final rule to a particular entity, consult
either the air permit authority for the entity or your EPA regional
representative as listed in 40 CFR 63.13.
III. Where Can I Obtain a Copy of This Action?
In addition to being available in the docket, an electronic copy of
this direct final rule is also available on the World Wide Web through
the Technology Transfer Network (TTN). Following signature, a copy of
this direct final rule will be posted on the TTN's policy and guidance
page for newly proposed or promulgated rules at the following address:
https://www.epa.gov/ttn/oarpg. The TTN provides information and
technology exchange in various areas of air pollution control.
IV. How Is This Document Organized?
The information presented in this preamble is organized as
follows:
I. Why Is EPA Using a Direct Final Rule?
II. Does This Action Apply to Me?
III. Where Can I Obtain a Copy of This Action?
IV. How Is This Document Organized?
V. Background
VI. This Action
VII. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory Planning and Review
B. Paperwork Reduction Act
C. Regulatory Flexibility Act
D. Unfunded Mandates Reform Act
E. Executive Order: 13132: Federalism
F. Executive Order 13175: Consultation and Coordination With
Indian Tribal Governments
G. Executive Order 13045: Protection of Children From
Environmental Health and Safety Risks
H. Executive Order 13211: Actions That Significantly Affect
Energy Supply, Distribution, or Use
I. National Technology Transfer and Advancement Act
J. Executive Order 12898: Federal Actions To Address
Environmental Justice in Minority Populations and Low-Income
Populations
K. Congressional Review Act
V. Background
On May 18, 2005, in the preamble of the Clean Air Mercury Rule
(CAMR) (70 FR 28608), EPA stated its intention to propose and
promulgate an instrumental reference method as an alternative to the
use of ASTM Method D6784-02 (the Ontario Hydro Method) to perform
Relative Accuracy Test Audits (RATAs) of Hg continuous emission
monitoring systems (CEMS) and sorbent trap monitoring systems used to
monitor Hg emissions from coal-fired power plants.
In comments on the proposed CAMR, commenters had two primary
objections to the use of the Ontario Hydro Method as the reference test
method for RATAs. Some expressed concern that the complexity of this
wet chemical method could lead to results that would cause a properly
functioning Hg CEMS to fail a RATA. Other commenters noted that, unlike
instrumental reference methods used to audit CEMS for SO2
and NOX that provide real-time values, test results from the
Ontario Hydro Method can take weeks to be received from the laboratory.
Commenters stated that this time lag can lead to implementation
problems with regard to both missing data and emissions reporting.
Since the CAMR was promulgated, EPA has proposed changes to 40 CFR
part 75, which would allow the use of EPA Method 29, with enhanced
quality-assurance procedures, as an alternative Hg reference method (71
FR 49257; August 22, 2006). Although Method 29 is somewhat simpler than
the Ontario Hydro Method and is more familiar to stack testers and
State regulatory agencies, it is also a wet chemistry method and is,
therefore, subject to the same limitations that make the Ontario Hydro
method less than optimal for RATA testing.
In view of these considerations, EPA believes that for RATA
testing, an instrumental Hg reference method
[[Page 51496]]
would be preferable to both the Ontario Hydro Method and to Method 29.
An instrumental method would provide real-time data that would best
facilitate implementation of a mercury cap and trade program.
Therefore, this action approves a performance-based instrumental
reference method for measuring Hg emission concentrations.
Another commenter to the proposed CAMR recommended that the sorbent
trap monitoring approach, now specified in 40 CFR part 75, appendix K,
be considered for use as a reference method. Although EPA did not
commit to establishing a sorbent trap reference method at the time of
CAMR promulgation, stakeholder interest in this methodology has
increased significantly. In an August 22, 2006 Federal Register notice,
EPA solicited comment on the use of sorbent trap technology for Hg
reference method testing, and numerous supportive comments were
received. In view of this, we initiated a review of available
historical test data where concurrent measurements of Hg concentration
were made with sorbent trap systems and either the Ontario Hydro Method
or Method 29. These data, taken together with additional supporting
data from recent field tests that were performed after the CAMR was
promulgated, suggest that using the sorbent trap methodology for Hg
reference method testing is viable. The Hg sorbent trap approach is
less onerous to use than either Ontario Hydro or Method 29, and
although it does not measure real-time Hg concentrations, a thermal
technique can be used to analyze the samples on the same day that they
are collected, facilitating RATA testing in the context of a cap and
trade program. Therefore, this action also approves a sorbent trap
reference method for Hg, as an alternative to the Ontario Hydro Method
and Method 29.
This direct final rule also includes several carefully considered
amendments to the Hg emission monitoring provisions of 40 CFR parts 72
and 75. EPA believes these amendments will facilitate implementation of
the CAMR by clarifying portions of that rule and by providing added
regulatory flexibility to the affected sources.
VI. This Action
This direct final rule allows for the earliest possible use of two
optional reference test methods for measuring total vapor phase mercury
emissions from stationary sources as well as several related amendments
to the Hg monitoring provisions of the CAMR. Both an instrumental test
method and a sorbent trap test method for measurement of total vapor
phase mercury emissions are being added to Appendix A-8 of 40 CFR part
60 as approved alternatives to the Ontario Hydro Method and EPA Method
29 to perform RATAs of installed mercury monitoring systems. The two
methods are discussed below, and the related amendments are explained
in detail later in this section.
The first method being added to appendix A-8 of 40 CFR part 60
today is titled ``Method 30A--Determination of Total Vapor Phase
Mercury Emissions from Stationary Sources (Instrumental Analyzer
Procedure).'' In Method 30A, a sample of the effluent gas is
continuously extracted and conveyed to an analyzer capable of measuring
the total vapor phase Hg concentration. Elemental and oxidized mercury
(i.e., Hg\0\ and Hg+\2\) may be measured separately or
simultaneously but, for purposes of this method, total vapor phase Hg
is the sum of Hg\0\ and Hg+\2\. Method 30A provides test
program-specific verification of method performance using a dynamic
spiking approach, coupled with other performance criteria, which
include system calibration, interference testing, and system integrity/
drift checks. The dynamic spiking requirement, which is a gaseous
``method of standard additions,'' is the only part of Method 30A not
parallel to the routinely applied instrumental reference methods used
to perform relative accuracy testing of CEMS for SO2 and
NOX. The dynamic spiking procedure is included in Method 30A
to characterize measurement bias for Hg, which can be highly reactive
on a site-specific basis (i.e., for each emissions sample matrix), with
recovery criteria set to ensure that the bias is held to a minimal
level. All performance requirements of Method 30A must be met for the
data to be considered valid. The availability of an instrumental
reference method for Hg testing is consistent with the approach EPA has
taken in the successful Acid Rain and NOX Budget emissions
trading programs.
Method 30A is performance based in keeping with the criteria
established under our Notice of Intent to Implement Performance Based
Measurement Systems for Environmental Monitoring (62 FR 52098, October
6, 1997). Use of the performance-based measurement approach will allow
for continued development and application of new, improved, and more
cost-effective Hg measurement technologies while ensuring the
collection of data of known quality.
Based on EPA's experience in conducting test programs to evaluate
the procedures and performance criteria included in Method 30A, EPA
recognizes that although prototypes of all equipment needed to perform
this method have been successfully demonstrated in the field, at
present the equipment needed to follow all procedures required by the
method is commercially available only on a limited basis, and is being
further refined. One of the issues of greatest concern in the
development of an instrumental reference method for Hg has been the
design of the sampling probe. Most of the commercially-available probes
suitable for Hg measurement are very heavy (over 100 lbs.) making it
difficult to move the probe from point-to-point and port-to-port for Hg
stratification testing and/or sample traverses. Much progress is being
made in probe redesign. One manufacturer has recently developed a probe
that weighs less than 40 lbs., samples at significantly lower flow
rates, and is suitable for dynamic spiking. Additional field testing of
this probe and others currently under development is underway, and EPA
plans to continue to actively encourage equipment development and
evaluation. To encourage the use of Method 30A, including further
development of the supporting equipment, which we believe will
eventually enable source testers to perform Hg monitoring system RATAs
more efficiently and will become the reference method of choice for
many testing companies and affected sources, we are deferring the
requirement for implementation of the dynamic spiking and Hg
stratification test procedures until January 1, 2009. EPA believes this
deferral is reasonable because Hg monitoring data reported to EPA in
2009 will not be used in the trading of Hg allowances, as allowance
accounting under the CAMR does not begin until 2010. Source testers are
encouraged to use this time to acquire the necessary equipment and
familiarize themselves with these procedures. Also, for all emissions
test programs and RATAs performed under CAMR prior to January 1, 2009,
we are allowing either: (1) A 12-point traverse for sulfur dioxide
(SO2) to be substituted for a 12-point Hg traverse, in cases
where stratification testing is used to determine the appropriate
number and location of the reference method sampling points, or (2) use
of the alternate three-point traverse line (0.4, 1.2, and 2.0 meters
from the stack wall) as specified in section 8.1.3.2 of Performance
Specification 2 (40 CFR part 60, appendix B). We
[[Page 51497]]
believe that in the short-term, these temporary deferrals will
encourage the application of Method 30A and will help affected CAMR
sources meet the January 1, 2009 deadline for initial certification of
the required Hg monitoring systems. Several additional Method 30A
development considerations are worthy of note. A preliminary draft of
Method 30A was first available for public consideration on an EPA Web
site (www.epa.gov/ttn/emc/) on February 28, 2006. Since that time, EPA
and several stakeholder groups have evaluated the various technical
aspects of the method. Based on the combined laboratory and field
observations, EPA has been able to simplify several procedural
requirements that we believe are essential to the method. The dynamic
spiking requirement (for test program-specific verification of
measurement system data quality) has been reduced to only a pretest
requirement. The interference test has been made optional. The three-
point system calibration error test using Hg+\2\ has been
streamlined to a system integrity check using a zero gas and a single
upscale Hg+\2\ gas. Another change has been to relax the
Hg\0\ calibration error specification from 2 percent to 5 percent of
span, in recognition of the fact that this procedure is a check of the
entire measurement system, as well as the current knowledge regarding
the uncertainty of NIST traceable standards. EPA does plan, however, to
reconsider this specification relaxation as more field data become
available. A final consideration in development of Method 30A has been
the requirement for calibration with both Hg\0\ and Hg+\2\.
Some stakeholders have recommended that we eliminate the Hg\0\
calibration and rely solely on the Hg+\2\ calibration. EPA,
however, believes this approach would not be adequate, because if only
Hg+\2\ were used, instrument calibration response adjustment
could compensate for an unknown amount of converter inefficiency, which
would then result in an inaccurate total mercury measurement in
situations where Hg\0\ is an appreciable fraction of the total stack
gas Hg.
The second method being added to appendix A-8 of 40 CFR part 60
today is titled ``Method 30B--Use of Sorbent Traps to Measure Total
Vapor Phase Mercury Emissions from Coal-Fired Combustion Sources.'' In
Method 30B, a sample of the effluent gas is continuously drawn through
a series of tubes containing activated carbon or another sorbent
material. After sampling, the tubes are sealed. The Hg captured by the
sorbent is then either: (1) Thermally desorbed and analyzed; or (2) the
tubes are transferred to a laboratory for extraction of Hg and
analysis. Like Method 30A, Method 30B is a performance-based method and
contains performance specifications and procedures for hardware
selection and calibration, sorbent spiking, and analytical recovery/
analysis which allow for development and application of new, improved,
and more cost-effective Hg measurement technologies while still
ensuring the collection of data of known quality. In particular, Method
30B contains five key measurement performance tests designed to ensure:
(1) Selection of a sorbent and analytical technique combination capable
of quantitative collection and analysis of gaseous Hg, (2) collection
during field testing of enough Hg on each sorbent trap to be reliably
quantified, and (3) adequate performance of the method for each test
program.
In considering development of a sorbent trap-based reference
method, EPA has reviewed historical emissions data where sorbent trap
measurement systems were operated concurrently with either the Ontario
Hydro Method or Method 29 (40 CFR part 60, appendix A-8). EPA has also
conducted several field test evaluations of sorbent trap systems versus
the Ontario Hydro Method in collaboration with the Electric Power
Research Institute (EPRI). Based on these efforts, we have concluded
that a sorbent trap-based technique coupled with appropriate
performance criteria and QA procedures can provide Hg emissions data of
quality comparable to that produced by the Ontario Hydro Method. Data
supporting this conclusion are presented in the docket, EPA-HQ-OAR-
2007-0164.
As we have done for Method 30A, for Method 30B emission tests and
RATAs performed prior to January 1, 2009, we are allowing either: (1) A
12-point traverse for sulfur dioxide (SO2) to be substituted
for a 12-point Hg traverse for the stratification testing used to
determine the number and location of the reference method sampling
points, or (2) use of the alternate three-point traverse line (0.4,
1.2, and 2.0 meters from the stack wall) as specified in section
8.1.3.2 of Performance Specification 2 (40 CFR part 60, appendix B). We
also intend to extend this temporary deferral of mercury stratification
testing to application of the Ontario Hydro Method and Method 29. EPA
believes this deferral is reasonable because Hg monitoring data
reported to EPA in 2009 will not be used in the trading of Hg
allowances, as allowance accounting under the CAMR does not begin until
2010.
This direct final rule also amends Performance Specification 12A of
appendix B to part 60 by adding Methods 30A and 30B to the list of
reference methods acceptable for relative accuracy testing of Hg
emissions monitoring systems. Once this direct final rule becomes
effective, the reference methods acceptable for Hg measurement in
Performance Specification 12A will include Methods 29, 30A, 30B, and
ASTM D6784-02.
With today's action, EPA is taking the opportunity to include
several considered revisions to the Hg emission monitoring provisions
of 40 CFR parts 72 and 75 as described in detail below. EPA is
including these revisions in this direct final rule because we believe
that they will facilitate implementation of the Hg monitoring under
CAMR.
First, Sec. 75.81(a) is being revised to confirm that the Hg CEMS
and sorbent trap monitoring systems required under subpart I of part 75
are to measure the total vapor phase mass concentration of Hg in the
flue gas, including both the elemental and oxidized forms of Hg,
expressed in units of micrograms per standard cubic meter ([mu]g/scm).
Although it is generally understood that total vapor phase Hg is the
regulated pollutant under CAMR, it recently was brought to EPA's
attention that subpart I of part 75 does not explicitly state that Hg
monitoring systems only need to measure total vapor phase Hg. The
amended language in Sec. 75.81(a) clarifies this.
Second, paragraph (i) in Sec. 75.15 is being revised and a new
paragraph (d)(2)(ix) is being added to Sec. 75.20, to codify the rules
for using optional non-redundant (``cold'') backup Hg monitoring
systems and like-kind replacement Hg analyzers, when the primary Hg
monitoring system is unable to provide quality-assured data. For the
other types of monitoring systems required by part 75, these monitoring
options have been in place since May 1999 (see 64 FR 28597, May 26,
1999). Today's action simply extends these provisions to Hg monitoring
systems. Through the years, the regulated community has found these
backup monitoring options to be beneficial, in that they minimize the
use of missing data substitution procedures during outages of the
primary monitoring system.
In particular, Sec. 75.20(d)(2)(ix) specifies that a non-redundant
backup Hg monitoring system can either be a Hg CEMS or a sorbent trap
monitoring system. The non-redundant backup Hg
[[Page 51498]]
monitoring system must be initially certified at each unit or stack
location where it will be used, in accordance with Sec.
75.20(d)(2)(i). For a non-redundant backup Hg CEMS, all of the initial
certification tests specified in Sec. 75.20(c)(1) are required, except
for the 7-day calibration error test. However, for ongoing quality
assurance (QA), a RATA is required only once every two years (8
calendar quarters), as specified in Sec. 75.20(d)(2)(vi). For a non-
redundant backup sorbent trap monitoring system, a RATA is required for
initial certification, and once every two years thereafter for ongoing
QA.
When a certified non-redundant backup Hg CEMS or a like-kind
replacement Hg analyzer is brought into service, a three-point
linearity check with elemental Hg standards and a single-point system
integrity check will be required. Alternatively, a three-level system
integrity check may be performed instead of these two tests. When a
certified non-redundant backup sorbent trap monitoring system is
brought into service, only the routine sampling and QA procedures of
Sec. 75.15 and appendix K of part 75 will be required.
Each non-redundant backup Hg monitoring system and each like-kind
replacement Hg analyzer will be subject to the applicable ongoing QA
requirements, restrictions and conditions specified in Sec.
75.20(d)(2). For certified non-redundant backup Hg CEMS and like-kind
replacement Hg analyzers, the weekly system integrity checks described
in section 2.6 of appendix B of 40 CFR part 75 will also be required as
long as the system or analyzer remains in service, unless the daily
calibration error tests of the analyzer are done using NIST-traceable
oxidized Hg standards.
Third, a new paragraph (k) is being added to Sec. 75.15 that: (1)
Clarifies that, when the RATA of an appendix K sorbent trap monitoring
system is performed, the type of sorbent material used in the appendix
K sorbent traps must be the same as that used for daily operation of
the appendix K monitoring system, and (2) allows the appendix K traps
used during RATA testing to be smaller than the traps used for daily
operation of the appendix K monitoring system. This change will be
particularly advantageous at very low Hg concentrations as it will
facilitate shorter RATA test run times. Parallel changes are being made
to section 6.5.7 of appendix A of part 75 to be consistent with the
provisions of Sec. 75.15(k). Section 6.5.7 currently requires the
appendix K sorbent traps used for the RATA to be the same size as the
traps used for daily operation of the appendix K monitoring system.
Fourth, today's action revises a number of sections of part 75,
appendix K, pertaining to the use of sorbent trap monitoring systems.
EPA is withdrawing the requirement to use the percentage recovery of
the elemental Hg spike in section 3 of each sorbent trap to adjust or
``normalize'' the Hg mass collected in sections 1 and 2 of the trap.
The requirement to spike the third section of each trap is being
retained and data from each pair of traps must still be invalidated if
either or both spike recovery percentages fall outside the acceptable
limits;\1\ however, the results of the spike recoveries will no longer
be used to adjust the Hg mass collected in the first two sections of
the traps. EPA is making this rule change based on an analysis of
recent spike recovery data from long-term appendix K field
demonstrations. Although the vast majority of the spike recoveries in
these studies have been within the currently acceptable limits of 75 to
125 percent, the requirement to normalize based on spike recovery could
affect data precision. For a given pair of traps, if one spike recovery
was high (e.g., 110 percent) and the other one low (e.g., 90 percent),
normalization of the Hg mass collected in the first two trap sections
using third section spike recoveries could make it difficult for a pair
of sorbent traps to meet the relative deviation (RD) specifications in
appendix K. In the example cited, normalization of the data would cause
the Hg concentrations measured by the traps to be adjusted by 10
percent in opposite directions, i.e., one upward and one downward.
Thus, two Hg concentrations that may have been in close agreement
without normalization now might not be able to meet the RD
specifications. In view of this, EPA has concluded that evaluating the
spike recovery data on a pass/fail basis instead of using the percent
recovery values to adjust the emissions data is more technically sound
and is also consistent with the way in which the results of daily and
quarterly QA assessments of CEMS are interpreted.
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\1\ On August 22, 2006, EPA proposed to amend Appendix K to
allow the data from a pair of sorbent traps to be validated in cases
where the third section spike recovery from only one of the traps
meets the percent recovery specifications (see 71 FR 49275). EPA
proposed to allow the results from the trap that meets the
specifications to be used for reporting, provided that a single trap
adjustment factor (STAF) of 1.222 is applied. EPA is evaluating the
comments received on this proposal and expects to publish the final
rule in the summer of 2007.
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Regarding the range of acceptable third section spike recoveries,
EPA is not changing the 75 to 125 percent acceptance criteria. As
previously noted, early field experience with appendix K monitoring
systems has demonstrated that spike recoveries within this range are
achievable. However, recent appendix K data indicate that more
stringent acceptance criteria may be justifiable. It appears that there
has been a marked improvement in third section spike recovery
percentages. Recoveries in the range from 85 to 115 percent are
consistently being achieved. If this trend continues, EPA may propose
to tighten the spike recovery acceptance criteria in a future
rulemaking. Toward that end, EPA will continue to collect and evaluate
third section spike recovery data from appendix K monitoring systems in
the months ahead.
To effect these changes to appendix K, section 11.5 is being
removed and reserved; section 10.4 is being revised; Equations K-6 and
K-7 are being redesignated as Equations K-5 and K-6, respectively; and
the definition of ``M*'' in redesignated Equation K-5 is being revised.
EPA is also revising appendix K to allow the owner or operator to
use other types of gas flow meters besides the conventional dry gas
meter (DGM) to quantify sample gas volume. Since the publication of
appendix K (see 70 FR 28695, May 18, 2005), numerous requests have been
received from the regulated community to allow this flexibility. In
response to these requests, EPA initiated an investigation of the
feasibility of replacing the DGM in a sorbent trap monitoring system
with a thermal mass flow meter. As a result of its investigation, EPA
has concluded that a properly calibrated thermal mass flow meter can be
at least as accurate as a DGM. The mass flow meter is also a more
modern technology than the DGM; since it has no moving parts, it may be
more reliable than a DGM for continuous duty.
Having found one type of gas flow meter that can measure as
accurately as a DGM, EPA is persuaded that there may be other
commercially available gas flow meter technologies that are equally
capable and may be suitable for appendix K applications. Accordingly,
EPA has decided that a performance-based approach, rather than a
prescriptive one, is more appropriate for appendix K gas flow meters.
Today's action allows the use of any type of gas flow meter that is
capable of accurately measuring gas volumes to within 2 percent.
Section 9.2.2.1 of appendix K now requires the manufacturer of the
gas flow meter to perform all necessary set-
[[Page 51499]]
up, testing, programming, etc. of the meter and to provide any
necessary instructions so that for the particular field application,
the meter will give an accurate readout of dry gas volume in units of
standard cubic meters. Then, prior to its initial use, the flow meter
must be calibrated at a minimum of three settings covering the expected
range of sample flow rates for the appendix K system. The initial
calibration may be performed either by the manufacturer or by the end
user. The calibration of the gas flow meter must be checked quarterly
thereafter, at an intermediate flow rate. For mass flow meters, the
initial three-point calibration must be performed by using either a
compressed gas mixture containing CO2, O2, and
N2 in proportions representative of the stack gas
composition or by using the actual stack gas. However, when the initial
calibration is done with a compressed gas mixture, the mass flow meter
may not be used until an additional on-site calibration check of the
flow meter at an intermediate flow rate is performed and passed, using
the actual stack gas.
To calibrate the gas flow meter, the owner or operator may either
follow the basic procedures in section 10.3 or section 16 of Method 5
in appendix A-3 of part 60 for calibration of dry gas meters, or
alternatively, may temporarily install a reference gas flow meter
(RGFM) at the discharge of the appendix K monitoring system while the
monitoring system is in operation and make concurrent measurements of
dry stack gas volume with the RGFM and the appendix K gas flow meter.
If the latter option is chosen, the RGFM may either be a gas flow
metering device that has been calibrated according to section 10.3.1 or
section 16 of Method 5 or a NIST-traceable volumetric calibration
device with an accuracy of 1 percent. Note that this
alternative calibration technique allows required QA checks to be
performed with little or no disruption of the operation of the sorbent
trap monitoring system.
Regardless of which calibration approach is used, a calibration
factor, Yi, must be obtained at each tested flow rate, where
Yi is the ratio of the volume measured by the reference
meter to the volume measured by the flow meter being calibrated. For
the initial three-point calibration, the three Yi values
must be averaged, and each individual Yi must be within
0.02 of the average value. The average value, Y, must then
be used to correct the gas volumes measured by the gas flow meter. For
single-level calibration checks (e.g., the quarterly checks performed
for routine QA), the Yi value obtained at the tested flow
rate must be compared with the current value of Y. If Yi
differs from Y by more than 5 percent, a full three-point recalibration
is then required to determine a new Y value.
In this direct final action, the majority of the revised rule
provisions pertaining to gas flow meters can be found in sections 5.1.5
and 9.2 of appendix K. Minor revisions to sections 7.2.3 and 7.2.5,
Figure K-1, and Table K-1 are being made to be consistent with the
changes to sections 5.1.5 and 9.2. In several other places throughout
part 75 and in the definition of ``Sorbent trap monitoring system'' in
part 72, the term ``dry gas meter,'' when used in reference to a
sorbent trap monitoring system, is being replaced with the more general
term ``gas flow meter.'' Revisions to section 1.5.2 of appendix B of
part 75 will require the gas flow meter calibration procedures and
protocols for periodic recalibration of reference gas flow meters to be
included in the QA plan for the affected unit.
This direct final action, which approves the use of two optional
methods (Methods 30A and 30B) for determining total vapor phase Hg
emissions from stationary sources, is being taken in response to
numerous public comments concerning the desirability of allowing the
use of these types of methods to comply with the Hg emission monitoring
requirements of the CAMR for electric utility steam generating units.
In the May 18, 2005 final rule (70 FR 28636), we summarized the public
comments that we received regarding the use of an instrumental method
as an alternative to the Ontario Hydro Method specified in the proposed
CAMR. As noted earlier in this preamble, the commenters primarily
objected to the required use of the Ontario Hydro Method as the
reference method for the RATAs of Hg monitoring systems and expressed
concern about the complexities in the method and the amount of time
that is required to perform the testing and to receive the results.
Commenters pointed out that it could take days to complete the testing
and weeks to receive the results from a laboratory. Commenters claimed
that for the cap and trade program proposed under CAMR, these delays
could lead to significant implementation problems with respect to the
timely reporting of emissions data. Further, if a RATA should be failed
or invalidated (e.g., if fewer than nine test runs meet the relative
deviation criterion for the paired Ontario Hydro trains), data from the
Hg monitoring system would be invalidated from the hour of the failed
or invalidated test until the hour of completion of a successful RATA.
Conservatively high substitute data values would have to be reported
during that entire time period. In our response to those comments in
the final CAMR rule, we stated that the alternative use of an
instrumental method for the required RATAs of Hg monitoring systems and
sorbent trap monitoring systems is allowed by the final rule but is
subject to approval by the Administrator. We also stated our commitment
to propose and promulgate a Hg instrumental reference method once
sufficient supporting field test data become available. We further
stated that ``A Hg instrumental reference method for RATA testing is
vastly preferable to the Ontario Hydro Method and will greatly
facilitate the implementation of a Hg cap-and-trade program.''
Since promulgation of CAMR, we have continued to communicate with
stakeholders interested in the Hg monitoring requirements of the rule,
and we have come to more clearly understand that it is of great
interest to the affected entities to have additional reference method
options available for relative accuracy testing of installed Hg
monitoring systems as soon as possible. Accordingly, at the end of
2005, we began developing an instrumental test method for Hg and
solicited feedback from the stakeholders on a working draft of the
method (referred to as PRE-009 at https://www.epa.gov/ttn/emc/
prelim.html). More recently, we have been developing a viable sorbent
trap reference method. These efforts have resulted in Methods 30A and
30B.
The general beneficial impacts of this direct final rule to approve
the two optional Hg test methods and amend targeted portions of 40 CFR
parts 72 and 75 include: Allowing affected sources to choose the use of
an alternative to the Ontario Hydro Method without the administrative
burden of applying for Administrator approval on a case-by-case basis;
providing the availability of real-time RATA results (Method 30A);
reducing the overall RATA testing times; reducing costs relative to the
Ontario Hydro Method; and providing additional flexibility in appendix
K sorbent trap monitoring and backup monitoring approaches. The two
optional methods being approved by this direct final rule are
considered to be comparable to the Ontario Hydro Method in terms of the
quality of the results produced. Over the last year, EPA has
collaborated with EPRI and some of its members in a number of field
test programs that have confirmed that the instrumental reference
method approved/established in this notice will provide data comparable
to or better
[[Page 51500]]
than that of the ``Ontario Hydro Method.''
Assuming we do not receive adverse comment on this direct final
rulemaking and Methods 30A and 30B become final, we plan to post
information relevant to Method 30A and 30B applications and equipment
advances on EPA's Web site at https://www.epa.gov/airmarkets.
VII. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory Planning and Review
This action is not a ``significant regulatory action'' under the
terms of Executive Order (EO) 12866 (58 FR 51735, October 4, 1993) and
is therefore not subject to review under the EO.
B. Paperwork Reduction Act
This action does not impose an information collection burden under
the provisions of the Paperwork Reduction Act, 44 U.S.C. 3501 et seq.
Burden means the total time, effort, or financial resources expended by
persons to generate, maintain, retain, or disclose or provide
information to or for a Federal agency. This includes the time needed
to review instructions; develop, acquire, install, and utilize
technology and systems for the purposes of collecting, validating, and
verifying information, processing and maintaining information, and
disclosing and providing information; adjust the existing ways to
comply with any previously applicable instructions and requirements;
train personnel to be able to respond to a collection of information;
search data sources; complete and review the collection of information;
and transmit or otherwise disclose the information.
An agency may not conduct or sponsor, and a person is not required
to respond to a collection of information, unless it displays a
currently valid OMB control number. The OMB control numbers for EPA's
regulations in 40 CFR are listed in 40 CFR part 9.
C. Regulatory Flexibility Act
The Regulatory Flexibility Act (RFA) generally requires an agency
to prepare a regulatory flexibility analysis of any rule subject to
notice and comment rulemaking requirements under the Administrative
Procedure Act or any other statute unless the agency certifies that the
rule will not have a significant economic impact on a substantial
number of small entities. Small entities include small businesses,
small organizations, and small governmental jurisdictions.
For purposes of assessing the impacts of today's rule on small
entities, small entity is defined as: (1) A small business whose parent
company has fewer than 100 or 1,000 employees, or fewer than 4 billion
kilowatt-hr per year of electricity usage, depending on the size
definition for the affected North American Industry Classification
System code; (2) a small governmental jurisdiction that is a government
of a city, county, town, school district or special district with a
population of less than 50,000; and (3) a small organization that is
any not-for-profit enterprise which is independently owned and operated
and is not dominant in its field.
After considering the economic impacts of today's direct final rule
on small entities, I certify that this action will not have a
significant economic impact on a substantial number of small entities.
This direct final rule will not impose any requirements on small
entities because it does not impose any additional regulatory
requirements, but rather provides clarification and additional
regulatory flexibilty.
D. Unfunded Mandates Reform Act
Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Pub.
L. 104-4, establishes requirements for Federal agencies to assess the
effects of their regulatory actions on State, local, and tribal
governments and the private sector. Under section 202 of the UMRA, EPA
generally must prepare a written statement, including a cost-benefit
analysis, for proposed and final rules with ``Federal mandates'' that
may result in expenditures to State, local, and tribal governments, in
the aggregate, or to the private sector, of $100 million or more in any
one year. Before promulgating an EPA rule for which a written statement
is needed, section 205 of the UMRA generally requires EPA to identify
and consider a reasonable number of regulatory alternatives and adopt
the least costly, most cost-effective or least burdensome alternative
that achieves the objectives of the rule. The provisions of section 205
do not apply when they are inconsistent with applicable law. Moreover,
section 205 allows EPA to adopt an alternative other than the least
costly, most cost-effective, or least burdensome alternative if the
Administrator publishes with the final rule an explanation why that
alternative was not adopted. Before EPA establishes any regulatory
requirements that may significantly or uniquely affect small
governments, including tribal governments, it must have developed under
section 203 of the UMRA a small government agency plan. The plan must
provide for notifying potentially affected small governments, enabling
officials of affected small governments to have meaningful and timely
input in the development of EPA regulatory proposals with significant
Federal intergovernmental mandates, and informing, educating, and
advising small governments on compliance with the regulatory
requirements.
EPA has determined that this direct final rule does not contain a
Federal mandate that may result in expenditures of $100 million or more
for State, local, and tribal governments in the aggregate, or to the
private sector in any 1 year, nor does this rule significantly or
uniquely impact small governments, because it contains no requirements
that impose new obligations upon them. Thus, this direct final rule is
not subject to the requirements of sections 202 and 205 of the UMRA.
E. Executive Order 13132: Federalism
Executive Order 13132, entitled ``Federalism'' (64 FR 43255, August
10, 1999), requires EPA to develop an accountable process to ensure
``meaningful and timely input by State and local officials in the
development of regulatory policies that have federalism implications.''
``Policies that have federalism implications'' is defined in the
Executive Order to include regulations that have ``substantial direct
effects on the States, on the relationship between the national
government and the States, or on the distribution of power and
responsibilities among the various levels of government.''
This direct final rule does not have federalism implications. It
will not have substantial direct effects on the States, on the
relationship between the national government and the States, or on the
distribution of power and responsibilities among the various levels of
government, as specified in Executive Order 13132. The use of these
methods is optional on the part of the regulated entities listed. Thus,
Executive Order 13132 does not apply to this direct final rule.
F. Executive Order 13175: Consultation and Coordination With Indian
Tribal Governments
Executive Order 13175, entitled ``Consultation and Coordination
with Indian Tribal Governments'' (65 FR 67249, November 9, 2000),
requires EPA to develop an accountable process to ensure ``meaningful
and timely input by tribal officials in the development of regulatory
policies that have tribal implications.'' This direct final rule does
not have tribal implications, as specified in Executive Order 13175. It
will not have substantial direct effects on tribal governments, on the
[[Page 51501]]
relationship between the Federal government and Indian tribes, or on
the distribution of power and responsibilities between the Federal
government and Indian tribes. Thus, Executive Order 13175 does not
apply to this final rule.
G. Executive Order 13045: Protection of Children From Environmental
Health and Safety Risks
Executive Order 13045: ``Protection of Children from Environmental
Health Risks and Safety Risks'' (62 FR 19885, April 23, 1997) applies
to any rule that: (1) Is determined to be ``economically significant''
as defined under Executive Order 12866, and (2) concerns an
environmental health or safety risk that EPA has reason to believe may
have a disproportionate effect on children. If the regulatory action
meets both criteria, the Agency must evaluate the environmental health
or safety effects of the planned rule on children, and explain why the
planned regulation is preferable to other potentially effective and
reasonably feasible alternatives considered by the Agency. EPA
interprets Executive Order 13045 as applying only to those regulatory
actions that are based on health or safety risks, such that the
analysis required under section 5-501 of the Order has the potential to
influence the regulation. This rule is not subject to Executive Order
13045 because it does not establish an environmental standard intended
to mitigate health or safety risks.
H. Executive Order 13211: Actions That Significantly Affect Energy
Supply, Distribution, or Use
This rule is not subject to Executive Order 13211, ``Actions
Concerning Regulations That Significantly Affect Energy Supply,
Distribution, or Use'' (66 FR 28355, May 22, 2001) because it is not a
significant regulatory action under Executive Order 12866.
I. National Technology Transfer Advancement Act
Section 12(d) of the National Technology Transfer and Advancement
Act of 1995 (NTTAA), Public Law No. 104-113, section 12(d) (15 U.S.C.
272 note) directs EPA to use voluntary consensus standards in its
regulatory activities unless to do so would be inconsistent with
applicable law or otherwise impractical. Voluntary consensus standards
are technical standards (e.g., materials specifications, test methods,
sampling procedures, and business practices) that are developed or
adopted by voluntary consensus standards bodies. The NTTAA directs EPA
to provide Congress, through OMB, explanations when the Agency decides
not to use available and applicable voluntary consensus standards. This
rulemaking involves technical standards. Consistent with the NTTAA, EPA
in a previous related rulemaking (70 FR 28606, May 18, 2005) identified
an acceptable VCS for measuring Hg emissions. The standard ASTM D6784-
02, Standard Test Method for Elemental, Oxidized, Particle-Bound and
Total Mercury Gas Generated from Coal-Fired Stationary sources (Ontario
Hydro Method) was cited in that final rule for measuring Hg emissions.
After today's action becomes effective, the Ontario Hydro Method will
remain an acceptable method for measuring Hg emissions.
J. Executive Order 12898: Federal Actions To Address Environmental
Justice in Minority Populations and Low-Income Populations
Executive Order 12898 (59 FR 7629 (Feb. 16, 1994)) establishes
federal executive policy on environmental justice. Its main provision
directs federal agencies, to the greatest extent practicable and
permitted by law, to make environmental justice part of their mission
by identifying and addressing, as appropriate, disproportionately high
and adverse human health or environmental effects of their programs,
policies, and activities on minority populations and low-income
populations in the United States.
EPA has determined that this direct final rule will not have
disproportionately high and adverse human health or environmental
effects on minority or low-income populations because it does not
affect the level of protection provided to human health or the
environment. This direct final rule does not affect or relax the
control measures on sources impacted by this rule and therefore will
not cause emissions increases from these sources.
K. Congressional Review Act
The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the
Small Business Regulatory Enforcement Fairness Act of 1996, generally
provides that before a rule may take effect, the Agency promulgating
the rule must submit a rule report, which includes a copy of the rule,
to each House of the Congress and to the Comptroller General of the
United States. EPA will submit a report containing this rule and other
required information to the U.S. Senate, the U.S. House of
Representatives, and the Comptroller General of the United States prior
to publication of the rule in the Federal Register. A major rule cannot
take effect until 60 days after it is published in the Federal
Register. This action is not a ``major rule'' as defined by 5 U.S.C.
804(2). This rule will be effective on November 6, 2007.
List of Subjects
40 CFR Part 60
Environmental protection, Administrative practice and procedures,
Air pollution control, Continuous emission monitors, Electric
utilities, Mercury, Test methods and procedures.
40 CFR Part 72
Environmental protection, Administrative practice and procedures,
Air pollution control, Continuous emission monitors, Electric
utilities, Mercury, Test methods and procedures.
40 CFR Part 75
Environmental protection, Administrative practice and procedures,
Air pollution control, Continuous emission monitors, Electric
utilities, Mercury, Test methods and procedures.
Dated: August 17, 2007.
Stephen L. Johnson,
Administrator.
0
For the reasons set out in the preamble, title 40, chapter I, parts 60,
72, and 75 of the Code of Federal Regulations are amended as follows:
PART 60--STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES
0
1. The authority citation for part 60 continues to read as follows:
Authority: 42 U.S.C. 7401-7601.
Appendix A-8 [Amended]
0
2. Amend Appendix A-8 by revising the heading and adding in numerical
order Methods 30A and 30B to read as follows:
APPENDIX A-8 TO PART 60--TEST METHODS 26 THROUGH 30B
* * * * *
Method 30A--Determination of Total Vapor Phase Mercury Emissions From
Stationary Sources (Instrumental Analyzer Procedure)
1.0 Scope and Application
What Is Method 30A?
Method 30A is a procedure for measuring total vapor phase
mercury (Hg) emissions from stationary sources using an instrumental
analyzer. This method is particularly appropriate for performing
emissions testing and for conducting relative accuracy test audits
(RATAs) of mercury continuous emissions monitoring systems (Hg CEMS)
and sorbent trap monitoring systems at coal-fired combustion
sources. Quality assurance and quality control
[[Page 51502]]
requirements are included to assure that you, the tester, collect
data of known and acceptable quality for each testing site. This
method does not completely describe all equipment, supplies, and
sampling procedures and analytical procedures you will need but
refers to other test methods for some of the details. Therefore, to
obtain reliable results, you should also have a thorough knowledge
of these additional methods which are also found in appendices A-1
and A-3 to this part:
(a) Method 1--Sample and Velocity Traverses for Stationary
Sources.
(b) Method 4--Determination of Moisture Content in Stack Gases.
1.1 Analytes. What does this method determine? This method is
designed to measure the mass concentration of total vapor phase Hg
in flue gas, which represents the sum of elemental Hg (Hg\0\) and
oxidized forms of Hg (Hg+\2\), in mass concentration
units of micrograms per cubic meter ([mu]g/m\3\).
------------------------------------------------------------------------
Analyte CAS No. Sensitivity
------------------------------------------------------------------------
Elemental Hg (Hg\0\).............. 7439-97-6 Typically <2% of
Calibration Span.
Oxidized Hg (Hg+\2\).............. .............. (Same).
------------------------------------------------------------------------
1.2 Applicability. When is this method required? Method 30A is
offered as a reference method for emission testing and for RATAs of
Hg CEMS and sorbent trap monitoring systems at coal-fired boilers.
Method 30A may also be specified for other source categories in the
future, either by New Source Performance Standards (NSPS), National
Emission Standards for Hazardous Air Pollutants (NESHAP), emissions
trading programs, State Implementation Plans (SIP), or operating
permits that require measurement of Hg concentrations in stationary
source emissions to determine compliance with an applicable emission
standard or limit, or to conduct RATAs of Hg CEMS and sorbent trap
monitoring systems.
1.3 Data Quality Objectives (DQO). How good must my collected
data be? Method 30A has been designed to provide data of high and
known quality for Hg emission testing and for relative accuracy
testing of Hg monitoring systems including Hg CEMS and sorbent trap
monitoring systems. In these and other applications, the principle
objective is to ensure the accuracy of the data at the actual
emission levels encountered. To meet this objective, calibration
standards prepared according to an EPA traceability protocol must be
used and measurement system performance tests are required.
2.0 Summary of Method
In this method, a sample of the effluent gas is continuously
extracted and conveyed to an analyzer capable of measuring the total
vapor phase Hg concentration. Elemental and oxidized mercury (i.e.,
Hg\0\ and Hg+\2\) may be measured separately or
simultaneously but, for purposes of this method, total vapor phase
Hg is the sum of Hg\0\ and Hg+\2\. You must meet the
performance requirements of this method (i.e., system calibration,
interference testing, dynamic spiking, and