44488 Federal Register / Vol. 77, No. 146 / Monday, July 30, 2012 / Rules and Regulations 

Act of 1995 (15 U.S.C. 272 note) because 

application of those requirements would 

be inconsistent with the CAA; and 

• Does not provide EPA with the 

discretionary authority to address, as 

appropriate, disproportionate human 

health or environmental effects, using 

practicable and legally permissible 

methods, under Executive Order 12898 

(59 FR 7629, February 16, 1994). 

In addition, this rule does not have 

tribal implications as specified by 

Executive Order 13175 (65 FR 67249, 

November 9, 2000), because the SIP is 

not approved to apply in Indian country 

located in the state, and EPA notes that 

it will not impose substantial direct 

costs on tribal governments or preempt 

tribal law. 

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 action 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). 

Under section 307(b)(1) of the CAA, 

petitions for judicial review of this 

action must be filed in the United States 

Court of Appeals for the appropriate 

circuit by September 28, 2012. Filing a 

petition for reconsideration by the 

Administrator of this final rule does not 

affect the finality of this action for the 

purposes of judicial review nor does it 

extend the time within which a petition 

for judicial review may be filed and 

shall not postpone the effectiveness of 

such rule or action. This action may not 

be challenged later in proceedings to 

enforce its requirements. (See section 

307(b)(2)). 

List of Subjects in 40 CFR Part 52 

Environmental protection, Air 

pollution control, Incorporation by 

reference, Intergovernmental relations, 

Nitrogen dioxide, Ozone, Reporting and 

recordkeeping requirements, Volatile 

organic compounds. 

Dated: July 16, 2012. 

A. Stanley Meiburg, 

Acting Regional Administrator, Region 4. 

Therefore, 40 CFR part 52 is amended 

as follows: 

PART 52—[AMENDED] 

■ 1. The authority citation for part 52 

continues to read as follows: 

Authority: 42 U.S.C. 7401 et seq. 

■ 2. Section 52.520 in paragraph (e) is 

amended by adding three new entries 

for ‘‘110(a)(1) and (2) Infrastructure 

Requirements for the 1997 8-Hour 

Ozone National Ambient Air Quality 

Standards,’’ ‘‘Section 128 

Requirements,’’ and ‘‘Sections 

110(a)(2)(E)(ii) and (G) Infrastructure 

Requirements for the 1997 8-Hour 

Ozone National Ambient Air Quality 

Standards’’ at the end of the table to 

read as follows: 

§ 52.520 Identification of plan. 

* * * * * 

(e) * * * 

EPA-APPROVED FLORIDA NON-REGULATORY PROVISIONS

Provision State effective 

date 

EPA approval 

date Federal Register notice Explanation 

*******

110(a)(1) and (2) Infrastructure Requirements for the 

1997 8-Hour Ozone National Ambient Air Quality 

Standards.

12/13/2007 7/30/2012 [Insert citation of publication].

Section 128 Requirements ......................................... 5/24/2012 7/30/2012 [Insert citation of publication].

Sections 110(a)(2)(E)(ii) and (G) Infrastructure Requirements for the 1997 8-Hour Ozone National 

Ambient Air Quality Standards.

5/24/2012 7/30/2012 [Insert citation of publication].

■ 3. Section 52.523 is added to read as 

follows: 

§ 52.523 Control strategy: Ozone 

(a) Disapproval. EPA is disapproving 

portions of Florida’s infrastructure SIP 

for the 1997 8-hour ozone NAAQS 

regarding the State’s ability to provide 

adequate legal authority for the 

implementation of a Greenhouse Gas 

Prevention of Significant Deterioration 

program, specifically with respect to 

sections 110(a)(2)(C) and 110(a)(2)(J). A 

FIP is currently in place and approved 

for Florida at 40 CFR 52.37 for these 

requirements. 

(b) [Reserved] 

[FR Doc. 2012–18316 Filed 7–27–12; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 60 

[EPA–HQ–OAR–2010–0115; FRL–9701–9] 

RIN 2060–AQ23 

Method 16C for the Determination of 

Total Reduced Sulfur Emissions From 

Stationary Sources 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Final rule. 

SUMMARY: This action promulgates 

Method 16C for measuring total reduced 

sulfur (TRS) emissions from stationary 

sources. Method 16C offers the 

advantages of real-time data collection 

and uses procedures that are already in 

use for measuring other pollutants. 

Method 16C will be a testing option that 

is used at the discretion of the tester. 

DATES: This final rule is effective on July 

30, 2012. 

ADDRESSES: The EPA has established a 

docket for this action under Docket ID 

No. EPA–HQ–OAR–2010–0115. All 

documents in the docket are listed in 

the http://www.regulations.gov index. 

Although listed in the index, some 

information is not publicly available, 

e.g., confidential business information 

(CBI) or other information whose 

disclosure is restricted by statute. 

Certain other material, such as 

copyrighted material, is not placed on 

the Internet and will be publicly 

available only in hard copy form. 

Publicly available docket materials are 


tkelley on DSK3SPTVN1PROD with RULES
Federal Register / Vol. 77, No. 146 / Monday, July 30, 2012 / Rules and Regulations 44489 

available either electronically at 

www.regulations.gov or in hard copy at 

the Air Docket, EPA/DC, EPA West, 

Room 3334, 1301 Constitution Avenue 

NW., Washington, DC. The Docket 

Facility and the Public Reading Room 

are 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 

Docket is (202) 566–1742. 

FOR FURTHER INFORMATION CONTACT: Mr. 

Foston Curtis, Office of Air Quality 

Planning and Standards, Air Quality 

Assessment Division, Measurement 

Technology Group (E143–02), U.S. 

Environmental Protection Agency, 

Research Triangle Park, North Carolina 

27711; telephone number: (919) 541– 

1063; fax number: (919) 541–0516; 

email address: curtis.foston@epa.gov. 

SUPPLEMENTARY INFORMATION: 

Table of Contents 

I. General Information 

A. Does this action apply to me? 

B. Where can I obtain a copy of this action? 

C. Judicial Review 

II. Background 

III. Summary of Method 16C 

IV. Public Comments on Proposed Method 

16C 

V. Statutory and Executive Order Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review and Executive 

Order 13563: Improving Regulation and 

Regulatory 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 

Risks and Safety Risks 

H. Executive Order 13211: Actions 

Concerning Regulations 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 

I. General Information 

A. Does this action apply to me? 

Method 16C applies to TRS 

measurement from kraft pulp mills 

subject to Subpart BB of the New Source 

Performance Standards (NSPS). The 

methods required under Subpart BB for 

TRS are sometimes used under the 

petroleum refineries NSPS (Subpart J). 

Method 16C may also be applicable to 

sources regulated by state and local 

regulations that adopt the Subpart BB 

testing requirements. 

Regulated Entities. Categories and 

entities potentially affected include the 

following: 

Category NAICSa Examples of regulated 

entities 

Industry .... 322110 Kraft Pulp Mills. 

Industry .... 324110 Petroleum Refineries. 

a North American Industry Classification 

System. 

This table is not intended to be 

exhaustive, but rather to provide a guide 

for readers regarding entities likely to be 

affected by this action. This table lists 

examples of the types of entities the 

EPA is now aware could potentially be 

affected by this final action. Other types 

of entities not listed could also be 

affected. If you have any questions 

regarding the applicability of this action 

to a particular entity, consult the person 

listed in the preceding FOR FURTHER

INFORMATION CONTACT section. 

B. Where can I obtain a copy of this 

action? 

In addition to being available in the 

docket, an electronic copy of this rule 

will also be available on the Worldwide 

Web (www) through the Technology 

Transfer Network (TTN). Following the 

Administrator’s signature, a copy of the 

final rule will be placed on the TTN’s 

policy and guidance page for newly 

proposed or promulgated rules at 

http://www.epa.gov/ttn/oarpg. The TTN 

provides information and technology 

exchange in various areas of air 

pollution control. 

C. Judicial Review 

Under section 307(b)(1) of the Clean 

Air Act (CAA), judicial review of this 

final rule is available by filing a petition 

for review in the U.S. Court of Appeals 

for the District of Columbia Circuit by 

September 28, 2012. Under section 

307(d)(7)(B) of the CAA, only an 

objection to this final rule that was 

raised with reasonable specificity 

during the period for public comment 

can be raised during judicial review. 

Moreover, under section 307(b)(2) of the 

CAA, the requirements established by 

this action may not be challenged 

separately in any civil or criminal 

proceedings brought by EPA to enforce 

these requirements. 

II. Background 

Method 16C was proposed in the 

Federal Register on September 2, 2010, 

with a public comment period that 

ended November 1, 2010. Two comment 

letters were received from the public. 

III. Summary of Method 16C 

Method 16C uses the sampling 

procedures of Method 16A and the 

analytical procedures of Method 6C to 

measure TRS. Total reduced sulfur is 

defined as hydrogen sulfide, methyl 

mercaptan, dimethyl sulfide, and 

dimethyl disulfide. As in Method 16A, 

the sample is collected from the source 

through a heated probe and immediately 

conditioned in a citrate buffer scrubber. 

The conditioned sample is oxidized in 

a tube furnace to convert TRS to sulfur 

dioxide (SO2). The oxidized sample is 

then analyzed for SO2 using a real-time 

SO2 analyzer as in Method 6C. 

This method may be used as an 

alternative to Methods 16, 16A, and 16B 

for determining TRS. Its use has been 

allowed on a case-by-case basis and, 

based on our experience, it is a good 

alternative. Method 16C offers 

advantages over currently required 

methods by supplying real-time data in 

the field using analyzers and procedures 

that are currently used for other 

pollutants. Performance checks 

contained in the method ensure that 

bias and calibration precision are 

periodically checked and maintained. 

This rule will not require the use of 

Method 16C but will allow it as an 

alternative method at the discretion of 

the user. This method does not impact 

testing stringency; data are collected 

under the same conditions and time 

intervals as the current methods. 

IV. Public Comments on Proposed 

Method 16C 

Two public comment letters were 

received on the proposed rule. The 

comments pointed out contradictions in 

different sections of the method for the 

analyzer calibration error test and the 

system bias check. In one instance, the 

analyzer calibration acceptance criterion 

was listed as 5 percent and in another 

place it was listed as 2 percent. The rule 

was corrected to state that 5 percent is 

the correct criterion for this test. For the 

system bias check, unclear language was 

amended to specifically state that the 

pre-test bias check is mandatory, not 

optional. An additional comment led to 

the dropping of the sample correction 

for moisture since it is not needed for 

most analyzers. The public comments 

are addressed in the Summary of 

Comments and Responses Document 

that has been added to the docket. 


tkelley on DSK3SPTVN1PROD with RULES
44490 Federal Register / Vol. 77, No. 146 / Monday, July 30, 2012 / Rules and Regulations 

V. Statutory and Executive Order 

Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review and Executive 

Order 13563: Improving Regulation and 

Regulatory Review 

This action is not a ‘‘significant 

regulatory action’’ under the terms of 

Executive Order 12866 (58 FR 51735, 

October 4, 1993) and is, therefore, not 

subject to review under Executive 

Orders 12866 and 13563 (76 FR 3821, 

January 21, 2011). 

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 is 

defined at 5 CFR 1320.3(b). This final 

rule does not add information collection 

requirements beyond those currently 

required under the applicable 

regulations. This final rule adds an 

alternative test method that may be used 

at the discretion of the source. 

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 this rule on small entities, small 

entity is defined as: (1) A small business 

as defined by the Small Business 

Administration’s (SBA) regulations at 13 

CFR 121.201; (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 this 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 final rule will not impose any 

requirements on small entities because 

Method 16C is not a required test 

method but may be used at the 

discretion of the source. Any small 

entity choosing to use Method 16C 

would likely do so because it is less 

burdensome or more advantageous than 

the other methods allowed. 

D. Unfunded Mandates Reform Act 

This action contains no federal 

mandates under the provisions of Title 

II of the Unfunded Mandates Reform 

Act of 1995 (UMRA), 2 U.S.C. 1531– 

1538 for State, local, or tribal 

governments or the private sector. This 

action imposes no enforceable duty on 

any State, local or tribal governments or 

the private sector. Therefore, this action 

is not subject to the requirements of 

sections 202 or 205 of the UMRA. This 

action is also not subject to the 

requirements of section 203 of UMRA 

because it contains no regulatory 

requirements that might significantly or 

uniquely affect small governments. Any 

small entity choosing to use Method 

16C would likely do so because it is less 

burdensome or more advantageous than 

the other methods allowed. 

E. Executive Order 13132: Federalism 

This action 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. This final rule 

adds Method 16C for use as a new 

alternative method. Thus, Executive 

Order 13132 does not apply to this 

action. 

F. Executive Order 13175: Consultation 

and Coordination With Indian Tribal 

Governments 

This action does not have tribal 

implications, as specified in Executive 

Order 13175 (65 FR 67249, November 9, 

2000). This final rule provides an 

additional testing option for measuring 

pollutants to what is currently 

mandated. It does not add any new 

requirements and does not affect 

pollutant emissions or air quality. Thus, 

Executive Order 13175 does not apply 

to this action. 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

Risks and Safety Risks 

The EPA interprets EO 13045 (62 FR 

19885, April 23, 1997) as applying only 

to those regulatory actions that concern 

health or safety risks, such that the 

analysis required under section 5–501 of 

the EO has the potential to influence the 

regulation. This action is not subject to 

EO 13045 because it does not establish 

an environmental standard intended to 

mitigate health or safety risks. 

H. Executive Order 13211: Actions 

Concerning Regulations That 

Significantly Affect Energy Supply, 

Distribution, or Use 

This rule is not subject to Executive 

Order 13211 (66 FR 28355 (May 22, 

2001)), because it is not a significant 

regulatory action under Executive Order 

12866. 

I. National Technology Transfer and 

Advancement Act 

Section 12(d) of the National 

Technology Transfer and Advancement 

Act of 1995 (‘‘NTTAA’’), Public Law 

104–113, 12(d)(15 U.S.C. 272 note) 

directs the 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 

the EPA to provide Congress, through 

OMB, explanations when the Agency 

decides not to use available and 

applicable voluntary consensus 

standards. 

This action does not involve technical 

standards. Therefore, the EPA did not 

consider the use of any voluntary 

consensus standards. 

J. Executive Order 12898: Federal 

Actions To Address Environmental 

Justice in Minority Populations and 

Low-Income Populations 

Executive Order (EO) 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. 

The EPA has determined that this 

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 final rule does 

not relax the control measures on 

sources regulated by the rule and, 

therefore, will not cause emissions 

increases from these sources. 


tkelley on DSK3SPTVN1PROD with RULES
Federal Register / Vol. 77, No. 146 / Monday, July 30, 2012 / Rules and Regulations 44491 

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. The 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 

July 30, 2012. 

List of Subjects in 40 CFR Part 60 

Administrative practice and 

procedures, Air pollution control, 

Intergovernmental relations, Reporting 

and recordkeeping requirements. 

Dated: July 23, 2012. 

Lisa P. Jackson, 

Administrator. 

For the reasons set out in the 

preamble, Title 40, Chapter I of the Code 

of Federal Regulations is amended as 

follows: 

PART 60—STANDARDS OF 

PERFORMANCE FOR NEW 

STATIONARY SOURCES 

■ 1. The authority citation for part 60 

continues to read as follows: 

Authority: 42 U.S.C. 7401–7601. 

■ 2. Amend Appendix A–6 to Part 60 by 

adding ‘‘Method 16C’’ in alphanumeric 

order to read as follows: 

Appendix A–6 to Part 60—Test 

Methods 16 Through 18 

* * * * * 

Method 16C—Determination of Total 

Reduced Sulfur Emissions From Stationary 

Sources 

1.0 Scope and Application 

What is Method 16C? 

Method 16C is a procedure for measuring 

total reduced sulfur (TRS) in stationary 

source emissions using a continuous 

instrumental analyzer. Quality assurance and 

quality control requirements are included to 

assure that you, the tester, collect data of 

known quality. You must document your 

adherence to these specific requirements for 

equipment, supplies, sample collection and 

analysis, calculations, and data analysis. This 

method does not completely describe all 

equipment, supplies, and sampling and 

analytical procedures you will need but 

refers to other methods for some of the 

details. Therefore, to obtain reliable results, 

you should also have a thorough knowledge 

of these additional test methods which are 

found in appendix A to this part: 

(a) Method 6C—Determination of Sulfur 

Dioxide Emissions from Stationary Sources 

(Instrumental Analyzer Procedure) 

(b) Method 7E—Determination of Nitrogen 

Oxides Emissions from Stationary Sources 

(Instrumental Analyzer Procedure) 

(c) Method 16A—Determination of Total 

Reduced Sulfur Emissions from Stationary 

Sources (Impinger Technique) 

1.1 Analytes. What does Method 16C 

determine? 

Analyte CAS No. 

Total reduced sulfur including: N/A 

Dimethyl disulfide (DMDS), 

[(CH3)2S2] ............................ 62–49–20 

Dimethyl sulfide (DMS), 

[(CH3)2S] .............................. 75–18–3 

Hydrogen sulfide (H2S) ........... 7783–06–4 

Methyl mercaptan (MeSH), 

(CH4S) ................................. 74–93–1 

Reported as: Sulfur dioxide 

(SO2) ....................................... 7449–09–5 

1.2 Applicability. This method is 

applicable for determining TRS emissions 

from recovery furnaces (boilers), lime kilns, 

and smelt dissolving tanks at kraft pulp 

mills, and from other sources when specified 

in an applicable subpart of the regulations. 

1.3 Data Quality Objectives. Adherence to 

the requirements described in Method 16C 

will enhance the quality of the data obtained. 

2.0 Summary of Method 

2.1 An integrated gas sample is extracted 

from the stack. The SO2 is removed 

selectively from the sample using a citrate 

buffer solution. The TRS compounds are then 

thermally oxidized to SO2 and determined as 

SO2 by an instrumental analyzer. This 

method is a combination of the sampling 

procedures of Method 16A and the analytical 

procedures of Method 6C (referenced in 

Method 7E), with minor modifications to 

facilitate their use together. 

3.0 Definitions 

Analyzer calibration error, Calibration 

curve, Calibration gas, Low-level gas, Midlevel gas, High-level gas, Calibration drift, 

Calibration span, Data recorder, Direct 

calibration mode, Gas analyzer, Interference 

check, Measurement system, Response time, 

Run, System calibration mode, System 

performance check, and Test are the same as 

used in Methods 16A and 6C. 

4.0 Interferences 

4.1 Reduced sulfur compounds other 

than those defined as TRS, if present, may be 

measured by this method. Compounds like 

carbonyl sulfide, which is partially oxidized 

to SO2 and may be present in a lime kiln exit 

stack, would be a positive interferent. 

Interferences may vary among instruments, 

and instrument-specific interferences must 

be evaluated through the interference check. 

4.2 Particulate matter from the lime kiln 

stack gas (primarily calcium carbonate) can 

cause a negative bias if it is allowed to enter 

the citrate scrubber; the particulate matter 

will cause the pH to rise and H2S to be 

absorbed before oxidation. Proper use of the 

particulate filter, described in Section 6.1.3 

of Method 16A, will eliminate this 

interference. 

5.0 Safety 

5.1 Disclaimer. This method may involve 

hazardous materials, operations, and 

equipment. This test method may not address 

all of the safety problems associated with its 

use. It is the responsibility of the user to 

establish appropriate safety and health 

practices before performing this test method. 

5.2 Hydrogen Sulfide. Hydrogen sulfide 

is a flammable, poisonous gas with the odor 

of rotten eggs. Hydrogen sulfide is extremely 

hazardous and can cause collapse, coma, and 

death within a few seconds of one or two 

inhalations at sufficient concentrations. Low 

concentrations irritate the mucous 

membranes and may cause nausea, dizziness, 

and headache after exposure. It is the 

responsibility of the user of this test method 

to establish appropriate safety and health 

practices. 

6.0 Equipment and Supplies 

What do I need for the measurement system? 

The measurement system is similar to 

those applicable components in Methods 

16A and 6C. Modifications to the apparatus 

are accepted provided the performance 

criteria in Section 13.0 are met. 

6.1 Probe. Teflon tubing, 6.4-mm 

(1⁄4 in.) diameter, sequentially wrapped with 

heat-resistant fiber strips, a rubberized heat 

tape (plug at one end), and heat-resistant 

adhesive tape. A flexible thermocouple or 

other suitable temperature measuring device 

must be placed between the Teflon tubing 

and the fiber strips so that the temperature 

can be monitored to prevent softening of the 

probe. The probe must be sheathed in 

stainless steel to provide in-stack rigidity. A 

series of bored-out stainless steel fittings 

placed at the front of the sheath will prevent 

moisture and particulate from entering 

between the probe and sheath. A 6.4-mm (1⁄4

in.) Teflon elbow (bored out) must be 

attached to the inlet of the probe, and a 2.54 

cm (1 in.) piece of Teflon tubing must be 

attached at the open end of the elbow to 

permit the opening of the probe to be turned 

away from the particulate stream; this will 

reduce the amount of particulate drawn into 

the sampling train. The probe is depicted in 

Figure 16A–2 of Method 16A. 

6.2 Probe Brush. Nylon bristle brush with 

handle inserted into a 3.2-mm (1⁄8 in.) Teflon 

tubing. The Teflon tubing should be long 

enough to pass the brush through the length 

of the probe. 

6.3 Particulate Filter. 50-mm Teflon filter 

holder and a 1- to 2-mm porosity, Teflon filter 

(may be available through Savillex 

Corporation, 5325 Highway 101, Minnetonka, 

Minnesota 55343, or other suppliers of 

filters). The filter holder must be maintained 

in a hot box at a temperature sufficient to 

prevent moisture condensation. A 

temperature of 121 °C (250 °F) was found to 


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44492 Federal Register / Vol. 77, No. 146 / Monday, July 30, 2012 / Rules and Regulations 

be sufficient when testing a lime kiln under 

sub-freezing ambient conditions. 

6.4 SO2 Scrubber. Three 300-ml Teflon 

segmented impingers connected in series 

with flexible, thick-walled, Teflon tubing. 

(Impinger parts and tubing may be available 

through Savillex or other suppliers.) The first 

two impingers contain 100 ml of citrate 

buffer, and the third impinger is initially dry. 

The tip of the tube inserted into the solution 

should be constricted to less than 3 mm (1⁄8

in.) ID and should be immersed to a depth 

of at least 5 cm (2 in.). 

6.5 Combustion Tube. Quartz glass tubing 

with an expanded combustion chamber 2.54 

cm (1 in.) in diameter and at least 30.5 cm 

(12 in.) long. The tube ends should have an 

outside diameter of 0.6 cm (1⁄4 in.) and be at 

least 15.3 cm (6 in.) long. This length is 

necessary to maintain the quartz-glass 

connector near ambient temperature and 

thereby avoid leaks. Alternative combustion 

tubes are acceptable provided they are shown 

to combust TRS at concentrations 

encountered during tests. 

6.6 Furnace. A furnace of sufficient size 

to enclose the combustion chamber of the 

combustion tube with a temperature 

regulator capable of maintaining the 

temperature at 800 ± 100 °C (1472 ± 180 °F). 

The furnace operating temperature should be 

checked with a thermocouple to ensure 

accuracy. 

6.7 Sampling Pump. A leak-free pump is 

required to pull the sample gas through the 

system at a flow rate sufficient to minimize 

the response time of the measurement system 

and must be constructed of material that is 

non-reactive to the gas it contacts. For 

dilution-type measurement systems, an 

eductor pump may be used to create a 

vacuum that draws the sample through a 

critical orifice at a constant rate. 

6.8 Calibration Gas Manifold. The 

calibration gas manifold must allow the 

introduction of calibration gases either 

directly to the gas analyzer in direct 

calibration mode or into the measurement 

system, at the probe, in system calibration 

mode, or both, depending upon the type of 

system used. In system calibration mode, the 

system must be able to flood the sampling 

probe and vent excess gas. Alternatively, 

calibration gases may be introduced at the 

calibration valve following the probe. 

Maintain a constant pressure in the gas 

manifold. For in-stack dilution-type systems, 

a gas dilution subsystem is required to 

transport large volumes of purified air to the 

sample probe, and a probe controller is 

needed to maintain the proper dilution ratio. 

6.9 Sample Gas Manifold. The sample gas 

manifold diverts a portion of the sample to 

the analyzer, delivering the remainder to the 

by-pass discharge vent. The manifold should 

also be able to introduce calibration gases 

directly to the analyzer. The manifold must 

be made of material that is non-reactive to 

SO2 and be configured to safely discharge the 

bypass gas. 

6.10 SO2 Analyzer. You must use an 

instrument that uses an ultraviolet, nondispersive infrared, fluorescence, or other 

detection principle to continuously measure 

SO2 in the gas stream provided it meets the 

performance specifications in Section 13.0. 

6.11 Data Recording. A strip chart 

recorder, computerized data acquisition 

system, digital recorder, or data logger for 

recording measurement data must be used. 

7.0 Reagents and Standards 

Note: Unless otherwise indicated, all 

reagents must conform to the specifications 

established by the Committee on Analytical 

Reagents of the American Chemical Society. 

When such specifications are not available, 

the best available grade must be used. 

7.1 Water. Deionized distilled water must 

conform to ASTM Specification D 1193–77 or 

91 Type 3 (incorporated by reference—see 

§ 60.17). The KMnO4 test for oxidizable 

organic matter may be omitted when high 

concentrations of organic matter are not 

expected to be present. 

7.2 Citrate Buffer. Dissolve 300 g of 

potassium citrate (or 284 g of sodium citrate) 

and 41 g of anhydrous citric acid in 1 liter 

of water (200 ml is needed per test). Adjust 

the pH to between 5.4 and 5.6 with 

potassium citrate or citric acid, as required. 

7.3 Calibration Gas. Refer to Section 7.1 

of Method 7E (as applicable) for the 

calibration gas requirements. Example 

calibration gas mixtures are listed below. 

(a) SO2 in nitrogen (N2). 

(b) SO2 in air. 

(c) SO2 and carbon dioxide (CO2) in N2. 

(d) SO2 and oxygen (O2) in N2. 

(e) SO2/CO2/O2 gas mixture in N2. 

(f) CO2/NOX gas mixture in N2.

(g) CO2/SO2/NOX gas mixture in N2.

For fluorescence-based analyzers, the O2 and 

CO2 concentrations of the calibration gases as 

introduced to the analyzer must be within 1.0 

percent (absolute) O2 and 1.0 percent 

(absolute) CO2 of the O2 and CO2

concentrations of the effluent samples as 

introduced to the analyzer. Alternatively, for 

fluorescence-based analyzers, use calibration 

blends of SO2 in air and the nomographs 

provided by the vendor to determine the 

quenching correction factor (the effluent O2

and CO2 concentrations must be known). 

This requirement does not apply to ambientlevel fluorescence analyzers that are used in 

conjunction with sample dilution systems. 

Alternatively, H2S in O2 or air may be used 

to calibrate the analyzer through the tube 

furnace. 

7.4 System Performance Check Gas. You 

must use H2S (100 ppmv or less) stored in 

aluminum cylinders with the concentration 

certified by the manufacturer. Hydrogen 

sulfide in nitrogen is more stable than H2S 

in air, but air may be used as the balance gas. 

Note: Alternatively, H2S recovery gas 

generated from a permeation device 

gravimetrically calibrated and certified at 

some convenient operating temperature may 

be used. The permeation rate of the device 

must be such that at the appropriate dilution 

gas flow rate, an H2S concentration can be 

generated in the range of the stack gas or 

within 20 percent of the emission standard. 

7.5 Interference Check. Examples of test 

gases for the interference check are listed in 

Table 7E–3 of Method 7E. 

8.0 Sample Collection, Preservation, 

Storage, and Transport 

8.1 Pre-sampling Tests. Before measuring 

emissions, perform the following procedures: 

(a) Calibration gas verification, 

(b) Calibration error test, 

(c) System performance check, 

(d) Verification that the interference check 

has been satisfied. 

8.1.1 Calibration Gas Verification. Obtain 

a certificate from the gas manufacturer 

documenting the quality of the gas. Confirm 

that the manufacturer certification is 

complete and current. Ensure that your 

calibration gas certifications have not 

expired. This documentation should be 

available on-site for inspection. To the extent 

practicable, select a high-level gas 

concentration that will result in the 

measured emissions being between 20 and 

100 percent of the calibration span. 

8.1.2 Analyzer Calibration Error Test. 

After you have assembled, prepared, and 

calibrated your sampling system and 

analyzer, you must conduct a 3-point 

analyzer calibration error test before the first 

run and again after any failed system 

performance check or failed drift test to 

ensure the calibration is acceptable. 

Introduce the low-, mid-, and high-level 

calibration gases sequentially to the analyzer 

in direct calibration mode. For each 

calibration gas, calculate the analyzer 

calibration error using Equation 16C–1 in 

Section 12.2. The calibration error for the 

low-, mid-, and high-level gases must not 

exceed 5.0 percent or 0.5 ppmv. If the 

calibration error specification is not met, take 

corrective action and repeat the test until an 

acceptable 3-point calibration is achieved. 

8.1.3 System Performance Check. A 

system performance check is done (1) to 

validate the sampling train components and 

procedure (prior to testing), and (2) to 

validate a test run (after a run). You must 

conduct a performance check in the field 

prior to testing, and after each 3-hour run or 

after three 1-hour runs. A performance check 

consists of sampling and analyzing a known 

concentration of H2S (system performance 

check gas) and comparing the analyzed 

concentration to the known concentration. 

To conduct the system performance check, 

mix the system performance check gas 

(Section 7.4) and ambient air, that has been 

conditioned to remove moisture and sulfurcontaining gases, in a dilution system such 

as that shown in Figure 16A–3 of Method 

16A. Alternatively, ultra-high purity (UHP) 

grade air may be used. Adjust the gas flow 

rates to generate an H2S concentration in the 

range of the stack gas or within 20 percent 

of the applicable standard and an oxygen 

concentration greater than 1 percent at a total 

flow rate of at least 2.5 liters/min (5.3 ft3/hr). 

Use Equation 16A–3 from Method 16A to 

calculate the concentration of system 

performance check gas generated. Calibrate 

the flow rate from both gas sources with a 

soap bubble flow meter so that the diluted 

concentration of H2S can be accurately 

calculated. Alternatively, mass flow 

controllers with documented calibrations 

may be used if UHP grade air is being used. 

Sample duration should be sufficiently long 

to ensure a stable response from the analyzer. 


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Analyze in the same manner as the emission 

samples. Collect the sample through the 

probe of the sampling train using a manifold 

or other suitable device that will ensure 

extraction of a representative sample. The 

TRS sample concentration measured between 

system performance checks is corrected by 

the average of the pre- and post-system 

performance checks. 

8.1.4 Interference Check. Same as in 

Method 7E, Section 8.2.7. 

8.2 Measurement System Preparation. 

8.2.1 For the SO2 scrubber, measure 100 

ml of citrate buffer into the first and second 

impingers; leave the third impinger empty. 

Immerse the impingers in an ice bath, and 

locate them as close as possible to the filter 

heat box. The connecting tubing should be 

free of loops. Maintain the probe and filter 

temperatures sufficiently high to prevent 

moisture condensation, and monitor with a 

suitable temperature sensor. Prepare the 

oxidation furnace and maintain at 800 ± 

100°C (1472 ± 180°F). 

8.2.2 Citrate Scrubber Conditioning 

Procedure. Condition the citrate buffer 

scrubbing solution by pulling stack gas 

through the Teflon impingers as described in 

Section 8.4.1. 

8.3 Pretest Procedures. After the complete 

measurement system has been set up at the 

site and deemed to be operational, the 

following procedures must be completed 

before sampling is initiated. 

8.3.1 Leak-Check. Appropriate leak-check 

procedures must be employed to verify the 

integrity of all components, sample lines, and 

connections. For components upstream of the 

sample pump, attach the probe end of the 

sample line to a manometer or vacuum 

gauge, start the pump and pull a vacuum 

greater than 50 mm (2 in.) Hg, close off the 

pump outlet, and then stop the pump and 

ascertain that there is no leak for 1 minute. 

For components after the pump, apply a 

slight positive pressure and check for leaks 

by applying a liquid (detergent in water, for 

example) at each joint. Bubbling indicates the 

presence of a leak. 

8.3.2 Initial System Performance Check. 

A system performance check using the test 

gas (Section 7.4) is performed prior to testing 

to validate the sampling train components 

and procedure. 

8.4 Sample Collection and Analysis. 

8.4.1 After performing the required 

pretest procedures described in Section 8.1, 

insert the sampling probe into the test port 

ensuring that no dilution air enters the stack 

through the port. Condition the sampling 

system and citrate buffer solution for a 

minimum of 15 minutes before beginning 

analysis. Begin sampling and analysis. A 

source test consists of three test runs. A test 

run shall consist of a single sample collected 

over a 3-hour period or three separate 

1-hour samples collected over a period not to 

exceed six hours. 

8.5 Post-Run Evaluations. 

8.5.1 System Performance Check. Perform 

a post-run system performance check before 

replacing the citrate buffer solution and 

particulate filter and before the probe is 

cleaned. The check results must not exceed 

the 100 ± 20 percent limit set forth in Section 

13.2. If this limit is exceeded, the intervening 

run is considered invalid. However, if the 

recovery efficiency is not in the 100 ± 20 

percent range, but the results do not affect 

the compliance or noncompliance status of 

the affected facility, the Administrator may 

decide to accept the results of the compliance 

test. 

8.5.2 Calibration Drift. After a run or 

series of runs, not to exceed a 24-hour period 

after initial calibration, perform a calibration 

drift test using a calibration gas (preferably 

the level that best approximates the sample 

concentration) in direct calibration mode. 

This drift must not differ from the initial 

calibration error percent by more than 3.0 

percent or 0.5 ppm. If the drift exceeds this 

limit, the intervening run or runs are 

considered valid, but a new analyzer 

calibration error test must be performed and 

passed before continuing sampling. 

9.0 Quality Control 

Section Quality control measure Effect 

8.1.2 ........................... Analyzer calibration error test .............................................. Establishes initial calibration accuracy within 5.0%. 

8.1.3, 8.5.1 ................. System performance check ................................................. Ensures accuracy of sampling/analytical procedure to 100 

± 20%. 

8.5.2 ........................... Calibration drift test .............................................................. Ensures calibration drift is within 3.0%. 

8.1.4 ........................... Interference check ................................................................ Checks for analytical interferences. 

8.3 .............................. Sampling equipment leak-check .......................................... Ensures accurate measurement of sample gas flow rate, 

sample volume. 

10.0 Calibration 

10.1 Calibrate the system using the gases 

described in Section 7.3. Perform the initial 

3-point calibration error test as described in 

Section 8.1.2 before you start the test. The 

specification in Section 13 must be met. 

Conduct an initial system performance test 

described in Section 8.1.3 as well before the 

test to validate the sampling components and 

procedures before sampling. After the test 

commences, a system performance check is 

required after each run. You must include a 

copy of the manufacturer’s certification of the 

calibration gases used in the testing as part 

of the test report. This certification must 

include the 13 documentation requirements 

in the EPA Traceability Protocol for Assay 

and Certification of Gaseous Calibration 

Standards, September 1997, as amended 

August 25, 1999. 

11.0 Analytical Procedure 

Because sample collection and analysis are 

performed together (see Section 8.0), 

additional discussion of the analytical 

procedure is not necessary. 

12.0 Calculations and Data Analysis 

12.1 Nomenclature. 

ACE = Analyzer calibration error, percent of 

calibration span. 

CD = Calibration drift, percent. 

CDir = Measured concentration of a 

calibration gas (low, mid, or high) when 

introduced in direct calibration mode, 

ppmv. 

CH2S = Concentration of the system 

performance check gas, ppmv H2S. 

CM = Average of initial and final system 

calibration bias check responses for the 

upscale calibration gas, ppmv. 

CMA = Actual concentration of the upscale 

calibration gas, ppmv. 

CO = Average of the initial and final system 

calibration bias check responses from the 

low-level (or zero) calibration gas, ppmv. 

COA = Actual concentration of the low-level 

calibration gas, ppmv. 

CS = Measured concentration of the system 

performance gas when introduced in 

system calibration mode, ppmv H2S. 

CV = Manufacturer certified concentration of 

a calibration gas (low, mid, or high), 

ppmv SO2. 

CSO2 = Unadjusted sample SO2 concentration, 

ppmv. 

CTRS = Total reduced sulfur concentration 

corrected for system performance, ppmv. 

DF = Dilution system (if used) dilution factor, 

dimensionless. 

SP = System performance, percent. 

12.2 Analyzer Calibration Error. Use 

Equation 16C–1 to calculate the 

analyzer calibration error for the low-, 

mid-, and high-level calibration gases. 


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12.3 System Performance Check. 

Use Equation 16C–2 to calculate the 

system performance. 

12.4 Calibration Drift. Use Equation 

16C–3 to calculate the calibration drift 

at a single concentration level after a 

run or series of runs (not to exceed a 24- 

hr period) from initial calibration. 

Compare the single-level calibration gas 

error (ACEn) to the original error 

obtained for that gas in the initial 

analyzer calibration error test (ACEi). 

12.5 TRS Concentration as SO2. For 

each sample or test run, calculate the 

arithmetic average of SO2 concentration 

values (e.g., 1-minute averages). Then 

calculate the sample TRS concentration 

by adjusting the average value of CSO2

for system performance using Equation 

16C–4a if you use a non-zero gas as your 

low-level calibration gas, or Equation 

16C–4b if you use a zero gas as your 

low-level calibration gas. 

13.0 Method Performance 

13.1 Analyzer Calibration Error. At 

each calibration gas level (low, mid, and 

high), the calibration error must either 

not exceed 5.0 percent of the calibration 

gas concentration or ⎢CDir¥Cv⎢ must be 

≤0.5 ppmv. 

13.2 System Performance. Each 

system performance check must not 

deviate from the system performance 

gas concentration by more than 20 

percent. Alternatively, the results are 

acceptable if ⎢Cs¥CH2S⎢ is ≤0.5 ppmv. 

13.3 Calibration Drift. The 

calibration drift at the end of any run or 

series of runs within a 24-hour period 

must not differ by more than 3.0 percent 

from the original ACE at the test 

concentration level or ⎢ACEi¥ACEn⎢ 

must not exceed 0.5 ppmv. 

13.4 Interference Check. For the 

analyzer, the total interference response 

(i.e., the sum of the interference 

responses of all tested gaseous 

components) must not be greater than 

2.5 percent of the calibration span. Any 

interference is also acceptable if the sum 

of the responses does not exceed 0.5 

ppmv for a calibration span of 5 to 10 

ppmv, or 0.2 ppmv for a calibration 

span <5 ppmv. 

14.0 Pollution Prevention [Reserved] 

15.0 Waste Management [Reserved] 

16.0 References 

1. The references are the same as in Section 

16.0 of Method 16, Section 17.0 of 

Method 16A, and Section 17.0 of Method 

6C. 

2. National Council of the Paper Industry for 

Air and Stream Improvement, Inc,. A 

Study of TRS Measurement Methods. 

Technical Bulletin No. 434. New York, 

NY. May 1984. 12p. 

3. Margeson, J.H., J.E. Knoll, and M.R. 

Midgett. A Manual Method for TRS 

Determination. Draft available from the 

authors. Source Branch, Quality 

Assurance Division, U.S. Environmental 

Protection Agency, Research Triangle 

Park, NC 27711. 

17.0 Tables, Diagrams, Flowcharts, 

and Validation Data [Reserved] 

* * * * * 

[FR Doc. 2012–18513 Filed 7–27–12; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 122 

[EPA–HQ–OW–2012–0142; FRL–9705–6] 

RIN 2040–AF40 

National Pollutant Discharge 

Elimination System Permit Regulation 

for Concentrated Animal Feeding 

Operations: Removal of Vacated 

Elements in Response to 2011 Court 

Decision 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Final rule. 

SUMMARY: The EPA is amending its 

regulations to eliminate the requirement 

that an owner or operator of a 

Concentrated Animal Feeding Operation 

(CAFO) that ‘‘proposes to discharge’’ 

must apply for a National Pollutant 

Discharge Elimination System (NPDES) 

Permit. This rulemaking also removes 

the voluntary certification option for 

unpermitted CAFOs because removal of 

the ‘‘propose to discharge’’ requirement 

renders the certification option 

unnecessary. Its purpose had been to 

allow CAFO owners and operators to 

certify that they were not violating the 

requirement that owners or operators of 

CAFOs that propose to discharge must 

seek permit coverage. Both of these 


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