53908 Federal Register / Vol. 75, No. 170 / Thursday, September 2, 2010 / Proposed Rules 

unpaved parking lots, haul and access 

roads, vehicle track-out, and disturbed 

soil associated with these activities. 

Rule 310.01 is a rule designed to limit 

the emissions of fugitive dust or 

particulate matter from disturbed 

surfaces and vehicle use in open areas 

and vacant lots, unpaved roadways and 

parking lots, livestock activities, 

erosion-caused deposition of bulk 

material on paved roadways, and 

easements, rights-of-way, and access 

roads for utilities. 

II. EPA’s Evaluation and Action 

A. How is EPA evaluating the rules? 

SIP rules must be enforceable (see 

section 110(a) of the Act) and must not 

relax existing requirements (see sections 

110(l) and 193). In addition, SIP rules 

must implement Reasonably Available 

Control Measures (RACM), including 

Reasonably Available Control 

Technology (RACT), in moderate PM 

nonattainment areas, and Best Available 

Control Measures (BACM), including 

Best Available Control Technology 

(BACT), in serious PM nonattainment 

areas (see CAA sections 189(a)(1) and 

189(b)(1)). The MCAQD regulates a PM 

nonattainment area classified as serious 

(see 40 CFR part 81), so Rule 310 and 

Rule 310.01 must implement BACM. 

Guidance and policy documents that 

we use to evaluate enforceability and 

RACM or BACM requirements 

consistently include the following: 

1. ‘‘Issues Relating to VOC Regulation 

Cutpoints, Deficiencies, and Deviations; 

Clarification to Appendix D of 

November 24, 1987 Federal Register 

Notice,’’ (Blue Book), notice of 

availability published in the May 25, 

1988 Federal Register. 

2. ‘‘Guidance Document for Correcting 

Common VOC & Other Rule 

Deficiencies,’’ EPA Region 9, August 21, 

2001 (the Little Bluebook). 

3. ‘‘State Implementation Plans; 

General Preamble for the 

Implementation of Title I of the Clean 

Air Act Amendments of 1990,’’ 57 FR 

13498 (April 16, 1992); 57 FR 18070 

(April 28, 1992). 

4. ‘‘State Implementation Plans for 

Serious PM–10 Nonattainment Areas, 

and Attainment Date Waivers for PM–10 

Nonattainment Areas Generally; 

Addendum to the General Preamble for 

the Implementation of Title I of the 

Clean Air Act Amendments of 1990,’’ 59 

FR 41998 (August 16, 1994). 

5. ‘‘PM–10 Guideline Document,’’ EPA 

452/R–93–008, April 1993. 

6. ‘‘Fugitive Dust Background 

Document and Technical Information 

Document for Best Available Control 

Measures,’’ EPA 450/2–92–004, 

September 1992. 

B. Do the rules meet the evaluation 

criteria? 

We believe these rules are consistent 

with the relevant policy and guidance. 

Our Technical Support Documents 

(TSD) on each rule has our detailed 

review and evaluation. 

C. EPA Recommendations To Further 

Improve the Rules 

We have no recommendation at this 

time. 

D. Public Comment and Final Action 

Because EPA believes the submitted 

rules fulfill all relevant requirements, 

we are proposing to fully approve them 

as described in section 110(k)(3) of the 

Act. We will accept comments from the 

public on this proposal for the next 30 

days. Unless we receive convincing new 

information during the comment period, 

we intend to publish a final approval 

action that will incorporate these rules 

into the federally enforceable SIP. 

III. Statutory and Executive Order 

Reviews 

Under the Clean Air Act, the 

Administrator is required to approve a 

SIP submission that complies with the 

provisions of the Act and applicable 

Federal regulations. 42 U.S.C. 7410(k); 

40 CFR 52.02(a). Thus, in reviewing SIP 

submissions, EPA’s role is to approve 

State choices, provided that they meet 

the criteria of the Clean Air Act. 

Accordingly, this action merely 

approves State law as meeting Federal 

requirements and does not impose 

additional requirements beyond those 

imposed by State law. For that reason, 

this action: 

• Is not a ‘‘significant regulatory 

action’’ subject to review by the Office 

of Management and Budget under 

Executive Order 12866 (58 FR 51735, 

October 4, 1993); 

• Does not impose an information 

collection burden under the provisions 

of the Paperwork Reduction Act (44 

U.S.C. 3501 et seq.); 

• Is certified as not having a 

significant economic impact on a 

substantial number of small entities 

under the Regulatory Flexibility Act 

(5 U.S.C. 601 et seq.); 

• Does not contain any unfunded 

mandate or significantly or uniquely 

affect small governments, as described 

in the Unfunded Mandates Reform Act 

of 1995 (Pub. L. 104–4); 

• Does not have Federalism 

implications as specified in Executive 

Order 13132 (64 FR 43255, August 10, 

1999); 

• Is not an economically significant 

regulatory action based on health or 

safety risks subject to Executive Order 

13045 (62 FR 19885, April 23, 1997); 

• Is not a significant regulatory action 

subject to Executive Order 13211 (66 FR 

28355, May 22, 2001); 

• Is not subject to requirements of 

Section 12(d) of the National 

Technology Transfer and Advancement 

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

application of those requirements would 

be inconsistent with the Clean Air Act; 

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. 

List of Subjects in 40 CFR Part 52 

Environmental protection, Air 

pollution control, Intergovernmental 

relations, Particulate matter, Reporting 

and recordkeeping requirements. 

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

Dated: August 23, 2010. 

Jared Blumenfeld, 

Regional Administrator, Region IX. 

[FR Doc. 2010–21959 Filed 9–1–10; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 60 

[EPA–HQ–OAR–2010–0115; FRL–9195–9] 

RIN 2060–AQ23 

Method 16C for the Determination of 

Total Reduced Sulfur Emissions From 

Stationary Sources 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Proposed rule. 

SUMMARY: This action proposes a 

method for measuring total reduced 

sulfur (TRS) emissions from stationary 

sources. The EPA is making this method 

available for general use as requested by 

a number of source testing companies 

since it has been allowed for use in the 

past on a case-by-case basis for kraft 

pulp mills and refineries. This proposed 

method would offer advantages over 


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current methods in that real-time data 

are acquired and testers are allowed to 

use analyzers and procedures for 

measuring TRS that are commonly used 

to measure sulfur dioxide (SO2). The 

proposed method would offer an 

alternative to methods that are currently 

required. 

DATES: Comments must be received on 

or before November 1, 2010. 

ADDRESSES: Submit your comments, 

identified by Docket ID No. EPA–HQ– 

OAR–2010–0115, by one of the 

following methods: 

• http://www.regulations.gov: Follow 

the on-line instructions for submitting 

comments. 

• E-mail: a-and-r-docket@epa.gov, 

attention Docket ID No. EPA–HQ–OAR– 

2010–0115. 

• Fax: (202) 566–9744, attention 

Docket ID No. EPA–HQ–OAR–2010– 

0115. 

• Mail: Method 16C for the 

Determination of Total Reduced Sulfur 

Emissions from Stationary Sources, 

Docket ID No. EPA–HQ–OAR–2010– 

0115. Environmental Protection Agency, 

Mailcode: 2822T, 1200 Pennsylvania 

Ave., NW., Washington, DC 20460. 

Please include a total of two copies. 

• Hand Delivery: Deliver your 

comments to EPA Docket Center, Public 

Reading Room, EPA West, Room 3334, 

1301 Constitution Ave., NW., 

Washington, DC 20460, attention Docket 

ID No. EPA–HQ–OAR–2010–0115. 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–2010– 

0115. EPA’s policy is that all comments 

received will be included in the public 

docket without change and may be 

made available online at http:// 

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 http:// 

www.regulations.gov or e-mail. The 

http://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 http:// 

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 http:// 

www.epa.gov/epahome/dockets.htm. 

Docket: 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., 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 http:// 

www.regulations.gov or in hard copy at 

the Method 16C for the Determination of 

Total Reduced Sulfur Emissions from 

Stationary Sources Docket, EPA/DC, 

EPA West, Room 3334, 1301 

Constitution Ave., 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 

Docket is (202) 566–1742. 

FOR FURTHER INFORMATION CONTACT: Mr. 

Foston Curtis, U.S. Environmental 

Protection Agency, Office of Air Quality 

Planning and Standards, Air Quality 

Assessment Division (E143–02), 

Research Triangle Park, NC 27711; 

telephone number: (919) 541–1063; fax 

number: (919) 541–0516; and e-mail 

address: curtis.foston@epa.gov. 

SUPPLEMENTARY INFORMATION: 

I. General Information 

A. Does this action apply to me? 

Method 16C applies to the 

measurement of TRS at kraft pulp mills 

subject to Subpart BB of the New Source 

Performance Standards (NSPS). 

Currently, Methods 16, 16A, and 16B 

are allowed at these facilities. Method 

16C would offer an additional 

alternative. The methods required under 

Subpart BB are sometimes used in 

special cases under the petroleum 

refineries NSPS (Subpart J). Method 16C 

may be applicable to other sources 

regulated by State and local regulations 

that specify the use of Methods 16, 16A, 

or 16B if desired. The entities that are 

potentially affected by this proposal are 

included in the following table. 

Category NAICSa

Examples of 

regulated 

entities 

Industry .......... 324110 Petroleum Refineries. 

Industry .......... 322110 Kraft Pulp Mills. 

a North American Industry Classification 

System. 

B. What should I consider as I prepare 

my comments for EPA? 

1. Submitting CBI. Do not submit this 

information to EPA through http:// 

www.regulations.gov or e-mail. Clearly 

mark any of the information that you 

claim to be CBI. For CBI information in 

a disk or CD–ROM that you mail to EPA, 

mark the outside of the disk or CD–ROM 

as CBI and then identify electronically 

within the disk or CD–ROM the specific 

information that is claimed as CBI. In 

addition to one complete version of the 

comment that includes information 

claimed as CBI, a copy of the comment 

that does not contain the information 

claimed as CBI must be submitted for 

inclusion in the public docket. 

Information so marked will not be 

disclosed except in accordance with 

procedures set forth in 40 CFR part 2. 

2. Tips for Preparing Your Comments. 

When submitting comments, remember 

to: 

• Identify the rulemaking by docket 

number and other identifying 

information (subject heading, Federal 

Register date and page number). 

• Follow directions—The agency may 

ask you to respond to specific questions 

or organize comments by referencing a 

Code of Federal Regulations (CFR) part 

or section number. 

• Explain why you agree or disagree, 

suggest alternatives, and substitute 

language for your requested changes. 

• Describe any assumptions and 

provide any technical information and/ 

or data that you used. 

• If you estimate potential costs or 

burdens, explain how you arrived at 

your estimate in sufficient detail to 

allow for it to be reproduced. 

• Provide specific examples to 

illustrate your concerns, and suggest 

alternatives. 

• Explain your views as clearly as 

possible, avoiding the use of profanity 

or personal threats. 

• Make sure to submit your 

comments by the comment period 

deadline identified. 


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C. Where can I get a copy of this 

document? 

In addition to being available in the 

docket, an electronic copy of this 

proposed rule is also available on the 

Worldwide Web (WWW) through the 

Technology Transfer Network (TTN). 

Following the Administrator’s signature, 

a copy of this proposed rule will be 

posted on the TTN’s policy and 

guidance page for newly proposed or 

promulgated rules at the following 

address: http://www.epa.gov/ttn/oarpg/. 

The TTN provides information and 

technology exchange in various areas of 

air pollution control. 

D. How is this document organized? 

The information in this preamble is 

organized as follows: 

I. General Information 

A. Does this action apply to me? 

B. What should I consider as I prepare my 

comments for EPA? 

C. Where can I get a copy of this 

document? 

D. How is this document organized? 

II. Background and Summary of Method 16C 

III. 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 

Risks and Safety Risks 

H. Executive Order 13211: Actions 

Concerning Regulations That 

Significantly Affect Energy Supply, 

Distribution, or Use 

I. National Technology Transfer 

Advancement Act 

J. Executive Order 12898: Federal Actions 

To Address Environmental Justice in 

Minority Populations and Low-Income 

Populations 

II. Background and Summary of 

Method 16C 

The EPA is making Method 16C 

available for general use as requested by 

a number of source testing companies 

since it has been allowed on a case-bycase basis in the past. The proposed 

method would offer an alternative to 

methods that are currently required. 

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 described 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 

prescribed in Method 6C. In this 

method, we are combining the proven 

combustion process of Method 16A with 

the analytical techniques currently used 

for SO2 to form a new, improved 

method for measuring TRS. 

This method would become available 

as an option for use in connection with 

the New Source Performance Standards 

for kraft pulp mills and possibly 

petroleum refineries. We have allowed 

its use in approximately four tests over 

the past 10 years 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 are 

contained in the method to 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. 

III. 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 is 

defined at 5 CFR 1320.3(b). The method 

being proposed in this action does not 

add information collection requirements 

but makes an additional optional 

procedure available for use by affected 

parties. 

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 

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 today’s proposed rule on 

small entities, I certify that this action 

will not have a significant economic 

impact on a substantial number of small 

entities. This rulemaking does not 

impose emission measurement 

requirements beyond those specified in 

the current regulations, nor does it 

change any emission standard. As such, 

it will not present a significant 

economic impact on a substantial 

number of small businesses. 

We continue to be interested in the 

potential impacts of the proposed rule 

on small entities and welcome 

comments on issues related to such 

impacts. 

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. The 

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. This 

action makes available a new optional 

method for measuring pollutants but 

adds no new requirements. 

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 action 

simply makes an optional test method 


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available for affected sources who desire 

to use it. Thus, Executive Order 13132 

does not apply to this action. In the 

spirit of Executive Order 13132, and 

consistent with EPA policy to promote 

communications between EPA and State 

and local governments, EPA specifically 

solicits comment on this proposed rule 

from State and local officials. 

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 action makes available a 

new optional method for measuring 

pollutants but adds no new 

requirements. Thus, Executive Order 

13175 does not apply to this action. EPA 

specifically solicits additional comment 

on this proposed action from tribal 

officials. 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

Risks and Safety Risks 

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 action 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 (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. NTTAA directs EPA to provide 

Congress, through OMB, explanations 

when the Agency decides not to use 

available and applicable voluntary 

consensus standards. This proposed 

rulemaking does not involve technical 

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. 

EPA has determined that this 

proposed 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 rule adds an 

optional test method and does not cause 

emission increases from regulated 

sources. 

Method 16C for the Determination of 

Total Reduced Sulfur Emissions From 

Stationary Sources 

List of Subjects in 40 CFR Part 60 

Environmental protection, Air 

pollution control, Test methods and 

procedures, and Performance 

specifications. 

Dated: August 26, 2010. 

Lisa P. Jackson, 

Administrator. 

For the reasons stated in the 

preamble, the Environmental Protection 

Agency proposes to amend title 40, 

chapter I of the Code of Federal 

Regulations 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. Add Method 16C to Appendix A– 

6 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. 


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1.3 Data Quality Objectives. Adherence to 

the requirements described in Method 16C 

will enhance the quality of the data obtained 

from air pollutant sampling methods. 

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 regulated by the emission 

standards, 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. An example measurement 

system is shown in Figure 16C–1 and 

component parts are discussed below. 

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 heatresistant 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 boredout 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-μm 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 

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 constructed of material that is nonreactive to the gas it contacts. For dilutiontype 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 CO2 in N2. 

(d) SO2 and O2 in N2. 

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

(f) CO2/NOX gas mixture in N2.


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(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 

percent (absolute) O2 and 1 percent (absolute) 

CO2 of the O2 and CO2 concentrations of the 

effluent samples as introduced to the 

analyzer. Alternatively, for fluorescencebased 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 ambient-level 

fluorescence analyers that are used in 

conjunction with sample dilution systems. 

7.4 System Performance Check Gas. You 

must use hydrogen sulfide (100 ppmv or less) 

in nitrogen, stored in aluminum cylinders 

with concentration certified by the 

manufacturer. 

Note: Alternatively, hydrogen sulfide 

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 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. Same as 

in Method 16A, Section 8.5, except samples 

need not be 30 minutes in duration, and the 

TRS sample concentration measured between 

system performance checks is corrected by 

the average of the two system performance 

samples. System performance checks are 

conducted before sampling begins (optional) 

and after each sample run (mandatory). 

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. As an alternative to the 

initial leak-test, the system performance 

check in Section 8.3.2 may be performed to 

verify the integrity of components. 

8.3.2 Initial System Performance Check. 

A system performance check using the test 

gas (Section 7.4) is required 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. (This preconditioning may not be 

necessary if the initial system performance 

check is performed.) Begin the sampling and 

analysis. Determine the concentration of SO2

for the prescribed sample or run time. 

Method 16 defines a test run as sampling 

over a period of not less than 3 hours or more 

than 6 hours when testing kraft pulp mills. 

For Method 16C to be consistent with 

Method 16, a run may be obtained by: (1) 

sampling for three 60-minute intervals or (2) 

sampling for a 3-hour interval. (Three runs 

constitute a test.) 

8.5 Post-Run Evaluations 

8.5.1 System Performance Check. Perform 

a post-run system performance check 

(Section 8.5 of Method 16A) 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 13.3. If this 

limit is exceeded, the intervening run or runs 

are 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 

manufacturer certified concentration of the 

gas by more than 3 percent or 0.5 ppm. If the 

drift exceeds this limit, the intervening run 

or runs are considered valid, but a new 

analyzer calibration test must be performed 

and passed before continuing sampling. 

9.0 Quality Control 

Section Quality control measure Effect 

8.1 ...................... Sampling equipment leak-check and 

calibration.

Ensures accurate measurement of sample gas flow rate, sample volume. 

8.1.2 ................... Analyzer calibration error ........................ Establishes initial calibration accuracy within 2%. 

8.3.2, 8.5.1 ........ System performance check ..................... Ensures accuracy of sampling/analytical procedure within 20%. 

8.5.2 ................... Calibration drift test ................................. Ensures a stable calibration within 3%. 

10.0 .................... Interference check ................................... Checks for analytical interferences. 


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10.0 Calibration 

10.1 Calibrate the system using the gases 

described in Section 7.3. The initial 3-point 

calibration error test as described in Section 

8.1.2 is required and must meet the 

specifications in Section 13 before you start 

the test. We recommend you conduct an 

initial system performance test described in 

Section 8.1.4 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. 

BWO = Fraction of volume of water vapor in 

the gas stream. 

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. 

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 = Sample SO2 concentration, ppmv. 

CTRS = Total reduced sulfur concentration 

corrected for system performance and 

adjusted to dry conditions, ppmv. 

SP = System performance, percent. 

12.2 Analyzer Calibration Error. Use 

Equation 16C–1 to calculate the analyzer 

calibration error for the low-, mid-, and highlevel calibration gases. 

ACE = C C

C

Dir v

v

− ×100 Eq. 16C-1

12.3 System Performance. Use Equation 

16C–2 to calculate the system performance. 

SP = C C

C

S H2S

H2S

− ×100 Eq. 16C-2

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 calibration 

gas response to the original response 

obtained for the gas in the initial analyzer 

calibration test (ACEi). 

CD = ACE ACE i n − Eq. 16C-3

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 using Equation 16C–4. 

C = C

SP B TRS

SO2

WO 1− − Eq. 16C-4

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 |Cs¥Cv| must be ≤ 0.5 ppmv. 

13.2 System Performance. The system 

performance check result must be within 20 

percent of the system performance gas 

concentration. Alternatively, the results are 

acceptable if |Cs¥Cdir| 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 percent from the original ACE 

at that 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 2.50 percent of the calibration span. The 

results are 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. 2010–21954 Filed 9–1–10; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 140 

[EPA–R09–OW–2010–0438; FRL–9196–3] 

RIN 2009–AA04 

Marine Sanitation Devices (MSDs): 

Proposed Regulation To Establish a 

No Discharge Zone (NDZ) for California 

State Marine Waters 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Proposed rule. 

SUMMARY: EPA is proposing to establish 

a No Discharge Zone (NDZ) for sewage 

discharges from: Large passenger 

vessels; and oceangoing vessels of 300 

gross tons or more (referred to 

throughout this proposed rule as ‘‘Large 

oceangoing vessels’’) with two days or 

more sewage holding capacity to 

California State marine waters pursuant 

to Section 312(f)(4)(A) of the Clean 

Water Act (CWA), 33 U.S.C. 

1322(f)(4)(A). This action is being taken 

in response to an April 5, 2006 

application from the California State 

Water Resources Control Board (State) 

requesting establishment of this NDZ. 

Under Section 312(f)(4)(A), if EPA 

determines upon application by a State 

that the protection and enhancement of 

the quality of specified waters within 

such State requires such a prohibition, 

then EPA shall by regulation completely 

prohibit the discharge of any sewage 

(whether treated or not) from a vessel 

into such waters. California State 

marine waters would be defined as the 

territorial sea measured from the 

baseline, as determined in accordance 

with the Convention on the Territorial 

Sea and the Contiguous Zone, and 

extending seaward a distance of three 

miles, and would also include all 

enclosed bays and estuaries subject to 

tidal influences from the Oregon border 

to the Mexican border. (Federal Clean 

Water Act Section 502(8)). State marine 

waters also extend three miles from 

State islands, including the Farallones 

and the Northern and Southern Channel 

Islands. A map of California State 

marine waters can be obtained or 

viewed at the EPA’s Web site at 

http://www.epa.gov/region9/water/nodischarge/overview.html, or by calling 

(415) 972–3476. It should be noted that 

effective March 2009, the National 

Oceanic and Atmospheric 

Administration (NOAA) established 

prohibitions on the discharge of sewage 

from large vessels in waters within the 

boundaries of the four National Marine 


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