40000 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 

List of Subjects in 33 CFR Part 165 

Harbors, Marine safety, Navigation 

(water), Reporting and recordkeeping 

requirements, Security measures, 

Waterways. 

For the reasons discussed in the 

preamble, the Coast Guard amends 33 

CFR parts 165 as follows: 

PART 165—REGULATED NAVIGATION 

AREAS AND LIMITED ACCESS AREAS 

■ 1. The authority citation for part 165 

continues to read as follows: 

Authority: 33 U.S.C. 1231; 46 U.S.C. 

Chapters 701, 3306, 3703; 50 U.S.C. 191, 195; 

33 CFR 1.05–1, 6.04–1, 6.04–6, and 160.5; 

Pub. L. 107–295, 116 Stat. 2064; Department 

of Homeland Security Delegation No. 0170.1. 

■ 2. Add § 165.T09–0547 to read as 

follows: 

§ 165.T09–0547 Safety Zone; Grand Haven 

4th of July fireworks; Grand River, Grand 

Haven, MI. 

(a) Location. All waters of the Grand 

River within the arc of a circle with an 

800 foot radius with a center in position 

43° 3′ 55.7′′ N and 86° 14′ 13.8′′ W (NAD 

83). 

(b) Effective and Enforcement Period. 

This rule is effective and will be 

enforced from 9:30 p.m. until 11:30 p.m. 

on July 4, 2013. 

(c) Regulations. (1) In accordance with 

the general regulations in section 165.23 

of this part, entry into, transiting, or 

anchoring within this safety zone is 

prohibited unless authorized by the 

Captain of the Port, Lake Michigan or 

his designated on-scene representative. 

(2) This safety zone is closed to all 

vessel traffic, except as may be 

permitted by the Captain of the Port, 

Lake Michigan or his designated onscene representative. 

(3) The ‘‘on-scene representative’’ of 

the Captain of the Port, Lake Michigan 

is any Coast Guard commissioned, 

warrant or petty officer who has been 

designated by the Captain of the Port, 

Lake Michigan to act on his behalf. 

(4) Vessel operators desiring to enter 

or operate within the safety zone shall 

contact the Captain of the Port, Lake 

Michigan or his on-scene representative 

to obtain permission to do so. The 

Captain of the Port, Lake Michigan or 

his on-scene representative may be 

contacted via VHF Channel 16. Vessel 

operators given permission to enter or 

operate in the safety zone must comply 

with all directions given to them by the 

Captain of the Port, Lake Michigan, or 

his on-scene representative. 

Dated: June 21, 2013. 

M.W. Sibley, 

Captain, U.S. Coast Guard, Captain of the 

Port, Lake Michigan. 

[FR Doc. 2013–16043 Filed 7–2–13; 8:45 am] 

BILLING CODE 9110–04–P 

DEPARTMENT OF HOMELAND 

SECURITY 

Coast Guard 

33 CFR Part 165 

[Docket No. USCG–2013–0331] 

RIN 1625–AA00 

Eighth Coast Guard District Annual 

Safety Zones; Riverfront Independence 

Festival Fireworks; Ohio River 607.0– 

609.0; New Albany, KY 

AGENCY: Coast Guard, DHS. 

ACTION: Notice of enforcement of 

regulation. 

SUMMARY: The Coast Guard will enforce 

a Safety Zone for the Riverfront 

Independence Festival Fireworks on the 

Ohio River 607.0 to 609.0 from 9:30 

p.m. until 10:30 p.m. on July 3, 2013. 

This action is necessary for the 

safeguard of participants and spectators, 

including all crews, vessels, and 

persons on navigable waters during the 

Riverfront Independence Festival 

Fireworks. During the enforcement 

period, in accordance with a previously 

established Safety Zone, entry into, 

transiting through or anchoring in the 

Safety Zone is prohibited to all vessels 

not registered with the sponsor as 

participants or official patrol vessels, 

unless specifically authorized by the 

Captain of the Port (COTP) Ohio Valley 

or a designated representative. 

DATES: The regulations in 33 CFR 

165.801 will be enforced from 9:30 p.m. 

until 10:30 p.m. on July 3, 2013. 

FOR FURTHER INFORMATION CONTACT: If 

you have questions on this notice of 

enforcement, call Petty Officer Second 

Class Catherine M. Lawson, Coast Guard 

Sector Ohio Valley at 502–779–5432, or 

by email at 

Catherine.M.Lawson@uscg.mil. 

SUPPLEMENTARY INFORMATION: The Coast 

Guard will enforce the Safety Zone for 

the annual Riverfront Independence 

Festival Fireworks listed in 33 CFR 

165.801 Table 1, Table No. 18; Sector 

Ohio Valley, No. 21 on July 3, 2013 from 

9:30 p.m. until 10:30 p.m. 

Under the provisions of 33 CFR 

165.801, entry into the Safety Zone 

listed in Table 1, Table No. 18; Sector 

Ohio Valley, No. 21 is prohibited unless 

authorized by the Captain of the Port or 

a designated representative. Persons or 

vessels desiring to enter into or pass 

through the Safety Zone must request 

permission from the Captain of the Port 

or a designated representative. If 

permission is granted, all persons and 

vessels shall comply with the 

instructions of the Captain of the Port or 

designated representative. 

This notice is issued under authority 

of 5 U.S.C. 552(a); 33 U.S.C. 1231; 46 

U.S.C. Chapter 701, 3306, 3703; 50 

U.S.C. 191, 195; 33 CFR 1.05–1, 6.04–1, 

6.04–6, and 160.5; Public Law 107–295, 

116 Stat. 2064; Department of Homeland 

Security Delegation No. 0170.1. In 

addition to this notice in the Federal 

Register, the Coast Guard will provide 

the maritime community with advance 

notification of this enforcement period 

via Local Notice to Mariners and Marine 

Information Broadcasts. 

If the Captain of the Port Ohio Valley 

or Patrol Commander determines that 

the Safety Zone need not be enforced for 

the full duration stated in this notice of 

enforcement, he or she may use a 

Broadcast Notice to Mariners to grant 

general permission to enter the 

regulated area. 

Dated: June 13, 2013. 

L.W. Hewett, 

Captain, U.S. Coast Guard, Captain of the 

Port Ohio Valley. 

[FR Doc. 2013–16046 Filed 7–2–13; 8:45 am] 

BILLING CODE 9110–04–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 50 

[EPA–HQ–OAR–2012–0210; FRL–9822–1] 

RIN 2060–AP89 

Method for the Determination of Lead 

in Total Suspended Particulate Matter 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Final rule. 

SUMMARY: The EPA is establishing a new 

Federal Reference Method (FRM) for 

measuring Lead (Pb) in total suspended 

particulate matter (TSP) collected from 

ambient air. This method is intended for 

use by analytical laboratories 

performing the analysis of Pb in TSP to 

support data collection for the Pb 

National Ambient Air Quality Standard 

(NAAQS). The existing FRM for Pb is 

designated as a new Federal Equivalent 

Method (FEM), and the currently 

designated FEMs are retained. This 

action avoids any disruption to existing 

Pb monitoring networks and data 

collection and does not affect the FRM 

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Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 40001 

for TSP sample collection (High-Volume 

Method). 

DATES: This final rule is effective on 

August 2, 2013. 

ADDRESSES: The EPA has established a 

docket for this action under Docket No. 

EPA–HQ–OAR–2012–0210. All 

documents in the docket are listed on 

the www.regulations.gov Web site. 

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 

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 Air Docket 

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 additional 

information about EPA’s public docket 

visit the EPA Docket Center homepage 

at: http://www.epa.gov/epahome/ 

dockets.htm. 

FOR FURTHER INFORMATION CONTACT: Ms. 

Joann Rice, Office of Air Quality 

Planning and Standards, Air Quality 

Assessment Division, Ambient Air 

Monitoring Group (C304–06), U.S. 

Environmental Protection Agency, 

Research Triangle Park, North Carolina 

27711; telephone number: (919) 541– 

3372; fax number: (919) 541–1903; 

email address: rice.joann@epa.gov. 

SUPPLEMENTARY INFORMATION: 

Table of Contents 

I. Background 

A. Purpose of the New Reference Method 

B. Rationale for Selection of the New 

Reference Method 

C. Comments on the Proposed Rule 

D. Conclusions 

II. Summary of Method 

III. 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 

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. Background 

A. Purpose of the New Reference 

Method 

On November 12, 2008, the EPA 

substantially strengthened the NAAQS 

for Pb (73 FR 66964). The EPA revised 

the level of the primary (health-based) 

standard from 1.5 micrograms per cubic 

meter (mg/m3) of Pb to 0.15 mg/m3 of Pb 

measured in TSP and revised the 

secondary (welfare-based) standard to 

be identical in all respects to the 

primary standard. The current Pb in 

TSP FRM is based on Flame Atomic 

Absorption Spectroscopy (FAAS) as 

specified in 40 CFR part 50, Appendix 

G. The FRM in Appendix G was 

originally promulgated in 1978 when 

FAAS was widely used and considered 

the best available method to support Pb 

NAAQS data collection at a level of 1.5 

mg/m3. A new Pb in TSP FRM is needed 

to: (1) Take advantage of improved 

extraction methods that are now 

available with improved precision, 

sample throughput, and extraction 

efficiency; (2) address advances in 

measurement technology that have 

occurred since promulgation of the 

original FRM; and (3) address the 

improved measurement sensitivity 

(detection limits) needed in response to 

the tightened Pb NAAQS. 

The reference method for Pb in TSP 

includes two parts: the analysis method 

for Pb in TSP as specified in 40 CFR 50, 

Appendix G, and the reference method 

for high-volume sampling of TSP as 

specified in 40 CFR 50, Appendix B. 

The new FRM is for the analysis of Pb 

in TSP based on Inductively Coupled 

Plasma Mass Spectrometry (ICP–MS). 

The FRM serves as the definitive 

method for routinely analyzing Pb for 

comparison to the NAAQS and also 

serves as the standard of comparison for 

determining equivalence of candidate 

FEMs. This method replaces the existing 

method in 40 CFR 50, Appendix G. The 

FRM that was promulgated in 1978 as 

Appendix G becomes an approved FEM 

and the currently designated FEMs are 

retained. The EPA believes this is 

appropriate because the new FRM is 

based on two methods that were tested 

and approved as FEMs (EQL–0510–191 

and EQL–0710–192) to ensure 

comparability with the FAAS method. 

This approach permits continued use of 

the legacy FRM (as an FEM) and the 

existing FEMs. This avoids any 

disruption to state and local air 

monitoring agencies using these 

methods for Pb monitoring. The 

reference method for high volume 

sampling of TSP will continue to be 

performed in accordance with the FRM 

described in Appendix B, and, 

therefore, is not included as part of this 

FRM. 

With the tightened NAAQS in 2008 

and the need for increased measurement 

sensitivity, an improved measurement 

technology has become available to 

meet the needs of the current NAAQS. 

The FAAS method is less frequently 

used in the Pb ambient monitoring 

network (about 10 percent of the sites 

reported Pb in TSP data to the EPA’s Air 

Quality System in 2012 using the FAAS 

method) and ICP-based methods have 

increased in popularity. Recently, the 

FAAS method has mainly been used as 

the reference method for testing and 

designation of candidate FEMs for Pb in 

accordance with 40 CFR 53.33. With the 

lowered Pb concentration testing range 

in Part 53 and new requirement for a 

Method Detection Limit (MDL) of 

0.0075 mg/m3 (described below), the 

FAAS method sensitivity and 

availability of laboratories with FAAS 

capability have created some challenges 

for comparability testing of new FEMs. 

In 2008, the EPA also revised the 

performance-based requirements for Pb 

FEMs in Part 53. The performance 

requirements were revised to be 

consistent with the revised Pb NAAQS 

level. Specifically, the Pb concentration 

range at which the FEM comparability 

testing is conducted was lowered to a 

range of 0.045 to 0.375 mg/m3 and the 

requirement for a minimum method 

detection limit was established at 

0.0075 mg/m3. The detection limit of the 

new FRM is more than adequate to meet 

the reduced testing range and detection 

limit requirements. The FRM’s average 

detection limit for Pb-spiked filters is 

estimated at 0.00009 mg/m3, which is 

well below the requirement of 0.0075 

mg/m3. 

B. Rationale for Selection of the New 

Reference Method 

The FRM is based on two recently 

approved FEMs for extracting Pb from 

glass fiber filters for subsequent analysis 

by ICP–MS: (1) Method EQL–0510–191 

which uses a heated (80 ± 5°C) 

ultrasonic water bath with 1.03M nitric 

(HNO3)/2.23M hydrochloric (HCl) acids, 

and (2) Method EQL–0710–192 which 

uses a heated (95 ± 5°C) graphite block 

(hot block) with 3.5 percent volume/ 

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40002 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 

1CASAC’s final report on the Approach for the 

Development of a New Federal Reference Method 

(FRM) for Lead in Total Suspended Particulates 

(Pb–TSP) can be found at: http://yosemite.epa.gov/ 

sab/sabproduct.nsf/ 

DA39026E54BAF46E8525781D00606633/$File/ 

EPA-CASAC-11-002-unsigned.pdf. 

2FEM EQL–0400–0140 (65 FR 26603, May 8, 

2000). 3The list of current FEMs is located at: http:// 

epa.gov/ttn/amtic/files/ambient/criteria/referenceequivalent-methods-list.pdf. 

4Refer to: http://water.epa.gov/scitech/methods/ 

cwa/det/index.cfm for EPA’s Procedures for 

Detection and Quantitation. 

volume (v/v) HNO3. In selecting this 

methodology, the EPA’s primary 

considerations were: methods that have 

already been tested and approved 

against the FAAS method; use of 

equipment that is commonly used; a 

method that is practical (use of a single 

vessel for the entire extraction process 

and storage); and a method with 

improved sensitivity and throughput to 

increase efficiency and cost 

effectiveness over the legacy FRM. ICP– 

MS was chosen as the analytical 

technique because it has improved 

sensitivity, selectivity, linear range, and 

is more readily available than FAAS in 

laboratories today. 

The FRM uses methods from two 

existing FEMs that have been proven 

comparable to FAAS and, therefore, 

retains consistency with the legacy FRM 

(Rice, 2013). The FRM is only intended 

for the analysis of Pb in TSP and allows 

for the use of glass fiber, quartz, or 

polytetrafluoroethylene (PTFE) filters. 

HNO3 alone is sufficient for the 

extraction of Pb; however, the ultrasonic 

extraction method includes HCl to allow 

monitoring agencies some flexibility for 

future needs that may include the 

extraction of other metals. HCl is 

needed to aid the extraction of other 

metals that are not easily brought into 

solution with HNO3 alone. The FRM 

was evaluated for the extraction of Pb 

only. If the FRM is used for metals other 

than Pb, the user must evaluate the 

FRM’s applicability before use. The hot 

block extraction method uses only 

HNO3 and must also be evaluated by the 

user before use to extract metals other 

than Pb. 

The approach and key specifications 

of the method were submitted for peer 

review to the Clean Air Scientific 

Advisory Committee (CASAC) Ambient 

Air Monitoring and Methods 

Subcommittee. Public meetings were 

held to discuss the method and related 

monitoring issues on September 15, 

2010. Comments on the method and 

approach were provided in writing in a 

letter dated November 30, 2010 (EPA– 

CASAC–11–002),1 forwarded by CASAC 

to the Administrator. 

The CASAC was supportive of the 

ICP–MS analytical method and found 

the approach to be appropriate with 

superior sensitivity and specificity for 

Pb. The CASAC recommended a 

strategy, using a performance-based 

FRM, to provide flexibility for use of 

non-FRM or FEM measurement methods 

and recommended that a third 

extraction method (microwave) be 

added to the FRM for its greater sample 

throughput and potential for reduced 

sample-to-sample variability. The 

CASAC viewed the comprehensiveness 

of the FRM test plan to be appropriate, 

and recommended that the EPA 

consider separating the extraction 

methods from the analytical methods so 

that any of the FRM extraction methods 

can be used with any of the FRM 

analytical measurement methods. 

The federal reference and equivalence 

testing method for Pb in 40 CFR 53.33 

serves as the performance-based method 

approach for the FEM approval process. 

Candidate methods are tested using the 

performance specifications of part 40 

CFR part 53 for acceptance and approval 

as equivalent methods. Users also have 

the flexibility to test and submit 

additional extraction and analysis 

methods for review and approval as 

equivalent methods. The EPA believes 

that microwave extraction is a viable 

option and is already available as an 

approved FEM.2 The ultrasonic and hot 

block approaches are sufficient for the 

extraction of Pb and provide high 

sample throughput, low consumable 

costs, and lower equipment costs while 

minimizing the risk of cross 

contamination and sample loss. In 

addition, the EPA believes that the 

existing FEMs 3 currently provide a 

wide variety of extraction and analytical 

methods and the EPA strongly 

encourages monitoring agencies to 

consider adopting one of the already 

approved FEMs in lieu of submitting 

new FEM applications. The FRM has 

two extraction methods (heated 

ultrasonic and hot block) and one 

analytical method (ICP–MS). The FRM 

allows for the use of either of the two 

extraction methods specified with the 

ICP–MS analytical method. The method 

also allows for the use of glass fiber, 

PTFE, or quartz filter media for the 

collection of Pb in TSP. 

C. Comments on the Proposed Rule 

On February 5, 2013, the EPA 

proposed a new FRM for determination 

of Pb in TSP (78 FR 8066) and solicited 

comment on the proposed method. The 

EPA received one public comment by 

the close of the public comment period 

on March 7, 2013. The commenter 

questioned the meaning of the MDLs 

estimated from the analysis of blanks. 

The commenter recommended that an 

MDL estimated from blanks include the 

mean of the blanks and be consistent 

with the Report of the Federal Advisory 

Committee on Detection and 

Quantitation (FACDQ) Approaches and 

Uses in Clean Water Act Programs 

(FACDQ, 2007). The Federal Advisory 

Committee recommended that EPA 

adopt a new procedure for estimated 

method sensitivity and replace 40 CFR 

136, Appendix B (Definition and 

Procedure for the Determination of the 

Method Detection Limit) with the new 

procedure. The FACDQ procedure 

described an approach for calculating 

MDLs and quantitation limits. The EPA 

conducted a pilot study to assess 

whether the procedure recommended by 

the FACDQ could generate reliable 

estimates of the lowest concentration at 

which measurement quality objectives 

could be achieved (U.S. EPA, 2011). 

Based on the pilot study results, the 

EPA concluded that none of the 

procedures tested consistently generated 

accurate estimates of the lowest 

concentration at which the study 

measurement quality objectives were 

achieved. The EPA believes that more 

development and testing of the FACDQ 

procedure are warranted.4 Accordingly, 

based on the currently available 

information, the EPA believes that the 

procedures identified in 40 CFR 135, 

Appendix B are a more appropriate 

basis for estimating MDLs for the FRM. 

The EPA provided estimates in the 

proposed rule for MDLs based on 

reagent/filter blanks and reagent/filter 

blanks spiked with a Pb solution. The 

EPA estimated MDLs based on 40 CFR 

136, Appendix B which recommends 

that MDLs be determined using a 

concentration value that is between 1 

and 5 times the estimated MDL. 

However, 40 CFR 136, Appendix B does 

not specify the use of reagent/filter 

blanks for estimating the detection limit. 

The estimate of MDLs based on reagent/ 

filter blanks is not consistent with 40 

CFR 136, Appendix B; therefore, the 

MDL estimates from reagent/filter 

blanks have been removed. The 

remaining MDL estimates in Tables 1, 3, 

and 5 were determined using reagent/ 

filter blanks that were spiked with Pb at 

three times the estimated detection limit 

of 0.001 mg/mL. The MDLs were 

estimated to demonstrate method 

performance that is more than adequate 

to meet the MDL requirements of 0.0075 

mg/m3 for Pb in TSP. It is recommended 

that laboratories performing this method 

initially estimate MDLs in accordance 

with 40 CFR Part 136, Appendix B and 

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confirm the MDLs annually. In addition, 

the EPA recommends that laboratories 

consider performing the optional 

iterative procedure in Part 136, 

Appendix B to verify the reasonableness 

of the initially estimated MDL and 

subsequent MDL determinations. 

D. Conclusions 

After consideration of the public 

comment on the estimate of MDL from 

reagent/filter blanks, the EPA has 

concluded that the rule should be 

consistent with the provisions of 40 CFR 

Part 136, Appendix B. Accordingly, any 

language referring to the estimate of 

MDLs using reagent/filter blanks and 

the MDLs estimated from reagent/filter 

blanks in Tables 1, 3, and 5 have been 

removed. The MDLs estimated from the 

Pb-spiked reagent/filter blanks remain 

and demonstrate that the method has 

more than adequate sensitivity to 

support the Pb-TSP MDL requirement of 

0.0075 mg/m3. No other comments were 

received nor revisions made to the 

proposed rule. The rule is otherwise 

finalized as proposed. 

II. Summary of Method 

The FRM uses the ambient air sample 

collection procedures of the highvolume TSP method (40 CFR Part 50, 

Appendix B) and the analytical 

procedure for the measurement of Pb 

based on ICP–MS. Two extraction 

methods are used: One using heated 

ultrasonic and one using hot block 

digestion. The extraction methods and 

ICP–MS analysis method have been 

tested and found acceptable for 

extraction of Pb from glass fiber, PTFE, 

or quartz filter media. This method also 

met the precision and bias goals for Pb 

in TSP (Rice 2013). This method 

replaces the previous FRM specified in 

40 CFR Part 50, Appendix G. Although 

the previous FRM in Appendix G is 

adequate, this method offers advantages 

over the previous FRM by providing 

improved sensitivity or detection limits, 

precision, sample throughput, and 

extraction efficiency. 

III. 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 rule is 

to promulgate a new FRM for Pb in TSP, 

and to designate the existing FRM as an 

FEM, and does not add any information 

collection requirements beyond those 

imposed by the existing Pb monitoring 

requirements. 

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 rule on small entities, I 

certify that this action will not have a 

significant economic impact on a 

substantial number of small entities. 

This rule will not impose any additional 

monitoring requirements beyond those 

specified in the current regulations, nor 

will it require any changes in approved 

monitoring methods. As such, it will not 

impose any requirements on small 

entities. 

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. This 

action establishes a new FRM for state 

and local air monitoring agencies to use 

as one of the approved methods for 

measurement of Pb in TSP and to 

designate the existing FRM as an FEM. 

It does not create any additional 

monitoring requirements or require 

changes in approved monitoring 

methods. 

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 

establishes a new FRM for state and 

local air monitoring agencies to use as 

one of the approved methods for 

measurement of Pb in TSP and 

designates the existing FRM as an FEM. 

This action does not create any new 

monitoring requirements or require any 

changes in approved monitoring 

methods. 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 rule imposes no 

requirements on tribal governments. 

This action establishes a new FRM for 

state and local air monitoring agencies 

to use as one of the approved methods 

for measurement of Pb in TSP and 

designates the existing FRM as an FEM. 

This action does not create any new 

monitoring requirements, nor require 

any changes in approved monitoring 

methods. Thus, Executive Order 13175 

does not apply to this action. 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

and Safety Risks 

The EPA interprets EO 13045 (62 F.R. 

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. 

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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 

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. NTTAA directs the EPA to 

provide Congress, through OMB, 

explanations when the agency decides 

not to use available and applicable 

voluntary consensus standards. 

This rule involves environmental 

monitoring and measurement consistent 

with the agency’s Performance Based 

Measurement System (PBMS). The 

PBMS approach is intended to be more 

flexible and cost-effective for the 

regulated community; it is also intended 

to encourage innovation in analytical 

technology and improved data quality. 

Specifically, this rule establishes a new 

FRM for Pb in TSP measurements. The 

EPA used voluntary consensus 

standards in the preparation of this 

FRM. The FRM is the benchmark 

against which all ambient monitoring 

methods are compared. The FRM is not 

a voluntary consensus standard. 

The FEM equivalency criteria 

contained in 40 CFR part 53 constitute 

performance criteria. Therefore, the EPA 

is not precluding the use of any method, 

whether it constitutes a voluntary 

consensus standard or not, as long as it 

meets the specified performance criteria 

in 40 CFR part 53 and is approved by 

the EPA pursuant to those regulations. 

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 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 action establishes a 

new FRM for state and local air 

monitoring agencies to use as one of the 

approved methods for measurement of 

Pb in TSP and designates the existing 

FRM as an FEM. 

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 

August 2, 2013. 

List of Subjects in 40 CFR Part 50 

Environmental protection, Air 

pollution control, and Lead. 

Dated: June 26, 2013. 

Bob Perciasepe, 

Acting Administrator. 

For reasons stated in the preamble, 

title 40, chapter I of the Code of Federal 

Regulations sets forth the following. 

PART 50—NATIONAL PRIMARY AND 

SECONDARY AMBIENT AIR QUALITY 

STANDARDS 

■ 1. The authority citation for part 50 

continues to read as follows: 

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

■ 2. Appendix G to part 50 is revised to 

read as follows: 

Appendix G to Part 50—Reference 

Method for the Determination of Lead 

in Total Suspended Particulate Matter 

1.0 Scope and Applicability 

Based on review of the air quality criteria 

and national ambient air quality standard 

(NAAQS) for lead (Pb) completed in 2008, 

the EPA made revisions to the primary and 

secondary NAAQS for Pb to protect public 

health and welfare. The EPA revised the level 

from 1.5 mg/m3 to 0.15 mg/m3 while retaining 

the current indicator of Pb in total suspended 

particulate matter (Pb-TSP). 

Pb-TSP is collected for 24 hours on a TSP 

filter as described in Appendix B of part 50, 

the Reference Method for the Determination 

of Suspended Particulate Matter in the 

Atmosphere (High-Volume Method). This 

method is for the analysis of Pb from TSP 

filters by Inductively Coupled Plasma Mass 

Spectrometry (ICP–MS) using a heated 

ultrasonic bath with nitric acid (HNO3) and 

hydrochloric acid (HCl) or a heated block 

(hot block) digester with HNO3 for filter 

extraction. 

This method is based on the EPA’s Office 

of Solid Waste (SW–846) Method 6020A— 

Inductively Coupled Plasma Mass 

Spectrometry (U.S. EPA, 2007). Wording in 

certain sections of this method is 

paraphrased or taken directly from Method 

6020A. 

1.1 ICP–MS is applicable for the sub-mg/ 

mL (ppb) determination of Pb in a wide 

variety of matrices. Results reported for 

monitoring or compliance purposes are 

calculated in mg/m3 at local conditions (LC). 

This procedure describes a method for the 

acid extraction of Pb in particulate matter 

collected on glass fiber, quartz, or PTFE 

filters and measurement of the extracted Pb 

using ICP–MS. 

1.2 Due to variations in the isotopic 

abundance of Pb, the value for total Pb must 

be based on the sum of the signal intensities 

for isotopic masses, 206, 207, and 208. Most 

instrument software packages are able to sum 

the primary isotope signal intensities 

automatically. 

1.3 ICP–MS requires the use of an 

internal standard. 115In (Indium), 165Ho 

(Holmium), and 209Bi (Bismuth) are 

recommended internal standards for the 

determination of Pb. 

1.4 Use of this method is restricted to use 

by, or under supervision of, properly trained 

and experienced laboratory personnel. 

Requirements include training and 

experience in inorganic sample preparation, 

including acid extraction, and also 

knowledge in the recognition and in the 

correction of spectral, chemical and physical 

interference in ICP–MS. 

2.0 Summary of Method 

2.1 This method describes the acid 

extraction of Pb in particulate matter 

collected on glass fiber, quartz, or PTFE 

ambient air filters with subsequent 

measurement of Pb by ICP–MS. Estimates of 

the Method Detection Limit (MDL) or 

sensitivity of the method are provided in 

Tables 1, 3 and 5 and determined using Pbspiked filters or filter strips analyzed in 

accordance with the guidance provided in 40 

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CFR 136, Appendix B—Determination and 

procedures for the Determination of the 

Method Detection Limit—Revision 1.1. The 

analytical range of the method is 0.00024 mg/ 

m3 to 0.60 mg/m3, and based on the low and 

high calibration curve standards and a 

nominal filter sample volume of 2000 m3. 

2.2 This method includes two extraction 

methods. In the first method, a solution of 

HNO3 and HCl is added to the filters or filter 

strips in plastic digestion tubes and the tubes 

are placed in a heated ultrasonic bath for one 

hour to facilitate the extraction of Pb. 

Following ultrasonication, the samples are 

brought to a final volume of 40 mL (50 mL 

for PTFE filters), vortex mixed or shaken 

vigorously, and centrifuged prior to aliquots 

being taken for ICP–MS analysis. In the 

second method, a solution of dilute HNO3 is 

added to the filter strips in plastic digestion 

tubes and the tubes placed into the hot block 

digester. The filter strip is completely 

covered by the solution. The tubes are 

covered with polypropylene watch glasses 

and refluxed. After reflux, the samples are 

diluted to a final volume of 50 mL with 

reagent water and mixed before analysis. 

2.3 Calibration standards and check 

standards are prepared to matrix match the 

acid composition of the samples. ICP–MS 

analysis is then performed. With this 

method, the samples are first aspirated and 

the aerosol thus created is transported by a 

flow of argon gas into the plasma torch. The 

ions produced (e.g., Pb+1) in the plasma are 

extracted via a differentially-pumped 

vacuum interface and are separated on the 

basis of their mass-to-charge ratio. The ions 

are quantified by a channel electron 

multiplier or a Faraday detector and the 

signal collected is processed by the 

instrument’s software. Interferences must be 

assessed and corrected for, if present. 

3.0 Definitions 

Pb—Elemental or ionic lead 

HNO3—Nitric acid 

HCl—Hydrochloric acid 

ICP–MS—Inductively Coupled Plasma Mass 

Spectrometer 

MDL—Method detection limit 

RSD—Relative standard deviation 

RPD—Relative percent difference 

CB—Calibration Blank 

CAL—Calibration Standard 

ICB—Initial calibration blank 

CCB—Continuing calibration blank 

ICV—Initial calibration verification 

CCV—Continuing calibration verification 

LLCV—Lower Level Calibration Verification, 

serves as the lower level ICV and lower 

level CCV 

RB—Reagent blank 

RBS—Reagent blank spike 

MSDS—Material Safety Data Sheet 

NIST—National Institute of Standards and 

Technology 

D.I. water—Deionized water 

SRM—NIST Standard Reference Material 

CRM—Certified Reference Material 

EPA—Environmental Protection Agency 

v/v—Volume to volume ratio 

4.0 Interferences 

4.1 Reagents, glassware, plasticware, and 

other sample processing hardware may yield 

artifacts and/or interferences to sample 

analysis. If reagent blanks, filter blanks, or 

quality control blanks yield results above the 

detection limit, the source of contamination 

must be identified. All containers and 

reagents used in the processing of the 

samples must be checked for contamination 

prior to sample extraction and analysis. 

Reagents shall be diluted to match the final 

concentration of the extracts and analyzed for 

Pb. Labware shall be rinsed with dilute acid 

solution and the solution analyzed. Once a 

reagent or labware article (such as extraction 

tubes) from a manufacturer has been 

successfully screened, additional screening is 

not required unless contamination is 

suspected. 

4.2 Isobaric elemental interferences in 

ICP–MS are caused by isotopes of different 

elements forming atomic ions with the same 

nominal mass-to-charge ratio (m/z) as the 

species of interest. There are no species 

found in ambient air that will result in 

isobaric interference with the three Pb 

isotopes (206, 207, and 208) being measured. 

Polyatomic interferences occur when two or 

more elements combine to form an ion with 

the same mass-to-charge ratio as the isotope 

being measured. Pb is not subject to 

interference from common polyatomic ions 

and no correction is required. 

4.3 The distribution of Pb isotopes is not 

constant. The analysis of total Pb should be 

based on the summation of signal intensities 

for the isotopic masses 206, 207, and 208. In 

most cases, the instrument software can 

perform the summation automatically. 

4.4 Physical interferences are associated 

with the sample nebulization and transport 

processes as well as with ion-transmission 

efficiencies. Dissolved solids can deposit on 

the nebulizer tip of a pneumatic nebulizer 

and on the interface skimmers of the ICP– 

MS. Nebulization and transport processes 

can be affected if a matrix component causes 

a change in surface tension or viscosity. 

Changes in matrix composition can cause 

significant signal suppression or 

enhancement. These interferences are 

compensated for by use of internal standards. 

Sample dilution will reduce the effects of 

high levels of dissolved salts, but calibration 

standards must be prepared in the extraction 

medium and diluted accordingly. 

4.5 Memory interferences are related to 

sample transport and result when there is 

carryover from one sample to the next. 

Sample carryover can result from sample 

deposition on the sample and skimmer cones 

and from incomplete rinsing of the sample 

solution from the plasma torch and the spray 

chamber between samples. These memory 

effects are dependent upon both the analyte 

being measured and sample matrix and can 

be minimized through the use of suitable 

rinse times. 

5.0 Health and Safety Cautions 

5.1 The toxicity or carcinogenicity of 

reagents used in this method has not been 

fully established. Each chemical should be 

regarded as a potential health hazard and 

exposure to these compounds should be as 

low as reasonably achievable. Each 

laboratory is responsible for maintaining a 

current file of OSHA regulations regarding 

the safe handling of the chemicals specified 

in this method. A reference file of material 

safety data sheets (MSDSs) should be 

available to all personnel involved in the 

chemical analysis. Specifically, concentrated 

HNO3 presents various hazards and is 

moderately toxic and extremely irritating to 

skin and mucus membranes. Use this reagent 

in a fume hood whenever possible and if eye 

or skin contact occurs, flush with large 

volumes of water. Always wear safety glasses 

or a shield for eye protection, protective 

clothing, and observe proper mixing when 

working with these reagents. 

5.2 Concentrated HNO3 and HCl are 

moderately toxic and extremely irritating to 

the skin. Use these reagents in a fume hood, 

and if eye and skin contact occurs, flush with 

large volumes of water. Always wear safety 

glasses or a shield for eye protection when 

working with these reagents. The component 

of this procedure requiring the greatest care 

is HNO3. HNO3 is a strong, corrosive, 

oxidizing agent that requires protection of the 

eyes, skin, and clothing. Items to be worn 

during use of this reagent include: 

1. Safety goggles (or safety glasses with 

side shields), 

2. Acid resistant rubber gloves, and 

3. A protective garment such as a 

laboratory apron. HNO3 spilled on clothing 

will destroy the fabric; contact with the skin 

underneath will result in a burn. 

It is also essential that an eye wash 

fountain or eye wash bottle be available 

during performance of this method. An eye 

wash bottle has a spout that covers the eye. 

If acid or any other corrosive gets into the 

eye, the water in this bottle is squirted onto 

the eye to wash out the harmful material. Eye 

washing should be performed with large 

amounts of water immediately after 

exposure. Medical help should be sought 

immediately after washing. If either acid, but 

especially HNO3, is spilled onto the skin, 

wash immediately with large amounts of 

water. Medical attention is not required 

unless the burn appears to be significant. 

Even after washing and drying, HNO3 may 

leave the skin slightly brown in color; this 

will heal and fade with time. 

5.3 Pb salts and Pb solutions are toxic. 

Great care must be taken to ensure that 

samples and standards are handled properly; 

wash hands thoroughly after handling. 

5.4 Care must be taken when using the 

ultrasonic bath and hot block digester as they 

are capable of causing mild burns. Users 

should refer to the safety guidance provided 

by the manufacturer of their specific 

equipment. 

5.5 Analytical plasma sources emit radio 

frequency radiation in addition to intense 

ultra violet (UV) radiation. Suitable 

precautions should be taken to protect 

personnel from such hazards. The 

inductively coupled plasma should only be 

viewed with proper eye protection from UV 

emissions. 

6.0 Equipment 

6.1 Thermo Scientific X-Series ICP–MS or 

equivalent. The system must be capable of 

providing resolution better or equal to 1.0 

atomic mass unit (amu) at 10 percent peak 

height. The system must have a mass range 

from at least 7 to 240 amu that allows for the 

application of the internal standard 

technique. For the measurement of Pb, an 

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5Certificates of Analysis for these SRMs can be 

found at: http://www.nist.gov/srm/index.cfm. 

instrument with a collision or reaction cell is 

not required. 

6.2 Ultrasonic Extraction Equipment 

6.2.1 Heated ultrasonic bath capable of 

maintaining a temperature of 80 °C; VWR 

Model 750HT, 240W, or equivalent. 

Ultrasonic bath must meet the following 

performance criteria: 

1. Cut a strip of aluminum foil almost the 

width of the tank and double the depth. 

2. Turn the ultrasonic bath on and lower 

the foil into the bath vertically until almost 

touching the bottom of the tank and hold for 

10 seconds. 

3. Remove the foil from the tank and 

observe the distribution of perforations and 

small pin prick holes. The indentations 

should be fine and evenly distributed. The 

even distribution of indentations indicates 

the ultrasonic bath is acceptable for use. 

6.2.2 Laboratory centrifuge, Beckman GS– 

6, or equivalent. 

6.2.3 Vortex mixer, VWR Signature 

Digital Vortex Mixer, VWR Catalog No. 

14005–824, or equivalent. 

6.3 Hot block extraction equipment 

6.3.1 Hot block digester, SCP Science 

DigiPrep Model MS, No. 010–500–205 block 

digester capable of maintaining a temperature 

of 95 °C, or equivalent. 

6.4 Materials and Supplies 

• Argon gas supply, 99.99 percent purity 

or better. National Welders Microbulk, or 

equivalent. 

• Plastic digestion tubes with threaded 

caps for extraction and storage, SCP Science 

DigiTUBE® Item No. 010–500–063, or 

equivalent. 

• Disposable polypropylene ribbed watch 

glasses (for heated block extraction), SCP 

Science Item No. 010–500–081, or 

equivalent. 

• Pipette, Rainin EDP2, 100 mL, ± 1 percent 

accuracy, ≤1 percent RSD (precision), with 

disposable tips, or equivalent. 

• Pipette, Rainin EDP2, 1000 mL, ± 1 

percent accuracy, ≤1 percent RSD (precision), 

with disposable tips, or equivalent. 

• Pipette, Rainin EDP2, 1–10 mL, ± 1 

percent accuracy, ≤1 percent RSD (precision), 

with disposable tips, or equivalent. 

• Pipette, Thermo Lab Systems, 5 mL, ± 1 

percent accuracy, ≤1 percent RSD (precision), 

with disposable tips, or equivalent. 

• Plastic tweezer, VWR Catalog No. 89026– 

420, or equivalent. 

• Laboratory marker. 

• Ceramic knife, Kyocera LK–25, and nonmetal ruler or other suitable cutting tools for 

making straight cuts for accurately measured 

strips. 

• Blank labels or labeling tape, VWR 

Catalog No. 36425–045, or equivalent. 

• Graduated cylinder, 1 L, VWR 89000– 

260, or equivalent. 

• Volumetric flask, Class A, 1 L, VWR 

Catalog No. 89025–778, or equivalent. 

• Millipore Element deionized water 

system, or equivalent, capable of generating 

water with a resistivity of ≥17.9 MW-cm). 

• Disposable syringes, 10-mL, with 0.45 

micron filters (must be Pb-free). 

• Plastic or PTFE wash bottles. 

• Glassware, Class A—volumetric flasks, 

pipettes, and graduated cylinders. 

• Glass fiber, quartz, or PTFE filters from 

the same filter manufacturer and lot used for 

sample collection for use in the 

determination of the MDL and for laboratory 

blanks. 

7.0 Reagents and Standards 

7.1 Reagent—or trace metals-grade 

chemicals must be used in all tests. Unless 

otherwise indicated, it is intended that all 

reagents conform to the specifications of the 

Committee on Analytical Reagents of the 

American Chemical Society, where such 

specifications are available. 

7.2 Concentrated nitric acid, 67–70 

percent, SCP Science Catalog No. 250–037– 

177, or equivalent. 

7.3 Concentrated hydrochloric acid (for 

the ultrasonic extraction method), 33–36 

percent, SCP Science Catalog No. 250–037– 

175, or equivalent. 

7.4 Deionized water—All references to 

deionized water in the method refer to 

deionized water with a resistivity ≥17.9 MWcm. 

7.5 Standard stock solutions may be 

commercially purchased for each element or 

as a multi-element mix. Internal standards 

may be purchased as a mixed multi-element 

solution. The manufacturer’s expiration date 

and storage conditions must be adhered to. 

7.5.1 Lead standard, 1000 mg/mL, NIST 

traceable, commercially available with 

certificate of analysis. High Purity Standards 

Catalog No. 100028–1, or equivalent. 

7.5.2 Indium (In) standard, 1000 mg/mL, 

NIST traceable, commercially available with 

certificate of analysis. High Purity Standards 

Catalog No. 100024–1, or equivalent. 

7.5.3 Bismuth (Bi) standard, 1000 mg/mL, 

NIST traceable, commercially available with 

certificate of analysis. High Purity Standards 

Catalog No. 100006–1, or equivalent. 

7.5.4 Holmium (Ho) standard, 1000 mg/ 

mL, NIST traceable, commercially available 

with certificate of analysis. High Purity 

Standards Catalog No. 100023–1, or 

equivalent. 

7.5.5 Second source lead standard, 1000 

mg/mL, NIST traceable, commercially 

available with certificate of analysis. Must be 

from a different vendor or lot than the 

standard described in 7.5.1. Inorganic 

Ventures Catalog No. CGPB–1, or equivalent. 

7.5.6 Standard Reference Materials, NIST 

SRM 2583, 2586, 2587 or 1648, or 

equivalent.5

Note: The In, Bi, and Ho internal standards 

may also be purchased as 10 mg/mL 

standards. Calibration standards are prepared 

by diluting stock standards to the appropriate 

levels in the same acid concentrations as in 

the final sample volume. The typical range 

for calibration standards is 0.001 to 2.00 mg/ 

mL. At a minimum, the curve must contain 

a blank and five Pb containing calibration 

standards. The calibration standards are 

stored at ambient laboratory temperature. 

Calibration standards must be prepared 

weekly and verified against a freshly 

prepared ICV using a NIST-traceable source 

different from the calibration standards. 

7.6 Internal standards may be added to 

the test solution or by on-line addition. The 

nominal concentration for an internal 

standard is 0.010 mg/mL (10 ppb). Bismuth 

(Bi) or holmium (Ho) are the preferred 

internal standards for Pb, but indium (In) 

may be used in the event the sample contains 

Bi and high recoveries are observed. 

7.7 Three laboratory blank solutions are 

required for analysis: (1) The calibration 

blank is used in the construction of the 

calibration curve and as a periodic check of 

system cleanliness (ICB and CCB); (2) the 

reagent blank (RB) is carried through the 

extraction process to assess possible 

contamination; and (3) the rinse blank is run 

between samples to clean the sample 

introduction system. If RBs or laboratory 

blanks yield results above the detection limit, 

the source of contamination must be 

identified. Screening of labware and reagents 

is addressed in Section 4.1. 

7.7.1 The calibration blank is prepared in 

the same acid matrix as the calibration 

standards and samples and contains all 

internal standards used in the analysis. 

7.7.2 The RB contains all reagents used in 

the extraction and is carried through the 

extraction procedure at the same time as the 

samples. 

7.7.3 The rinse blank is a solution of 1 to 

2 percent HNO3 (v/v) in reagent grade water. 

A sufficient volume should be prepared to 

flush the system between all standards and 

samples analyzed. 

7.7.4 The EPA currently provides glass 

fiber, quartz, and PTFE filters to air 

monitoring agencies as requested annually. 

As part of the procurement process, these 

filters are tested for acceptance by the EPA. 

The current acceptance criteria for glass fiber 

and quartz filters is 15 mg per filter or 0.0075 

mg/m3 using a nominal sample volume of 

2000 m3 and 4.8 ng/cm2 or 0.0024 mg/m3 for 

PTFE filters using a nominal sample volume 

of 24 m3. Acceptance test results for filters 

obtained by the EPA are typically well below 

the criterion specified and also below the 

recently revised Pb method performance 

detection limit of 0.0075 mg/m3; therefore, 

blank subtraction should not be performed. 

7.7.5 If filters are not provided by the 

EPA for sample collection and analysis, filter 

lot blanks should be analyzed for Pb content. 

For large filter lots (≤500 filters), randomly 

select 20 to 30 filters from the lot and analyze 

the filter or filter strips for Pb. For smaller 

filter lots, a lesser number of filters can be 

analyzed. Glass, quartz and PTFE filters must 

not have levels of Pb above the criteria 

specified in section 7.7.4 and, therefore, 

blank correction should not be performed. If 

acceptance testing shows levels of Pb above 

the criteria in Section 7.7.4, corrective action 

must be taken to reduce the levels before 

proceeding. 

7.8 The Initial Calibration Verification 

(ICV), Lower Level Calibration Verification 

(LLCV), and Continuing Calibration 

Verification (CCV) solutions are prepared 

from a different Pb source than the 

calibration curve standards and at a 

concentration that is either at or below the 

midpoint on the calibration curve, but within 

the calibration range. Both are prepared in 

the same acid matrix as the calibration 

standards. Note that the same solution may 

be used for both the ICV and CCV. The ICV/ 

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CCV and LLCV solutions must be prepared 

fresh daily. 

7.9 Tuning Solution. Prepare a tuning 

solution according to the instrument 

manufacturer’s recommendations. This 

solution will be used to verify the mass 

calibration and resolution of the instrument. 

8.0 Quality Control (QC) 

8.1 Standard QC practices shall be 

employed to assess the validity of the data 

generated, including: MDL, RB, duplicate 

samples, spiked samples, serial dilutions, 

ICV, CCV, LLCV, ICB, CCB, and SRMs/CRMs. 

8.2 MDLs must be calculated in 

accordance with 40 CFR part 136, Appendix 

B. RBs with low-level standard spikes are 

used to estimate the MDL. The low-level 

standard spike is added to at least 7 

individual filter strips and then carried 

through the entire extraction procedure. This 

will result in at least 7 individual samples to 

be used for the MDL. The recommended 

range for spiking the strips is 1 to 5 times the 

estimated MDL. 

8.3 For each batch of samples, one RB 

and one reagent blank spike (RBS) that is 

spiked at the same level as the sample spike 

(see Section 8.6) must be prepared and 

carried throughout the entire process. The 

results of the RB must be below 0.001 mg/mL. 

The recovery for the RBS must be within ± 

20 percent of the expected value. If the RB 

yields a result above 0.001 mg/mL, the source 

of contamination must be identified and the 

extraction and analysis repeated. Reagents 

and labware must be suspected as sources of 

contamination. Screening of reagents and 

labware is addressed in Section 4.1. 

8.4 Any samples that exceed the highest 

calibration standard must be diluted and 

rerun so that the concentration falls within 

the curve. The minimum dilution will be 1 

to 5 with matrix matched acid solution. 

8.5 The internal standard response must 

be monitored during the analysis. If the 

internal standard response falls below 70 

percent or rises above 120 percent of 

expected due to possible matrix effects, the 

sample must be diluted and reanalyzed. The 

minimum dilution will be 1 to 5 with matrix 

matched acid solution. If the first dilution 

does not correct the problem, additional 

dilutions must be run until the internal 

standard falls within the specified range. 

8.6 For every batch of samples prepared, 

there must be one duplicate and one spike 

sample prepared. The spike added is to be at 

a level that falls within the calibration curve, 

normally the midpoint of the curve. The 

initial plus duplicate sample must yield a 

relative percent difference ≤ 20 percent. The 

spike must be within ± 20 percent of the 

expected value. 

8.7 For each batch of samples, one extract 

must be diluted five-fold and analyzed. The 

corrected dilution result must be within ±10 

percent of the undiluted result. The sample 

chosen for the serial dilution shall have a 

concentration at or above 10X the lowest 

standard in the curve to ensure the diluted 

value falls within the curve. If the serial 

dilution fails, chemical or physical 

interference should be suspected. 

8.8 ICB, ICV, LLCV, CCB and CCV 

samples are to be run as shown in the 

following table. 

Sample Frequency Performance specification 

ICB .................... Prior to first sample .................................................................. Less than 0.001 μg/mL. 

ICV .................... Prior to first sample .................................................................. Within 90 to 110 percent of the expected value. 

LLCV ................. Daily, before first sample and after last sample ...................... ±10 percent of the expected value. 

CCB ................... After every 10 extracted samples ............................................ Less than 0.001 μg/mL. 

CCV ................... After every 10 extracted samples ............................................ Within 90–110 percent of the expected value. 

If any of these QC samples fails to meet 

specifications, the source of the unacceptable 

performance must be determined, the 

problem corrected, and any samples not 

bracketed by passing QC samples must be 

reanalyzed. 

8.9 For each batch of samples, one 

certified reference material (CRM) must be 

combined with a blank filter strip and carried 

through the entire extraction procedure. The 

result must be within ±10 percent of the 

expected value. 

8.10 For each run, a LLCV must be 

analyzed. The LLCV must be prepared at a 

concentration not more than three times the 

lowest calibration standard and at a 

concentration not used in the calibration 

curve. The LLCV is used to assess 

performance at the low end of the curve. If 

the LLCV fails (±10 percent of the expected 

value) the run must be terminated, the 

problem corrected, the instrument 

recalibrated, and the analysis repeated. 

8.11 Pipettes used for volumetric transfer 

must have the calibration checked at least 

once every 6 months and pass ± 1 percent 

accuracy and ≤ 1 percent RSD (precision) 

based on five replicate readings. The pipettes 

must be checked weekly for accuracy with a 

single replicate. Any pipette that does not 

meet ± 1 percent accuracy on the weekly 

check must be removed from service, 

repaired, and pass a full calibration check 

before use. 

8.12 Samples with physical deformities 

are not quantitatively analyzable. The analyst 

should visually check filters prior to 

proceeding with preparation for holes, tears, 

or non-uniform deposit which would prevent 

representative sampling. Document any 

deformities and qualify the data with flags 

appropriately. Care must be taken to protect 

filters from contamination. Filters must be 

kept covered prior to sample preparation. 

9.0 ICP MS Calibration 

Follow the instrument manufacturer’s 

instructions for the routine maintenance, 

cleaning, and ignition procedures for the 

specific ICP–MS instrument being used. 

9.1 Ignite the plasma and wait for at least 

one half hour for the instrument to warm up 

before beginning any pre-analysis steps. 

9.2 For the Thermo X-Series with Xt 

cones, aspirate a 10 ng/mL tuning solution 

containing In, Bi, and Ce (Cerium). Monitor 

the intensities of In, Bi, Ce, and CeO (Cerium 

oxide) and adjust the instrument settings to 

achieve the highest In and Bi counts while 

minimizing the CeO/Ce oxide ratio. For other 

instruments, follow the manufacturer’s 

recommended practice. Tune to meet the 

instrument manufacturer’s specifications. 

After tuning, place the sample aspiration 

probe into a 2 percent HNO3 rinse solution 

for at least 5 minutes to flush the system. 

9.3 Aspirate a 5 ng/mL solution 

containing Co, In, and Bi to perform a daily 

instrument stability check. Run 10 replicates 

of the solution. The percent RSD for the 

replicates must be less than 3 percent at all 

masses. If the percent RSD is greater than 3 

percent, the sample introduction system, 

pump tubing, and tune should be examined, 

and the analysis repeated. Place the sample 

aspiration probe into a 2 percent HNO3 rinse 

solution for at least 5 minutes to flush the 

system. 

9.4 Load the calibration standards in the 

autosampler and analyze using the same 

method parameters that will be used to 

analyze samples. The curve must include one 

blank and at least 5 Pb-containing calibration 

standards. The correlation coefficient must 

be at least 0.998 for the curve to be accepted. 

The lowest standard must recover ± 15 

percent of the expected value and the 

remaining standards must recover ± 10 

percent of the expected value to be accepted. 

9.5 Immediately after the calibration 

curve is completed, analyze an ICV and an 

ICB. The ICV must be prepared from a 

different source of Pb than the calibration 

standards. The ICV must recover 90–110 

percent of the expected value for the run to 

continue. The ICB must be less than 0.001 

mg/mL. If either the ICV or the ICB fails, the 

run must be terminated, the problem 

identified and corrected, and the analysis restarted. 

9.6 A LLCV, CCV and a CCB must be run 

after the ICV and ICB. A CCV and CCB must 

be run at a frequency of not less than every 

10 extracted samples. A typical analytical 

run sequence would be: Calibration blank, 

Calibration standards, ICV, ICB, LLCV, CCV, 

CCB, Extracts 1–10, CCV, CCB, Extracts 11– 

20, CCV, CCB, Extracts 21–30, CCV, CCB, 

LLCV, CCV, CCB. Extracts are any field 

sample or QC samples that have been carried 

through the extraction process. The CCV 

solution is prepared from a different source 

than the calibration standards and may be the 

same as the ICV solution. The LLCV must be 

within ± 10 percent of expected value. The 

CCV value must be within ± 10 percent of 

expected for the run to continue. The CCB 

must be less than 0.001 mg/mL. If either the 

CCV, LLCV, or CCB fails, the run must be 

terminated, the problem identified and 

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corrected, and the analysis re-started from 

the last passing CCV/LLCV/CCB set. 

9.7 A LLCV, CCV, and CCB set must be 

run at the end of the analysis. The LLCV 

must be within ± 30 percent of expected 

value. If either the CCV, LLCV, or CCB fails, 

the run must be terminated, the problem 

identified and corrected, and the analysis restarted from the last passing CCV/LLCV/CCB 

set. 

10.0 Heated Ultrasonic Filter Strip 

Extraction 

All plasticware (e.g., Nalgene) and 

glassware used in the extraction procedures 

is soaked in 1 percent HNO3 (v/v) for at least 

24 hours and rinsed with reagent water prior 

to use. All mechanical pipettes used must be 

calibrated to ±1 percent accuracy and ≤ 1 

percent RSD at a minimum of once every 6 

months. 

10.1 Sample Preparation—Heated 

Ultrasonic Bath 

10.1.1 Extraction solution (1.03M HNO3 + 

2.23M HCl). Prepare by adding 500 mL of 

deionized water to a 1000 mL flask, adding 

64.4 mL of concentrated HNO3 and 182 mL 

of concentrated HCl, shaking to mix, 

allowing solution to cool, diluting to volume 

with reagent water, and inverting several 

times to mix. Extraction solution must be 

prepared at least weekly. 

10.1.2 Use a ceramic knife and non-metal 

ruler, or other cutting device that will not 

contaminate the filter with Pb. Cut a 3⁄4 inch 

X 8 inch strip from the glass fiber or quartz 

filter by cutting a strip from the edge of the 

filter where it has been folded along the 10 

inch side at least 1 inch from the right or left 

side to avoid the un-sampled area covered by 

the filter holder. The filters must be carefully 

handled to avoid dislodging deposits. 

10.1.3 Using plastic tweezers, roll the 

filter strip up in a coil and place the rolled 

strip in the bottom of a labeled 50 mL 

extraction tube. In a fume hood, add 15.00 ± 

0.15 mL of the extraction solution (see 

Section 10.1.1) using a calibrated mechanical 

pipette. Ensure that the extraction solution 

completely covers the filter strip. 

10.1.4 Loosely cap the 50 mL extraction 

tube and place it upright in a plastic rack. 

When all samples have been prepared, place 

the racks in an uncovered heated ultrasonic 

water bath that has been preheated to 80 ± 

5°C and ensure that the water level in the 

ultrasonic is above the level of the extraction 

solution in the tubes but well below the level 

of the extraction tube caps to avoid 

contamination. Start the ultrasonic bath and 

allow the unit to run for 1 hour ± 5 minutes 

at 80 ± 5°C. 

10.1.5 Remove the rack(s) from the 

ultrasonic bath and allow the racks to cool. 

10.1.6 Add 25.00 ± 0.25 mL of D.I. water 

with a calibrated mechanical pipette to bring 

the sample to a final volume of 40.0 ± 0.4 mL. 

Tightly cap the tubes, and vortex mix or 

shake vigorously. Place the extraction tubes 

in an appropriate holder and centrifuge for 

20 minutes at 2500 revolutions per minute 

(RPM). 

CAUTION—Make sure that the centrifuge 

holder has a flat bottom to support the flat 

bottomed extraction tubes. 

10.1.7 Pour an aliquot of the solution into 

an autosampler vial for ICP–MS analysis to 

avoid the potential for contamination. Do not 

pipette an aliquot of solution into the 

autosampler vial. 

10.1.8 Decant the extract to a clean tube, 

cap tightly, and store the sample extract at 

ambient laboratory temperature. Extracts may 

be stored for up to 6 months from the date 

of extraction. 

10.2 47 mm PTFE Filter Extraction— 

Heated Ultrasonic Bath 

10.2.1 Extraction solution (1.03M HNO3 + 

2.23M HCl). Prepare by adding 500 mL of D.I. 

water to a 1000mL flask, adding 64.4 mL of 

concentrated HNO3 and 182 mL of 

concentrated HCl, shaking to mix, allowing 

solution to cool, diluting to volume with 

reagent water, and inverting several times to 

mix. Extraction solution must be prepared at 

least weekly. 

10.2.2 Using plastic tweezers, bend the 

PTFE filter into a U-shape and insert the 

filter into a labeled 50 mL extraction tube 

with the particle loaded side facing the 

center of the tube. Gently push the filter to 

the bottom of the extraction tube. In a fume 

hood, add 25.00 ± 0.15 mL of the extraction 

solution (see Section 10.2.1) using a 

calibrated mechanical pipette. Ensure that 

the extraction solution completely covers the 

filter. 

10.2.3 Loosely cap the 50 mL extraction 

tube and place it upright in a plastic rack. 

When all samples have been prepared, place 

the racks in an uncovered heated ultrasonic 

water bath that has been preheated to 80 ± 

5°C and ensure that the water level in the 

ultrasonic is above the level of the extraction 

solution in the tubes, but well below the 

level of the extraction tube caps to avoid 

contamination. Start the ultrasonic bath and 

allow the unit to run for 1 hour ± 5 minutes 

at 80 ± 5°C. 

10.2.4 Remove the rack(s) from the 

ultrasonic bath and allow the racks to cool. 

10.2.5 Add 25.00 ± 0.25 mL of D.I. water 

with a calibrated mechanical pipette to bring 

the sample to a final volume of 50.0 ± 0.4 mL. 

Tightly cap the tubes, and vortex mix or 

shake vigorously. Allow samples to stand for 

one hour to allow complete diffusion of the 

extracted Pb. The sample is now ready for 

analysis. 

Note: Although PTFE filters have only been 

extracted using the ultrasonic extraction 

procedure in the development of this FRM, 

PTFE filters are inert and have very low Pb 

content. No issues are expected with the 

extraction of PTFE filters using the heated 

block digestion method. However, prior to 

using PTFE filters in the heated block 

extraction method, extraction method 

performance test using CRMs must be done 

to confirm performance (see Section 8.9). 

11.0 Hot Block Filter Strip Extraction 

All plasticware (e.g., Nalgene) and 

glassware used in the extraction procedures 

is soaked in 1 percent HNO3 for at least 24 

hours and rinsed with reagent water prior to 

use. All mechanical pipettes used must be 

calibrated to ±1 percent accuracy and ≤ 1 

percent RSD at a minimum of once every 6 

months. 

11.1 Sample Preparation—Hot Block 

Digestion 

11.1.1 Extraction solution (1:19, v/v 

HNO3). Prepare by adding 500 mL of D.I. 

water to a 1000 mL flask, adding 50 mL of 

concentrated HNO3, shaking to mix, allowing 

solution to cool, diluting to volume with 

reagent water, and inverting several times to 

mix. The extraction solution must be 

prepared at least weekly. 

11.1.2 Use a ceramic knife and non-metal 

ruler, or other cutting device that will not 

contaminate the filter with Pb. Cut a 1-inch 

X 8-inch strip from the glass fiber or quartz 

filter. Cut a strip from the edge of the filter 

where it has been folded along the 10-inch 

side at least 1 inch from the right or left side 

to avoid the un-sampled area covered by the 

filter holder. The filters must be carefully 

handled to avoid dislodging particle 

deposits. 

11.1.3 Using plastic tweezers, roll the 

filter strip up in a coil and place the rolled 

strip in the bottom of a labeled 50 mL 

extraction tube. In a fume hood, add 20.0 ± 

0.15 mL of the extraction solution (see 

Section 11.1.1) using a calibrated mechanical 

pipette. Ensure that the extraction solution 

completely covers the filter strip. 

11.1.4 Place the extraction tube in the 

heated block digester and cover with a 

disposable polyethylene ribbed watch glass. 

Heat at 95 ± 5°C for 1 hour and ensure that 

the sample does not evaporate to dryness. For 

proper heating, adjust the temperature 

control of the hot block such that an 

uncovered vessel containing 50 mL of water 

placed in the center of the hot block can be 

maintained at a temperature approximately, 

but no higher than 85ßC. Once the vessel is 

covered with a ribbed watch glass, the 

temperature of the water will increase to 

approximately 95°C. 

11.1.5 Remove the rack(s) from the heated 

block digester and allow the samples to cool. 

11.1.6 Bring the samples to a final 

volume of 50 mL with D.I. water. Tightly cap 

the tubes, and vortex mix or shake vigorously 

for at least 5 seconds. Set aside (with the 

filter strip in the tube) for at least 30 minutes 

to allow the HNO3 trapped in the filter to 

diffuse into the extraction solution. 

11.1.7 Shake thoroughly (with the filter 

strip in the digestion tube) and let settle for 

at least one hour. The sample is now ready 

for analysis. 

12.0 Measurement Procedure 

12.1 Follow the instrument 

manufacturer’s startup procedures for the 

ICP–MS. 

12.2 Set instrument parameters to the 

appropriate operating conditions as 

presented in the instrument manufacturer’s 

operating manual and allow the instrument 

to warm up for at least 30 minutes. 

12.3 Calibrate the instrument per Section 

9.0 of this method. 

12.4 Verify the instrument is suitable for 

analysis as defined in Sections 9.2 and 9.3. 

12.5 As directed in Section 8.0 of this 

method, analyze an ICV and ICB immediately 

after the calibration curve followed by a 

LLCV, then CCV and CCB. The acceptance 

requirements for these parameters are 

presented in Section 8.8. 

12.6 Analyze a CCV and a CCB after every 

10 extracted samples. 

12.7 Analyze a LLCV, CCV and CCB at the 

end of the analysis. 

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12.8 A typical sample run will include 

field samples, field sample duplicates, spiked 

field sample extracts, serially diluted 

samples, the set of QC samples listed in 

Section 8.8 above, and one or more CRMs or 

SRMs. 

12.9 Any samples that exceed the highest 

standard in the calibration curve must be 

diluted and reanalyzed so that the diluted 

concentration falls within the calibration 

curve. 

13.0 Results 

13.1 The filter results must be initially 

reported in mg/mL as analyzed. Any 

additional dilutions must be accounted for. 

The internal standard recoveries must be 

included in the result calculation; this is 

done by the ICP–MS software for most 

commercially-available instruments. Final 

results should be reported in mg Pb/m3 to 

three significant figures as follows: 

C = ((mg Pb/mL * Vf * A)* D))/Vs 

Where: 

C = Concentration, mg Pb/m3

mg Pb/mL = Lead concentration in solution 

Vf = Total extraction solution volume 

A = Area correction; 3⁄4′′ × 8’’ strip = 5.25 in2

analyzed, A = 12.0 or 1’’ × 8′′ strip = 7 

in2 analyzed, A = 9.0 

D = dilution factor (if required) 

Vs = Actual volume of air sampled 

The calculation assumes the use of a 

standard 8-inch × 10-inch TSP filter which 

has a sampled area of 9-inch × 7-inch (63.0 

in2) due to the 1⁄2-inch filter holder border 

around the outer edge. The 3⁄4-inch × 8-inch 

strip has a sampled area of 3⁄4-inch × 7-inch 

(5.25 in2). The 1-inch × 8-inch strip has a 

sampled area of 1-inch × 7-inch (7.0 in2). If 

filter lot blanks are provided for analysis, 

refer to Section 7.7.5 of this method for 

guidance on testing. 

14.0 Method Performance 

Information in this section is an example 

of typical performance results achieved by 

this method. Actual performance must be 

demonstrated by each individual laboratory 

and instrument. 

14.1 Performance data have been collected 

to estimate MDLs for this method. MDLs 

were determined in accordance with 40 CFR 

136, Appendix B. MDLs were estimated for 

glass fiber, quartz, and PTFE filters using 

seven reagent/filter blank solutions spiked 

with low level Pb at three times the estimated 

MDL of 0.001 mg/mL. Tables 1, 3, and 5 

shows the MDLs estimated using both the 

ultrasonic and hot block extraction methods 

for glass fiber and quartz filters and the 

ultrasonic method for PTFE filters. The MDLs 

are well below the EPA requirement of five 

percent of the current Pb NAAQS or 0.0075 

mg/m3. These MDLs are provided to 

demonstrate the adequacy of the method’s 

performance for Pb in TSP. Each laboratory 

using this method should determine MDLs in 

their laboratory and verify them annually. It 

is recommended that laboratories also 

perform the optional iterative procedure in 

40 CFR 136, Appendix B to verify the 

reasonableness of the estimated MDL and 

subsequent MDL determinations. 

14.2 Extraction method recovery tests 

with glass fiber and quartz filter strips, and 

PTFE filters spiked with NIST SRMs were 

performed using the ultrasonic/HNO3 and 

HCl filter extraction methods and 

measurement of the dissolved Pb with ICP– 

MS. Tables 2, 4, and 6 show recoveries 

obtained with these SRM. The recoveries for 

all SRMs were ≥90 percent at the 95 percent 

confidence level. 

TABLE 1—METHOD DETECTION LIMITS DETERMINED BY ANALYSIS OF REAGENT/GLASS FIBER FILTER BLANKS SPIKED

WITH LOW-LEVEL PB SOLUTION

Ultrasonic 

extraction 

method 

Hotblock 

extraction 

method 

μg/m3* μg/m3* 

n = 1 ................................................................................................................................................................................ 0.0000702 0.000533 

n = 2 ................................................................................................................................................................................ 0.0000715 0.000482 

n = 3 ................................................................................................................................................................................ 0.0000611 0.000509 

n = 4 ................................................................................................................................................................................ 0.0000587 0.000427 

n = 5 ................................................................................................................................................................................ 0.0000608 0.000449 

n = 6 ................................................................................................................................................................................ 0.0000607 0.000539 

n = 7 ................................................................................................................................................................................ 0.0000616 0.000481 

Average ............................................................................................................................................................................ 0.0000635 0.000489 

Standard Deviation .......................................................................................................................................................... 0.0000051 0.000042 

MDL** ............................................................................................................................................................................... 0.0000161 0.000131 

* Assumes 2000 m3 of air sampled. 

** MDL is 3.143 times the standard deviation of the results for seven sample replicates analyzed. 

TABLE 2—RECOVERIES OF LEAD FROM NIST SRMS SPIKED ONTO GLASS FIBER FILTERS

Extraction method 

Recovery, ICP–MS, (percent) 

NIST 1547 

plant NIST 2709 soil NIST 2583 dust 

NIST 2582 

paint 

Ultrasonic Bath ................................................................................................ 100 ± 4 98 ± 1 103 ± 8 101 ± 0 

Block Digestion ................................................................................................ 92 ± 7 98 ± 3 103 ± 4 94 ± 4 

TABLE 3—METHOD DETECTION LIMITS DETERMINED BY ANALYSIS OF REAGENT/QUARTZ FILTER BLANKS SPIKED WITH

LOW-LEVEL PB SOLUTION

Ultrasonic 

extraction 

method 

Hotblock 

extraction 

method 

μg/m3* μg/m3* 

n = 1 ................................................................................................................................................................................ 0.000533 0.000274 

n = 2 ................................................................................................................................................................................ 0.000552 0.000271 

n = 3 ................................................................................................................................................................................ 0.000534 0.000281 

n = 4 ................................................................................................................................................................................ 0.000684 0.000269 

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TABLE 3—METHOD DETECTION LIMITS DETERMINED BY ANALYSIS OF REAGENT/QUARTZ FILTER BLANKS SPIKED WITH

LOW-LEVEL PB SOLUTION—Continued 

Ultrasonic 

extraction 

method 

Hotblock 

extraction 

method 

μg/m3* μg/m3* 

n = 5 ................................................................................................................................................................................ 0.000532 0.000278 

n = 6 ................................................................................................................................................................................ 0.000532 0.000272 

n = 7 ................................................................................................................................................................................ 0.000552 0.000261 

Average ............................................................................................................................................................................ 0.000560 0.000272 

Standard Deviation .......................................................................................................................................................... 0.000055 0.000007 

MDL** ............................................................................................................................................................................... 0.000174 0.000021 

* Assumes 2000 m3 of air sampled. 

** MDL is 3.143 times the standard deviation of the results for seven sample replicates analyzed. 

TABLE 4—RECOVERIES OF LEAD FROM NIST SRMS SPIKED ONTO QUARTZ FIBER FILTERS

Extraction method 

Recovery, ICP–MS, (percent) 

NIST 1547 

plant NIST 2709 soil NIST 2583 dust 

NIST 2582 

paint 

Ultrasonic Bath ................................................................................................ 101 ± 6 95 ± 1 91 ± 5 93 ± 1 

Block Digestion ................................................................................................ 106 ± 3 104 ± 3 92 ± 6 95 ± 2 

TABLE 5—METHOD DETECTION LIMITS DETERMINED BY ANALYSIS OF REAGENT/PTFE FILTER BLANKS SPIKED WITH LOWLEVEL PB SOLUTION

Ultrasonic 

extraction 

method 

μg/m3* 

n = 1 .................................................................................................................................................................................................... 0.001775 

n = 2 .................................................................................................................................................................................................... 0.001812 

n = 3 .................................................................................................................................................................................................... 0.001773 

n = 4 .................................................................................................................................................................................................... 0.001792 

n = 5 .................................................................................................................................................................................................... 0.001712 

n = 6 .................................................................................................................................................................................................... 0.001767 

n = 7 .................................................................................................................................................................................................... 0.001778 

Average ................................................................................................................................................................................................ 0.001773 

Standard Deviation .............................................................................................................................................................................. 0.000031 

MDL** ................................................................................................................................................................................................... 0.000097 

* Assumes 24 m3 of air sampled. 

** MDL is 3.143 times the standard deviation of the results for seven sample replicates analyzed. 

TABLE 6—RECOVERIES OF LEAD FROM NIST SRMS SPIKED ONTO PTFE FILTERS

Extraction method 

Recovery, ICP–MS, (percent) 

NIST 1547 

plant NIST 2709 soil NIST 2583 dust 

NIST 2582 

paint 

Ultrasonic Bath ................................................................................................ 104 ± 5 93 ± 1 108 ± 11 96 ± 3 

15.0 Pollution Prevention 

15.1 Pollution prevention encompasses 

any technique that reduces or eliminates the 

quantity and/or toxicity of waste at the point 

of generation. Numerous opportunities for 

pollution prevention exist in laboratory 

operations. Whenever feasible, laboratory 

personnel should use pollution prevention 

techniques to address their waste generation. 

The sources of pollution generated with this 

procedure are waste acid extracts and Pbcontaining solutions. 

15.2 For information about pollution 

prevention that may be applicable to 

laboratories and research institutions, consult 

Less is Better: Laboratory Chemical 

Management for Waste Reduction, available 

from the American Chemical Society’s 

Department of Government Relations and 

Science Policy, 1155 16th St. NW., 

Washington, DC 20036, www.acs.org. 

16.0 Waste Management 

16.1 Laboratory waste management 

practices must be conducted consistent with 

all applicable rules and regulations. 

Laboratories are urged to protect air, water, 

and land by minimizing all releases from 

hood and bench operations, complying with 

the letter and spirit of any sewer and 

discharge permits and regulations, and by 

complying with all solid and hazardous 

waste regulation. For further information on 

waste management, consult The Waste 

Management Manual for Laboratory 

Personnel available from the American 

Chemical Society listed in Section 15.2 of 

this method. 

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16.2 Waste HNO3, HCl, and solutions 

containing these reagents and/or Pb must be 

placed in labeled bottles and delivered to a 

commercial firm that specializes in removal 

of hazardous waste. 

17.0 References 

FACDQ (2007). Report of the Federal 

Advisory Committee on Detection and 

Quantitation Approaches and Uses in 

Clean Water Act Programs, submitted to 

the U.S. EPA December 2007. Available: 

http://water.epa.gov/scitech/methods/ 

cwa/det/upload/final-report-200712.pdf. 

Rice J (2013). Results from the Development 

of a New Federal Reference Method 

(FRM) for Lead in Total Suspended 

Particulate (TSP) Matter. Docket # EPA– 

HQ–OAR–2012–0210. 

U.S. EPA (2007). Method 6020A— 

Inductively Coupled Plasma Mass 

Spectrometry. U.S. Environmental 

Protection Agency. Revision 1, February 

2007. Available: http://www.epa.gov/ 

osw/hazard/testmethods/sw846/pdfs/ 

6020a.pdf. 

U.S. EPA (2011). A Laboratory Study of 

Procedures Evaluated by the Federal 

Advisory Committee on Detection and 

Quantitation Approaches and Uses in 

Clean Water Act Programs. December 

2011. Available: http://water.epa.gov/ 

scitech/methods/cwa/det/upload/ 

fac_report_2009.pdf. 

[FR Doc. 2013–15880 Filed 7–2–13; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 52 

[EPA–R03–OAR–2013–0376]; FRL–9828–2 

Approval and Promulgation of Air 

Quality Implementation Plans; Virginia; 

Removal of Consumer and Commercial 

Products Rules 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Direct final rule. 

SUMMARY: EPA is taking direct final 

action to approve revisions to the 

Virginia State Implementation Plan 

(SIP). The revisions remove four articles 

located in chapter 9VAC5–40 (Existing 

Stationary Sources) from the Virginia 

SIP. These articles are being removed 

from the Virginia SIP because they were 

repealed in their entirety and have been 

replaced by the updated corresponding 

articles in chapter 9VAC5–45 

(Consumer and Commercial Products). 

The provisions of chapter 9VAC5–45 are 

not affected by the removal of these 

regulations. EPA is approving these 

revisions to remove the above 

mentioned articles in accordance with 

the requirements of the Clean Air Act 

(CAA). 

DATES: This rule is effective on 

September 3, 2013 without further 

notice, unless EPA receives adverse 

written comment by August 2, 2013. If 

EPA receives such comments, it will 

publish a timely withdrawal of the 

direct final rule in the Federal Register 

and inform the public that the rule will 

not take effect. 

ADDRESSES: Submit your comments, 

identified by Docket ID Number EPA– 

R03–OAR–2013–0376 by one of the 

following methods: 

A. www.regulations.gov. Follow the 

on-line instructions for submitting 

comments. 

B. Email: fernandez.cristina@epa.gov. 

C. Mail: EPA–R03–OAR–2013–0376, 

Cristina Fernandez, Associate Director, 

Office of Air Program Planning, Air 

Protection Division, Mailcode 3AP30, 

U.S. Environmental Protection Agency, 

Region III, 1650 Arch Street, 

Philadelphia, Pennsylvania 19103. 

D. Hand Delivery: At the previouslylisted EPA Region III address. 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–R03–OAR–2013– 

0376. EPA’s policy is that all comments 

received will be included in the public 

docket without change, and may be 

made available online at 

www.regulations.gov, including any 

personal information provided, unless 

the comment includes information 

claimed to be Confidential Business 

Information (CBI) or other information 

whose disclosure is restricted by statute. 

Do not submit information that you 

consider to be CBI or otherwise 

protected through www.regulations.gov 

or email. The www.regulations.gov Web 

site is an ‘‘anonymous access’’ system, 

which means EPA will not know your 

identity or contact information unless 

you provide it in the body of your 

comment. If you send an email 

comment directly to EPA without going 

through www.regulations.gov, your 

email address will be automatically 

captured and included as part of the 

comment that is placed in the public 

docket and made available on the 

Internet. If you submit an electronic 

comment, EPA recommends that you 

include your name and other contact 

information in the body of your 

comment and with any disk or CD–ROM 

you submit. If EPA cannot read your 

comment due to technical difficulties 

and cannot contact you for clarification, 

EPA may not be able to consider your 

comment. Electronic files should avoid 

the use of special characters, any form 

of encryption, and be free of any defects 

or viruses. 

Docket: All documents in the 

electronic docket are listed in the 

www.regulations.gov index. Although 

listed in the index, some information is 

not publicly available, i.e., 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 available either 

electronically in www.regulations.gov or 

in hard copy during normal business 

hours at the Air Protection Division, 

U.S. Environmental Protection Agency, 

Region III, 1650 Arch Street, 

Philadelphia, Pennsylvania 19103. 

Copies of the State submittal are 

available at the Virginia Department of 

Environmental Quality, 629 East Main 

Street, Richmond, Virginia 23219. 

FOR FURTHER INFORMATION CONTACT: 

Gregory Becoat, (215) 814–2036, or by 

email at becoat.gregory@epa.gov. 

SUPPLEMENTARY INFORMATION: 

I. Summary of SIP Revision 

On April 2, 2013, the Commonwealth 

of Virginia submitted formal revisions to 

its SIP. These revisions consist of 

removing the following articles located 

in chapter 9VAC5–40 (Existing 

Stationary Sources), part II (Emission 

Standards) from the Virginia SIP: Article 

39 (Emission Standards for Asphalt 

Paving Operations), article 42 (Emission 

Standards for Portable Fuel Container 

Spillage), article 49 (Emission Standards 

for Architectural and Industrial 

Maintenance Coatings), and article 50 

(Emission Standards for Consumer 

Products). These articles are being 

removed from the Virginia SIP because 

they were repealed in their entirety from 

Virginia’s state-enforceable air pollution 

control regulations. They have been 

replaced by corresponding articles in 

chapter 9VAC5–45 (Consumer and 

Commercial Products), part II (Emission 

Standards), articles 1, 3, 5, and 7, which 

was approved by EPA and published as 

a final rule on January 26, 2012 (See 77 

FR 3928). This rule became effective on 

February 27, 2012 and contains the 

required elements for a Federally 

enforceable rule, including emission 

limitations, compliance procedures and 

test methods, compliance dates, and 

record keeping provisions. 

II. General Information Pertaining to 

SIP Submittals From the 

Commonwealth of Virginia 

In 1995, Virginia adopted legislation 

that provides, subject to certain 

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