Method for the Determination of Lead in Total Suspended Particulate Matter, 40000-40011 [2013-15880]

Download as PDF 40000 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations Dated: June 21, 2013. M.W. Sibley, Captain, U.S. Coast Guard, Captain of the Port, Lake Michigan. List of Subjects in 33 CFR Part 165 Harbors, Marine safety, Navigation (water), Reporting and recordkeeping requirements, Security measures, Waterways. [FR Doc. 2013–16043 Filed 7–2–13; 8:45 am] BILLING CODE 9110–04–P 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 DEPARTMENT OF HOMELAND SECURITY Coast Guard 1. The authority citation for part 165 continues to read as follows: 33 CFR Part 165 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. RIN 1625–AA00 ■ 2. Add § 165.T09–0547 to read as follows: ■ WREIER-AVILES on DSK5TPTVN1PROD with RULES (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. 15:18 Jul 02, 2013 Jkt 229001 Eighth Coast Guard District Annual Safety Zones; Riverfront Independence Festival Fireworks; Ohio River 607.0– 609.0; New Albany, KY Coast Guard, DHS. Notice of enforcement of regulation. AGENCY: § 165.T09–0547 Safety Zone; Grand Haven 4th of July fireworks; Grand River, Grand Haven, MI. VerDate Mar<15>2010 [Docket No. USCG–2013–0331] ACTION: 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 SUMMARY: PO 00000 Frm 00044 Fmt 4700 Sfmt 4700 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 Environmental Protection Agency (EPA). ACTION: Final rule. AGENCY: 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 SUMMARY: E:\FR\FM\03JYR1.SGM 03JYR1 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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: https://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: WREIER-AVILES on DSK5TPTVN1PROD with RULES 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 VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 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 PO 00000 Frm 00045 Fmt 4700 Sfmt 4700 40001 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/ E:\FR\FM\03JYR1.SGM 03JYR1 WREIER-AVILES on DSK5TPTVN1PROD with RULES 40002 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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 1 CASAC’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: https://yosemite.epa.gov/ sab/sabproduct.nsf/ DA39026E54BAF46E8525781D00606633/$File/ EPA-CASAC-11-002-unsigned.pdf. VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 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 2 FEM EQL–0400–0140 (65 FR 26603, May 8, 2000). 3 The list of current FEMs is located at: https:// epa.gov/ttn/amtic/files/ambient/criteria/referenceequivalent-methods-list.pdf. PO 00000 Frm 00046 Fmt 4700 Sfmt 4700 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 4 Refer to: https://water.epa.gov/scitech/methods/ cwa/det/index.cfm for EPA’s Procedures for Detection and Quantitation. E:\FR\FM\03JYR1.SGM 03JYR1 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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. WREIER-AVILES on DSK5TPTVN1PROD with RULES 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). 15:18 Jul 02, 2013 Jkt 229001 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. 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. C. Regulatory Flexibility Act E. Executive Order 13132: Federalism 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. 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. D. Unfunded Mandates Reform Act 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. VerDate Mar<15>2010 40003 G. Executive Order 13045: Protection of Children From Environmental Health and Safety Risks B. Paperwork Reduction 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 PO 00000 Frm 00047 Fmt 4700 Sfmt 4700 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. 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. E:\FR\FM\03JYR1.SGM 03JYR1 40004 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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 WREIER-AVILES on DSK5TPTVN1PROD with RULES 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. 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. J. Executive Order 12898: Federal Actions To Address Environmental Justice in Minority Populations and Low-Income Populations PART 50—NATIONAL PRIMARY AND SECONDARY AMBIENT AIR QUALITY STANDARDS 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 ■ VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 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: ■ PO 00000 Frm 00048 Fmt 4700 Sfmt 4700 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 E:\FR\FM\03JYR1.SGM 03JYR1 WREIER-AVILES on DSK5TPTVN1PROD with RULES Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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 VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 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 PO 00000 Frm 00049 Fmt 4700 Sfmt 4700 40005 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 E:\FR\FM\03JYR1.SGM 03JYR1 40006 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations instrument with a collision or reaction cell is not required. WREIER-AVILES on DSK5TPTVN1PROD with RULES 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. VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 • 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 5 Certificates of Analysis for these SRMs can be found at: https://www.nist.gov/srm/index.cfm. PO 00000 Frm 00050 Fmt 4700 Sfmt 4700 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/ E:\FR\FM\03JYR1.SGM 03JYR1 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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 Frequency ICB .................... ICV .................... LLCV ................. CCB ................... CCV ................... WREIER-AVILES on DSK5TPTVN1PROD with RULES Sample Prior to first sample .................................................................. Prior to first sample .................................................................. Daily, before first sample and after last sample ...................... After every 10 extracted samples ............................................ After every 10 extracted samples ............................................ 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 VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 Frm 00051 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. Performance specification Less than 0.001 μg/mL. Within 90 to 110 percent of the expected value. ±10 percent of the expected value. Less than 0.001 μg/mL. Within 90–110 percent of the expected value. 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 PO 00000 40007 Fmt 4700 Sfmt 4700 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 E:\FR\FM\03JYR1.SGM 03JYR1 WREIER-AVILES on DSK5TPTVN1PROD with RULES 40008 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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 VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 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. PO 00000 Frm 00052 Fmt 4700 Sfmt 4700 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. E:\FR\FM\03JYR1.SGM 03JYR1 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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 40009 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 μg/m3* n = 1 ................................................................................................................................................................................ n = 2 ................................................................................................................................................................................ n = 3 ................................................................................................................................................................................ n = 4 ................................................................................................................................................................................ n = 5 ................................................................................................................................................................................ n = 6 ................................................................................................................................................................................ n = 7 ................................................................................................................................................................................ Average ............................................................................................................................................................................ Standard Deviation .......................................................................................................................................................... MDL** ............................................................................................................................................................................... Hotblock extraction method μg/m3* 0.0000702 0.0000715 0.0000611 0.0000587 0.0000608 0.0000607 0.0000616 0.0000635 0.0000051 0.0000161 0.000533 0.000482 0.000509 0.000427 0.000449 0.000539 0.000481 0.000489 0.000042 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 Recovery, ICP–MS, (percent) Extraction method NIST 1547 plant Ultrasonic Bath ................................................................................................ Block Digestion ................................................................................................ NIST 2709 soil 100 ± 4 92 ± 7 NIST 2583 dust 98 ± 1 98 ± 3 103 ± 8 103 ± 4 NIST 2582 paint 101 ± 0 94 ± 4 WREIER-AVILES on DSK5TPTVN1PROD with RULES TABLE 3—METHOD DETECTION LIMITS DETERMINED BY ANALYSIS OF REAGENT/QUARTZ FILTER BLANKS SPIKED WITH LOW-LEVEL PB SOLUTION Ultrasonic extraction method μg/m3* n n n n = = = = 1 2 3 4 ................................................................................................................................................................................ ................................................................................................................................................................................ ................................................................................................................................................................................ ................................................................................................................................................................................ VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 PO 00000 Frm 00053 Fmt 4700 Sfmt 4700 E:\FR\FM\03JYR1.SGM 03JYR1 Hotblock extraction method μg/m3* 0.000533 0.000552 0.000534 0.000684 0.000274 0.000271 0.000281 0.000269 40010 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations TABLE 3—METHOD DETECTION LIMITS DETERMINED BY ANALYSIS OF REAGENT/QUARTZ FILTER BLANKS SPIKED WITH LOW-LEVEL PB SOLUTION—Continued Ultrasonic extraction method μg/m3* n = 5 ................................................................................................................................................................................ n = 6 ................................................................................................................................................................................ n = 7 ................................................................................................................................................................................ Average ............................................................................................................................................................................ Standard Deviation .......................................................................................................................................................... MDL** ............................................................................................................................................................................... Hotblock extraction method μg/m3* 0.000532 0.000532 0.000552 0.000560 0.000055 0.000174 0.000278 0.000272 0.000261 0.000272 0.000007 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 Recovery, ICP–MS, (percent) Extraction method NIST 1547 plant NIST 2709 soil 101 ± 6 106 ± 3 Ultrasonic Bath ................................................................................................ Block Digestion ................................................................................................ 95 ± 1 104 ± 3 NIST 2583 dust 91 ± 5 92 ± 6 NIST 2582 paint 93 ± 1 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 .................................................................................................................................................................................................... n = 2 .................................................................................................................................................................................................... n = 3 .................................................................................................................................................................................................... n = 4 .................................................................................................................................................................................................... n = 5 .................................................................................................................................................................................................... n = 6 .................................................................................................................................................................................................... n = 7 .................................................................................................................................................................................................... Average ................................................................................................................................................................................................ Standard Deviation .............................................................................................................................................................................. MDL** ................................................................................................................................................................................................... 0.001775 0.001812 0.001773 0.001792 0.001712 0.001767 0.001778 0.001773 0.000031 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 Recovery, ICP–MS, (percent) Extraction method NIST 1547 plant Ultrasonic Bath ................................................................................................ WREIER-AVILES on DSK5TPTVN1PROD with RULES 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. VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 NIST 2709 soil 104 ± 5 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. PO 00000 Frm 00054 Fmt 4700 Sfmt 4700 93 ± 1 NIST 2583 dust 108 ± 11 NIST 2582 paint 96 ± 3 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. E:\FR\FM\03JYR1.SGM 03JYR1 Federal Register / Vol. 78, No. 128 / Wednesday, July 3, 2013 / Rules and Regulations 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: https://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: https://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: https://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 Environmental Protection Agency (EPA). ACTION: Direct final rule. AGENCY: 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). WREIER-AVILES on DSK5TPTVN1PROD with RULES SUMMARY: VerDate Mar<15>2010 15:18 Jul 02, 2013 Jkt 229001 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 DATES: PO 00000 Frm 00055 Fmt 4700 Sfmt 4700 40011 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 E:\FR\FM\03JYR1.SGM 03JYR1

Agencies

[Federal Register Volume 78, Number 128 (Wednesday, July 3, 2013)]
[Rules and Regulations]
[Pages 40000-40011]
From the Federal Register Online via the Government Printing Office [www.gpo.gov]
[FR Doc No: 2013-15880]


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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.

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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

[[Page 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: https://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 ([mu]g/m\3\) of Pb 
to 0.15 [mu]g/m\3\ 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 [mu]g/m\3\. 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 [mu]g/m\3\ (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 [mu]g/m\3\ and the requirement 
for a minimum method detection limit was established at 0.0075 [mu]g/
m\3\. 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 
[mu]g/m\3\, which is well below the requirement of 0.0075 [mu]g/m\3\.

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[deg]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[deg]C) graphite block (hot block) with 3.5 percent volume/

[[Page 40002]]

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.
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    \1\ CASAC'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: https://yosemite.epa.gov/sab/
sabproduct.nsf/DA39026E54BAF46E8525781D00606633/$File/EPA-CASAC-11-
002-unsigned.pdf.
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    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.
---------------------------------------------------------------------------

    \2\ FEM EQL-0400-0140 (65 FR 26603, May 8, 2000).
    \3\ The list of current FEMs is located at: https://epa.gov/ttn/amtic/files/ambient/criteria/reference-equivalent-methods-list.pdf.
---------------------------------------------------------------------------

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.
---------------------------------------------------------------------------

    \4\ Refer to: https://water.epa.gov/scitech/methods/cwa/det/index.cfm for EPA's Procedures for Detection and Quantitation.
---------------------------------------------------------------------------

    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 [mu]g/mL. The MDLs were estimated to 
demonstrate method performance that is more than adequate to meet the 
MDL requirements of 0.0075 [mu]g/m\3\ 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

[[Page 40003]]

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 [mu]g/m\3\. 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 
high-volume 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.

[[Page 40004]]

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

0
1. The authority citation for part 50 continues to read as follows:

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


0
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 [mu]g/m\3\ to 0.15 [mu]g/m\3\ 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-[micro]g/mL (ppb) 
determination of Pb in a wide variety of matrices. Results reported 
for monitoring or compliance purposes are calculated in [mu]g/m\3\ 
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. \115\In 
(Indium), \165\Ho (Holmium), and \209\Bi (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 Pb-spiked filters 
or filter strips analyzed in accordance with the guidance provided 
in 40

[[Page 40005]]

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 [micro]g/m\3\ to 0.60 
[micro]g/m\3\, and based on the low and high calibration curve 
standards and a nominal filter sample volume of 2000 m\3\.
    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

[[Page 40006]]

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 [deg]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 [deg]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[supreg] 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 [mu]L,  1 percent 
accuracy, <=1 percent RSD (precision), with disposable tips, or 
equivalent.
     Pipette, Rainin EDP2, 1000 [mu]L,  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 non-metal 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 
M[Omega]-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 M[Omega]-
cm.
    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 [mu]g/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 [mu]g/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 [mu]g/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 [mu]g/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 [mu]g/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\
---------------------------------------------------------------------------

    \5\ Certificates of Analysis for these SRMs can be found at: 
https://www.nist.gov/srm/index.cfm.
---------------------------------------------------------------------------

    Note: The In, Bi, and Ho internal standards may also be 
purchased as 10 [micro]g/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 [micro]g/
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 [micro]g/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 [micro]g per filter or 0.0075 [micro]g/m\3\ using a 
nominal sample volume of 2000 m\3\ and 4.8 ng/cm\2\ or 0.0024 
[micro]g/m\3\ for PTFE filters using a nominal sample volume of 24 
m\3\. 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 
[micro]g/m\3\; 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/

[[Page 40007]]

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 [micro]g/mL. The 
recovery for the RBS must be within  20 percent of the 
expected value. If the RB yields a result above 0.001 [micro]g/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.

------------------------------------------------------------------------
                                                        Performance
          Sample                  Frequency            specification
------------------------------------------------------------------------
ICB.......................  Prior to first sample  Less than 0.001 [mu]g/
                                                    mL.
ICV.......................  Prior to first sample  Within 90 to 110
                                                    percent of the
                                                    expected value.
LLCV......................  Daily, before first    10
                             sample and after       percent of the
                             last sample.           expected value.
CCB.......................  After every 10         Less than 0.001 [mu]g/
                             extracted samples.     mL.
CCV.......................  After every 10         Within 90-110 percent
                             extracted samples.     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 [micro]g/mL. If either the ICV or the 
ICB fails, the run must be terminated, the problem identified and 
corrected, and the analysis re-started.
    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 [mu]g/mL. If either 
the CCV, LLCV, or CCB fails, the run must be terminated, the problem 
identified and

[[Page 40008]]

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 re-started 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[deg]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[deg]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[deg]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[deg]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[deg]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 85[ordm]C. Once 
the vessel is covered with a ribbed watch glass, the temperature of 
the water will increase to approximately 95[deg]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.

[[Page 40009]]

    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 [mu]g/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 [mu]g Pb/m\3\ to three significant figures as follows:

C = (([mu]g Pb/mL * Vf * A)* D))/Vs

Where:
C = Concentration, [mu]g Pb/m\3\
[mu]g Pb/mL = Lead concentration in solution
Vf = Total extraction solution volume
A = Area correction; \3/4\'' x 8'' strip = 5.25 in\2\ analyzed, A = 
12.0 or 1'' x 8'' strip = 7 in\2\ 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 x 10-inch 
TSP filter which has a sampled area of 9-inch x 7-inch (63.0 in\2\) 
due to the \1/2\-inch filter holder border around the outer edge. 
The \3/4\-inch x 8-inch strip has a sampled area of \3/4\-inch x 7-
inch (5.25 in\2\). The 1-inch x 8-inch strip has a sampled area of 
1-inch x 7-inch (7.0 in\2\). 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 [mu]g/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 
[mu]g/m\3\. 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    Hotblock
                                                 extraction   extraction
                                                   method       method
                                               -------------------------
                                                [mu]g/m\3\*  [mu]g/m\3\*
------------------------------------------------------------------------
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 m\3\ 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
----------------------------------------------------------------------------------------------------------------
                                                                    Recovery, ICP-MS, (percent)
                                                 ---------------------------------------------------------------
                Extraction method                    NIST 1547                                       NIST 2582
                                                       plant      NIST 2709 soil  NIST 2583 dust       paint
----------------------------------------------------------------------------------------------------------------
Ultrasonic Bath.................................      100  4        minus> 1        minus> 8        minus> 0
Block Digestion.................................       92  7        minus> 3        minus> 4        minus> 4
----------------------------------------------------------------------------------------------------------------


   Table 3--Method Detection Limits Determined by Analysis of Reagent/
         Quartz Filter Blanks Spiked With Low-level Pb Solution
------------------------------------------------------------------------
                                                 Ultrasonic    Hotblock
                                                 extraction   extraction
                                                   method       method
                                               -------------------------
                                                [mu]g/m\3\*  [mu]g/m\3\*
------------------------------------------------------------------------
n = 1.........................................     0.000533     0.000274
n = 2.........................................     0.000552     0.000271
n = 3.........................................     0.000534     0.000281
n = 4.........................................     0.000684     0.000269

[[Page 40010]]

 
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 m\3\ 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
----------------------------------------------------------------------------------------------------------------
                                                                    Recovery, ICP-MS, (percent)
                                                 ---------------------------------------------------------------
                Extraction method                    NIST 1547                                       NIST 2582
                                                       plant      NIST 2709 soil  NIST 2583 dust       paint
----------------------------------------------------------------------------------------------------------------
Ultrasonic Bath.................................      101  6        minus> 1        minus> 5        minus> 1
Block Digestion.................................      106  3        minus> 3        minus> 6        minus> 2
----------------------------------------------------------------------------------------------------------------


 Table 5--Method Detection Limits Determined by Analysis of Reagent/PTFE
             Filter Blanks Spiked With Low-Level Pb Solution
------------------------------------------------------------------------
                                                            Ultrasonic
                                                            extraction
                                                              method
                                                         ---------------
                                                            [mu]g/m\3\*
------------------------------------------------------------------------
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 m\3\ 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
----------------------------------------------------------------------------------------------------------------
                                                                    Recovery, ICP-MS, (percent)
                                                 ---------------------------------------------------------------
                Extraction method                    NIST 1547                                       NIST 2582
                                                       plant      NIST 2709 soil  NIST 2583 dust       paint
----------------------------------------------------------------------------------------------------------------
Ultrasonic Bath.................................      104  5        minus> 1       minus> 11        minus> 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 Pb-containing 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.

[[Page 40011]]

    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: https://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: https://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: 
https://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