Amendments for Testing and Monitoring Provisions

ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 60, 61, and 63

[FRL-5880-8]

RIN 2060-AG21

Amendments for Testing and Monitoring Provisions

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule: Amendments.

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SUMMARY: This action proposes amendments to 40 CFR parts 60, 61, and 63

to reflect miscellaneous editorial changes and technical corrections

throughout the parts in sections pertaining to source testing or

monitoring of emissions and operations, and proposes to add Performance

Specification 15 (PS 15) to Appendix B of Part 60. In addition, the

test methods in Appendix A of Part 60, Appendix B of Part 61, Appendix

A of Part 63, and the performance specifications in Appendix B of Part

60 are proposed to be restructured in the format recommended by the

Environmental Monitoring Management Council (EMMC) to achieve

uniformity and consistency between Agency methods. The editorial

changes and technical corrections to the subparts, test methods, and/or

performance specifications in Parts 60, 61, and 63 are proposed to

maintain the intent of the regulations.

DATES: Comments. Comments must be received on or before October 27,

1997 unless a hearing is requested by September 8, 1997. If a hearing

is requested, written comments must be received by October 14, 1997.

Public Hearing. Anyone requesting a public hearing must contact EPA

no later than September 8, 1997. If a hearing is held, it will take

place on September 10, 1997, beginning at 9:00 a.m.

Request To Speak at Hearing. Persons wishing to present oral

testimony must contact EPA by September 10, 1997.

ADDRESSES: Comments. Comments should be submitted (in duplicate, if

possible) to: Air and Radiation Docket and Information Center (6102),

Attention Docket No. A-97-12 (see docket section below), room M-1500,

U.S. Environmental Protection Agency, 401 M Street, SW., Washington, DC

20460. The Agency requests that a separate copy also be sent to the

person listed in the FOR FURTHER INFORMATION CONTACT section below.

Public Hearing. If anyone contacts EPA requesting a public hearing,

it will be held at the EPA's Emissions Measurement Laboratory, Research

Triangle Park, North Carolina. Persons interested in attending the

hearing or wishing to present oral testimony should notify Ms. Lala

Cheek (MD-19), U.S. Environmental Protection Agency, Research Triangle

Park, NC 27711, telephone (919) 541-5545.

Docket. Docket No. A-97-12, containing materials relevant to this

rulemaking, is available for public inspection and copying between 8:00

a.m. and 5:30 p.m., Monday through Friday, except for Federal holidays,

at the EPA's Air and Radiation Docket and Information Center, Room M-

1500, U.S. Environmental Protection Agency, 401 M Street, SW.,

Washington, DC 20460; telephone (202) 260-7548. A reasonable fee may be

charged for copying.

FOR FURTHER INFORMATION CONTACT:

Mr. Foston Curtis, Emission Measurement Center (MD-19), Emissions,

Monitoring, and Analysis Division, U.S. Environmental Protection

Agency, Research Triangle Park, North Carolina 27711, telephone number

(919) 541-1063 or at fax number (919) 541-1039.

SUPPLEMENTARY INFORMATION: The information presented in this preamble

is organized as follows:

I. Background and Purpose

II. EMMC Format

III. Significant Technical Revisions to Specific Test Methods,

Performance Specifications, and Rules

A. General

B. ASTM Methods Updates

C. Continuous Instrumental Methods (Part 60, Appendix A)--

Methods 3A, 6C, 7E, 10, and 20

D. Method 5 (Part 60, Appendix A)

E. Method 5E (Part 60, Appendix A)

F. Method 5H (Part 60, Appendix A)

G. Method 18 (Part 60, Appendix A)

H. Methods 306, 306A, and 306B (Part 63, Appendix A)

IV. Addition of Performance Specification 15

V. Copies of Regulatory Text

VI. Administrative Requirements

A. Docket

B. Office of Management and Budget Review

C. Regulatory Flexibility Act

D. Paperwork Reduction Act

E. Unfunded Mandates Reform Act

I. Background and Purpose

As part of its efforts to promote methods consolidation and

integration between EPA Program Offices, the EMMC developed a consensus

format for documentation of analytical methods. The Office of Air and

Radiation has adapted the format for its new methods and is attempting

to update its existing methods to this format. The EMMC format is shown

in Section II. To achieve consistency between the test methods and

performance specifications, EPA is proposing to restructure the test

methods and performance specifications shown in Table 1 in the EMMC

format. In addition, EPA reviewed the test methods and performance

specifications and associated regulations in 40 CFR Parts 60, 61, and

63 and found that corrections and revisions were necessary. The

corrections and revisions consisted primarily of typographical errors,

technical errors in equations and diagrams, and narrative that is no

longer applicable due to more recent additions. However, a few methods

required further revision due to needed technical updates and comments

received from the public. These methods are discussed in Section III.

It is important to note that although numerous technical corrections

were made to portions of the subparts in Parts 60, 61, and 63, changes

were not made to any compliance standard, reporting, or recordkeeping

requirement. For this notice, EPA is only proposing revisions to

sections of the subpart pertaining to source testing or monitoring of

emissions and operations.

II. EMMC Format

The test methods and performance specifications listed in Table 1

are being proposed in the restructured format shown in Table 2 which is

recommended by EMMC. Only in a few instances were there any deviations

from this recommended format.

Table 1.--Test Methods and Performance Specifications Restructured in the EMMC Format

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40 CFR 63, appendix

40 CFR part 60, appendix A 40 CFR part 60, appendix B 40 CFR 61, appendix B A

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1, 1a.......................... PS-2........................ 101, 101a................... 303, 303a

2, 2a, 2b, 2c,................. PS-3........................ 102......................... 304a,

2d, 2e......................... PS-4, PS-4a................. 103......................... 304b

3, 3a, 3b...................... PS-5........................ 104......................... 305

[[Page 45370]]

4.............................. PS-6........................ 105......................... 306,

5, 5a, 5b, 5d,................. PS-7........................ 106......................... 306a,

5e, 5f, 5g, 5h................. PS-8........................ 107, 107a................... 306b

6, 6a, 6b, 6c.................. PS-9........................ 108......................... ...................

7, 7a, 7b, 7c,................. ............................ 108a........................ ...................

7d, 7e......................... ............................ 108b........................ ...................

8.............................. ............................ 108c........................ ...................

10, 10a, 10b................... ............................ 111......................... ...................

11............................. ............................ ............................ ...................

12............................. ............................ ............................ ...................

13a, 13b....................... ............................ ............................ ...................

14............................. ............................ ............................ ...................

15, 15a........................ ............................ ............................ ...................

16, 16a, 16b................... ............................ ............................ ...................

17............................. ............................ ............................ ...................

18............................. ............................ ............................ ...................

19............................. ............................ ............................ ...................

20............................. ............................ ............................ ...................

21............................. ............................ ............................ ...................

22............................. ............................ ............................ ...................

23............................. ............................ ............................ ...................

24, 24a........................ ............................ ............................ ...................

25, 25a, 25b,.................. ............................ ............................ ...................

25c, 25d, 25e.................. ............................ ............................ ...................

26, 26a........................ ............................ ............................ ...................

27............................. ............................ ............................ ...................

28, 28a........................ ............................ ............................ ...................

29............................. ............................ ............................ ...................

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Table 2.--EMMC Format

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Section No. Section heading

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1.0................................. Scope and Application.

2.0................................. Summary of the Method.

3.0................................. Definitions.

4.0................................. Interferences.

5.0................................. Safety.

6.0................................. Equipment and Supplies.

7.0................................. Reagents and Standards.

8.0................................. Sample Collection, Preservation,

Storage and Transport.

9.0................................. Quality Control.

10.0................................ Calibration and Standardization.

11.0................................ Analytical Procedure.

12.0................................ Calculations and Data Analysis.

13.0................................ Method Performance.

14.0................................ Pollution Prevention.

15.0................................ Waste Management.

16.0................................ References.

17.0................................ Tables, Diagrams, Flowcharts, and

Validation Data.

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III. Significant Technical Revisions to Specific Test Methods,

Performance Specifications, and Rules

A. General

A safety section (Section 5) was added to most of the test methods

and performance specifications. This section discusses only those

safety issues specific to the method and any target analytes or

reagents that pose specific toxicity or safety issues.

B. ASTM Methods Updates

The American Society for Testing and Materials assisted EPA in

revising test method references of ASTM methods by providing an update

of all ASTM procedures cited in the test methods. Many Agency methods

cite obsolete versions of ASTM methods that have been improved and

redated or redesignated since the EPA methods were promulgated. Where

appropriate, the redated and redesignated versions are included to add

flexibility and clarify which methods may be used. In addition, the

Incorporation by Reference citations in Sec. 60.17 are amended to add

the updated ASTM versions. The Agency is grateful for ASTM's assistance

in this effort.

C. Continuous Instrumental Methods (Part 60, Appendix A)--Methods 3A,

6C, 7E, 10, and 20

The continuous instrumental methods have been coordinated to

require the same performance specifications and, where applicable, the

same testing procedures and equipment specifications.

D. Method 5 (Part 60, Appendix A)

Section 6.1.1.7 (formerly Section 2.1.6) specifies that a

temperature sensor be installed so that the sensing tip of the

temperature sensor is in direct contact with the sample gas and that

the temperature around the filter holder be regulated and monitored

during sampling. EPA recognized that, depending on the sampling

apparatus, temperature in the heating area may be measured at different

locations (e.g., near the heater or at the top of the heated area)

resulting in deviations from the recommended temperature range of

24825 deg.F. This modification was made so that temperature

inside the heating area is measured at a consistent location in the gas

stream. This modification requires that an extra temperature sensor be

used with the filter heating system.

E. Method 5E (Part 60, Appendix A)

Section 6.3.4 (formerly Section 2.3.4) no longer specifies the

Beckman Model 915 analyzer with a 215 B infrared or equivalent. Since

the Beckman Model 915 is no longer manufactured, the EPA determined

that the Rosemount Model 2100A TOC analyzer was comparable to the

Beckman 915 model. As a result, Section 6.3.4 no longer specifies the

Beckman Model 915 with 215 B infrared or equivalent but instead, the

Rosemount Model 2100A TOC analyzer.

F. Method 5H (Part 60, Appendix A)

Section 7.3.4.1 (formerly Section 3.3.1.4) has been revised to

specify that only three calibration gas levels (high-range, mid-range,

and zero gases) are needed to calibrate the carbon dioxide, carbon

monoxide, and sulfur dioxide

[[Page 45371]]

(SO2) analyzers instead of four calibration gas levels. The

low-range calibration gas is no longer required. This revision is

consistent with the gas levels used to calibrate the SO2

analyzer as described in Section 7.4 (formerly Section 5.3) of Method

6C (Determination of Sulfur Dioxide Emissions from Stationary Sources).

G. Method 18 (Part 60, Appendix A)

The Agency is soliciting comments on procedural modifications to

Method 18 being proposed in this action. In the direct interface

sampling procedure, the requirement for two consecutive samples to have

less than 5 percent difference is being replaced with taking 5

consecutive samples per run. This modification allows for direct

interface sampling to be used in cases where the process is highly

variable. The adsorbent tube procedure is being modified to allow the

source to choose any commercially available adsorbent material, instead

of relying on the few adsorbents listed in the previous version of the

method. In preparing calibration gases, it is proposed to allow the use

of gas dilution instruments meeting the requirements of Method 205 of

40 CFR part 51, appendix M.

H. Methods 306, 306A, and 306B (Part 63, Appendix A)

Numerous editorial revisions were made to clarify the requirements

of Methods 306, 306A, and 306B. The applicability sections of Methods

306, 306A, and 306B have been revised to add continuous chromium

plating at iron and steel facilities to the list of source categories

to which these methods apply. The requirement for filtration of all

samples to be analyzed by ion chromatography has been eliminated from

Section 9.2 (formerly Section 5.2.3) of Method 306 and Section 9.2

(formerly Section 5.2.3) of Method 306A. Instead, a qualifying note has

been added stating that filtration is not required if a sample does not

contain particulate matter. The filtration procedure would only apply

when visible particulate is present in the sample (chromium

electroplating and anodizing baths emit little, if any particulate);

when needed, the tester is referred to the filtration procedure in

Method 0061 in Test Methods for Evaluating Solid Waste, Physical/

Chemical Methods, SW-846 Manual, November 1986. Section 9.2.2 (formerly

Section 5.1) of Method 306 has been revised to modify the post-sampling

pH requirement for the sodium bicarbonate absorbing solution when it

will be submitted to analysis by ion chromatography for hexavalent

chromium. The pH must be 8.0 rather than 8.5, as

the sodium bicarbonate solution does not reach a pH of 8.5. This

requirement has also been added to Section 9.2.2 of Method 306A.

Specific requirements for sample storage and sample holding times have

been added to Sections 9.3 and 9.4, respectively, of Methods 306 and

306A. Section 9.1.2.3 (formerly Section 5.1.2.3) of Method 306A has

been revised to add an option to adjust the sample volume for leaks

discovered during the post-test leak-check. This option is consistent

with that of Method 5 (40 CFR part 60, appendix A).

IV. Addition of Performance Specification 15

Performance Specification 15 is being proposed for addition to

Appendix B of Part 60. Performance specification 15 may be used by

sources to certify extractive Fourier Transform Infrared spectroscopy

(FTIR) continuous emission monitors for regulated pollutants. The

specification will determine the acceptability of FTIR continuous

emission monitoring systems and is not source-specific. The procedure

gives the source the option of using several techniques for FTIR

certification including relative accuracy testing, spiking of target

compounds, and comparison of dual instruments.

V. Copies of Regulatory Text

The text of the other proposed amendments is not included in this

Federal Register action because of the magnitude of the reformatted

test methods and amendments. The significant proposed amendments are

discussed fully in this preamble. Performance Specification 15, which

is a new procedure, is being published with this action as a proposed

amendment to appendix B to part 60. The unpublished proposed amendments

are available in Docket A-97-12 or by request from the Air and

Radiation Docket and Information Center (see ADDRESSES) or the EPA

contact person listed in the preceding FOR FURTHER INFORMATION CONTACT

section. The proposed amendments may also be obtained over the Internet

at http://www.epa.gov/oar/oaqps/emc; choose the ``Test Methods'' menu,

then choose ``Proposed Test Methods.'' The amendments will be listed on

the EPA Technology Transfer Network (TTN). The TTN is a network of

electronic bulletin boards developed and operated by the Office of Air

Quality Planning and Standards. The TTN provides information and

technology exchange in various areas of air pollution control. The

service is free, except for the cost of the phone call. Dial (919) 541-

5742 for data transfer of up to a 14,400 bps modem. Select TTN Bulletin

Board: ``Emission Measurement Technical Information Center (EMTIC)''

and select menu item ``Proposed Methods.'' If more information on the

operation of the TTN is needed, contact the systems operator at (919)

541-5384.

VI. Administrative Requirements

A. Docket

The docket is an organized and complete file of all information

submitted to or otherwise considered by EPA in the development of this

proposed rulemaking. The principal purposes of the docket are: (1) To

allow interested parties to identify and locate documents so that they

can effectively participate in the rulemaking process, and (2) to serve

as the record in case of judicial review (except for interagency review

materials) [Clean Air Act Section 307(d)(7)(A)].

B. Office of Management and Budget Review

Under Executive Order 12866 (58 FR 51735 October 4, 1993), EPA is

required to judge whether a regulation is ``significant'' and therefore

subject to Office of Management and Budget (OMB) review and the

requirements of this Executive Order to prepare a regulatory impact

analysis (RIA). The Order defines ``significant regulatory action'' as

one that is likely to result in a rule that may:

(1) Have an annual effect on the economy of $100 million or more or

adversely affect in a material way the economy, a sector of the

economy, productivity, competition, jobs, the environment, public

health or safety, or State, local, or tribal governments or

communities;

(2) Create a serious inconsistency or otherwise interfere with an

action taken or planned by another agency;

(3) Materially alter the budgetary impact of entitlements, grants,

user fees, or loan programs, or the rights and obligation of recipients

thereof; or

(4) Raise novel legal or policy issues arising out of legal

mandates, the President's priorities, or the principles set forth in

the Executive Order. This rulemaking does not impose emission

measurement requirements beyond those specified in the current

regulations, nor does it change any emission standard. The Agency has

determined that this regulation would result in none of the adverse

economic effects set forth in Section 1 of the Order as grounds for

finding the regulation to be a significant rule. The Agency has,

[[Page 45372]]

therefore, concluded that this regulation is not a significant rule

under Executive Order 12866.

C. Regulatory Flexibility Act

The EPA has determined that it is not necessary to prepare a

regulatory flexibility analysis in connection with this proposed rule.

The EPA has also determined that this rule will not have a significant

adverse impact on a substantial number of small businesses. This

rulemaking does not impose emission measurement requirements beyond

those specified in the current regulations, nor does it change any

emission standard. As such, it will not present a significant economic

impact on a substantial number of small businesses.

D. Paperwork Reduction Act

The rule does not impose or change any information collection

requirements subject to OMB review under the Paperwork Reduction Act,

44 U.S.C. 3501 et seq.

E. Unfunded Mandates Reform Act

Under Section 202 of the Unfunded Mandates Reform Act of 1995

(``Unfunded Mandates Act'') signed into law on March 22, 1995, EPA must

prepare a budgetary impact statement to accompany any proposed or final

rule that includes a Federal mandate that may result in estimated costs

to State, local, or tribal governments in the aggregate, or to the

private sector, of $100 million or more. Under Section 205, EPA must

select the most cost-effective and least burdensome alternative that

achieves the objectives of the rule and is consistent with statutory

requirements. Section 203 requires EPA to establish a plan for

informing and advising any small governments that may be significantly

or uniquely impacted by the rule.

The EPA has determined that the action proposed today does not

include a Federal mandate that may result in estimated costs of $100

million or more to either State, local, or tribal governments in the

aggregate, or to the private sector, nor does this action significantly

or uniquely impact small governments, because this action contains no

requirements that apply to such governments or impose obligations upon

them. Therefore, the requirements of the Unfunded Mandates Act do not

apply to this action.

List of Subjects in 40 CFR Part 60

Environmental protection, Air pollution control, New sources, Test

methods and procedures, Performance specifications, Continuous emission

monitors.

40 CFR Part 61

Environmental protection, Air pollution control, Test methods and

procedures.

40 CFR Part 63

Environmental protection, Air pollution control, Hazardous air

pollutants, Test methods and procedures.

Dated: August 18, 1997.

Carol M. Browner,

Administrator.

It is proposed that 40 CFR part 60 be amended as follows:

1. The authority citation for part 60 continues to read as follows:

Authority: 42 U.S.C. 7401, 7411, 7414, 7416, 7601 and 7602.

2. By adding Performance Specification 15 in numerical order to

Appendix B to read as follows:

Appendix B--Performance Specifications

* * * * *

Performance Specification 15--Performance Specification for

Extractive FTIR Continuous Emissions Monitor Systems in Stationary

Sources

1.0 Scope and Application. 1.1 Analytes. This performance

specification is applicable for measuring all hazardous air

pollutants (HAPs) which absorb in the infrared region and can be

quantified using Fourier Transform Infrared Spectroscopy (FTIR), as

long as the performance criteria of this performance specification

are met. This specification is to be used for evaluating FTIR

continuous emission monitoring systems for measuring HAPs regulated

under Title III of the 1990 Clean Air Act Amendments. This

specification also applies to the use of FTIR CEMs for measuring

other volatile organic or inorganic species.

1.2 Applicability. A source which can demonstrate that the

extractive FTIR system meets the criteria of this performance

specification for each regulated pollutant may use the FTIR system

to continuously monitor for the regulated pollutants.

2.0 Summary of Performance Specification. For compound-specific

sampling requirements refer to FTIR sampling methods (e.g.,

reference 1). For data reduction procedures and requirements refer

to the EPA FTIR Protocol (reference 2), hereafter referred to as the

``FTIR Protocol.'' This specification describes sampling and

analytical procedures for quality assurance. The infrared spectrum

of any absorbing compound provides a distinct signature. The

infrared spectrum of a mixture contains the superimposed spectra of

each mixture component. Thus, an FTIR CEM provides the capability to

continuously measure multiple components in a sample using a single

analyzer. The number of compounds that can be speciated in a single

spectrum depends, in practice, on the specific compounds present and

the test conditions.

3.0 Definitions. For a list of definitions related to FTIR

spectroscopy refer to Appendix A of the FTIR Protocol. Unless

otherwise specified, spectroscopic terms, symbols and equations in

this performance specification are taken from the FTIR Protocol or

from documents cited in the Protocol. Additional definitions are

given below.

3.1 FTIR Continuous Emission Monitoring System (FTIR CEM).

3.1.1 FTIR System. Instrument to measure spectra in the mid-

infrared spectral region (500 to 4000 cm -1). It contains

an infrared source, interferometer, sample gas containment cell,

infrared detector, and computer. The interferometer consists of a

beam splitter that divides the beam into two paths, one path a fixed

distance and the other a variable distance. The computer is equipped

with software to run the interferometer and store the raw digitized

signal from the detector (interferogram). The software performs the

mathematical conversion (the Fourier transform) of the interferogram

into a spectrum showing the frequency dependent sample absorbance.

All spectral data can be stored on computer media.

3.1.2 Gas Cell. A gas containment cell that can be evacuated.

It contains the sample as the infrared beam passes from the

interferometer, through the sample, and to the detector. The gas

cell may have multi-pass mirrors depending on the required detection

limit(s) for the application.

3.1.3 Sampling System. Equipment used to extract sample from

the test location and transport the gas to the FTIR analyzer.

Sampling system components include probe, heated line, heated non-

reactive pump, gas distribution manifold and valves, flow

measurement devices and any sample conditioning systems.

3.2 Reference CEM. An FTIR CEM, with sampling system, that can

be used for comparison measurements.

3.3 Infrared Band (also Absorbance Band or Band). Collection of

lines arising from rotational transitions superimposed on a

vibrational transition. An infrared absorbance band is analyzed to

determine the analyte concentration.

3.4 Sample Analysis. Interpreting infrared band shapes,

frequencies, and intensities to obtain sample component

concentrations. This is usually performed by a software routine

using a classical least squares (cls), partial least squares (pls),

or K-or P-matrix method.

3.5 (Target) Analyte. A compound whose measurement is required,

usually to some established limit of detection and analytical

uncertainty.

3.6 Interferant. A compound in the sample matrix whose infrared

spectrum overlaps at least part of an analyte spectrum complicating

the analyte measurement. The interferant may not prevent the analyte

measurement, but could increase the analytical uncertainty in the

measured

[[Page 45373]]

concentration. Reference spectra of interferants are used to

distinguish the interferant bands from the analyte bands. An

interferant for one analyte may not be an interferant for other

analytes.

3.7 Reference Spectrum. Infrared spectra of an analyte, or

interferant, prepared under controlled, documented, and reproducible

laboratory conditions (see Section 4.6 of the FTIR Protocol). A

suitable library of reference spectra can be used to measure target

analytes in gas samples.

3.8 Calibration Spectrum. Infrared spectrum of a compound

suitable for characterizing the FTIR instrument configuration

(Section 4.5 in the FTIR Protocol).

3.9 One hundred percent line. A double beam transmittance

spectrum obtained by combining two successive background single beam

spectra. Ideally, this line is equal to 100 percent transmittance

(or zero absorbance) at every point in the spectrum. The zero

absorbance line is used to measure the RMS noise of the system.

3.10 Background Deviation. Any deviation (from 100 percent) in

the one hundred percent line (or from zero absorbance). Deviations

greater than 5 percent in any analytical region are

unacceptable. Such deviations indicate a change in the instrument

throughput relative to the single-beam background.

3.11 Batch Sampling. A gas cell is alternately filled and

evacuated. A Spectrum of each filled cell (one discreet sample) is

collected and saved.

3.12 Continuous Sampling. Sample is continuously flowing

through a gas cell. Spectra of the flowing sample are collected at

regular intervals.

3.13 Continuous Operation. In continuous operation an FTIR CEM

system, without user intervention, samples flue gas, records spectra

of samples, saves the spectra to a disk, analyzes the spectra for

the target analytes, and prints concentrations of target analytes to

a computer file. User intervention is permitted for initial set-up

of sampling system, initial calibrations, and periodic maintenance.

3.14 Sampling Time. In batch sampling--the time required to

fill the cell with flue gas. In continuous sampling--the time

required to collect the infrared spectrum of the sample gas.

3.15 PPM-Meters. Sample concentration expressed as the

concentration-path length product, ppm (molar) concentration

multiplied by the path length of the FTIR gas cell. Expressing

concentration in these units provides a way to directly compare

measurements made using systems with different optical

configurations. Another useful expression is (ppm-meters)/K, where K

is the absolute temperature of the sample in the gas cell.

3.16 CEM Measurement Time Constant. The Time Constant (TC,

minutes for one cell volume to flow through the cell) determines the

minimum interval for complete removal of an analyte from the FTIR

cell. It depends on the sampling rate (Rs in Lpm), the

FTIR cell volume (Vcell in L) and the chemical and

physical properties of an analyte.

[GRAPHIC] [TIFF OMITTED] TP27AU97.013

For example, if the sample flow rate (through the FTIR cell) is

5 Lpm and the cell volume is 7 liters, then TC is equal to 1.4

minutes (0.71 cell volumes per minute). This performance

specification defines 5 * TC as the minimum interval between

independent samples.

3.17 Independent Measurement. Two independent measurements are

spectra of two independent samples. Two independent samples are

separated by, at least 5 cell volumes. The interval between

independent measurements depends on the cell volume and the sample

flow rate (through the cell). There is no mixing of gas between two

independent samples. Alternatively, estimate the analyte residence

time empirically: (1) Fill cell to ambient pressure with a (known

analyte concentration) gas standard, (2) measure the spectrum of the

gas standard, (3) purge the cell with zero gas at the sampling rate

and collect a spectrum every minute until the analyte standard is no

longer detected spectroscopically. If the measured time corresponds

to less than 5 cell volumes, use 5 * TC as the minimum interval

between independent measurements. If the measured time is greater

than 5 * TC, then use this time as the minimum interval between

independent measurements.

3.18 Test Condition. A period of sampling where all process,

and sampling conditions, and emissions remain constant and during

which a single sampling technique and a single analytical program

are used. One Run may include results for more than one test

condition. Constant emissions means that the composition of the

emissions remains approximately stable so that a single analytical

program is suitable for analyzing all of the sample spectra. A

greater than two-fold change in analyte or interferant

concentrations or the appearance of additional compounds in the

emissions, may constitute a new test condition and may require

modification of the analytical program.

3.19 Run. A single Run consists of spectra (one spectrum each)

of at least 10 independent samples over a minimum of one hour. The

concentration results from the spectra can be averaged together to

give a run average for each analyte measured in the test run.

4.0 Interferences. Several compounds, including water, carbon

monoxide, and carbon dioxide, are known interferences in the

infrared region in which the FTIR instrument operates. Follow the

procedures in the FTIR protocol for subtracting or otherwise dealing

with these and other interferences.

5.0 Safety. The procedures required under this performance

specification may involve hazardous materials, operations, and

equipment. This performance specification does not purport to

address all of the safety problems associated with these procedures.

It is the responsibility of the user to establish appropriate safety

and health practices and determine the applicable regulatory

limitations prior to performing these procedures. The CEMS users

manual and materials recommended by this performance specification

should be consulted for specific precautions to be taken.

6.0 Equipment and Supplies. 6.1 Installation of sampling

equipment should follow requirements of FTIR test Methods such as

references 1 and 3 and the EPA FTIR Protocol (reference 2). Select

test points where the gas stream composition is representative of

the process emissions. If comparing to a reference method, the probe

tips for the FTIR CEM and the RM should be positioned close together

using the same sample port if possible.

6.2 FTIR Specifications. The FTIR CEM must be equipped with

reference spectra bracketing the range of path length-concentrations

(absorbance intensities) to be measured for each analyte. The

effective concentration range of the analyzer can be adjusted by

changing the path length of the gas cell or by diluting the sample.

The optical configuration of the FTIR system must be such that

maximum absorbance of any target analyte is no greater than 1.0 and

the minimum absorbance of any target analyte is at least 10 times

the RMSD noise in the analytical region. For example, if the

measured RMSD in an analytical region is equal to 10-3,

then the peak analyte absorbance is required to be at least 0.01.

Adequate measurement of all of the target analytes may require

changing path lengths during a run, conducting separate runs for

different analytes, diluting the sample, or using more than one gas

cell.

6.3 Data Storage Requirements. The system must have sufficient

capacity to store all data collected in one week of routine

sampling. Data must be stored to a write-protected medium, such as

write-once-read-many (WORM) optical storage medium or to a password

protected remote storage location. A back-up copy of all data can be

temporarily saved to the computer hard drive. The following items

must be stored during testing.

a. At least one sample interferogram per sampling Run or one

interferogram per hour, whichever is greater. This assumes that no

sampling or analytical conditions have changed during the run.

b. All sample absorbance spectra (about 12 per hr, 288 per day).

c. All background spectra and interferograms (variable, but

about 5 per day).

d. All CTS spectra and interferograms (at least 2 each 24 hour

period).

e. Documentation showing a record of resolution, path length,

apodization, sampling time, sampling conditions, and test conditions

for all sample, CTS, calibration, and background spectra.

Using a resolution of 0.5 cm-1, with analytical range

of 3500 cm-1, assuming about 65 Kbytes per spectrum and

130 Kb per interferogram, the storage requirement is about 164 Mb

for one week of continuous sampling. Lower spectral resolution

requires less storage capacity. All of the above data must be stored

for at least two weeks. After two weeks, storage requirements

include: (1) All analytical results (calculated concentrations), (2)

at least 1 sample spectrum with corresponding background and sample

interferograms for each test

[[Page 45374]]

condition, (3) CTS and calibration spectra with at least one

interferogram for CTS and all interferograms for calibrations, (4) a

record of analytical input used to produce results, and (5) all

other documentation. These data must be stored according to the

requirements of the applicable regulation.

7.0 Reagents and Standards. [Reserved]

8.0 Sample Collection, Preservation, Storage, and Transport.

[Reserved]

9.0 Quality Control. These procedures shall be used for

periodic quarterly or semiannual QA/QC checks on the operation of

the FTIR CEM. Some procedures test only the analytical program and

are not intended as a test of the sampling system.

9.1 Audit Sample. This can serve as a check on both the

sampling system and the analytical program.

9.1.1 Sample Requirements. The audit sample can be a mixture or

a single component. It must contain target analyte(s) at

approximately the expected flue gas concentration(s). If possible,

each mixture component concentration should be NIST traceable

(2 percent accuracy). If a cylinder mixture standard(s)

cannot be obtained, then, alternatively, a gas phase standard can be

generated from a condensed phase analyte sample. Audit sample

contents and concentrations are not revealed to the FTIR CEM

operator until after successful completion of procedures in 5.3.2.

9.1.2 Test Procedure. An audit sample is obtained from the

Administrator. Spike the audit sample using the analyte spike

procedure in Section 11. The audit sample is measured directly by

the FTIR system (undiluted) and then spiked into the effluent at a

known dilution ratio. Measure a series of spiked and unspiked

samples using the same procedures as those used to analyze the stack

gas. Analyze the results using Sections 12.1 and 12.2. The measured

concentration of each analyte must be within 5 percent

of the expected concentration (plus the uncertainty), i.e., the

calculated correction factor must be within 0.93 and 1.07 for an

audit with an analyte uncertainty of 2 percent.

9.2 Audit Spectra. Audit spectra can be used to test the

analytical program of the FTIR CEM, but provide no test of the

sampling system.

9.2.1 Definition and Requirements. Audit spectra are absorbance

spectra that: (1) Have been well characterized, and (2) contain

absorbance bands of target analyte(s) and potential interferants at

intensities equivalent to what is expected in the source effluent.

Audit spectra are provided by the administrator without identifying

information. Methods of preparing Audit spectra include: (1)

Mathematically adding sample spectra or adding reference and

interferant spectra, (2) obtaining sample spectra of mixtures

prepared in the laboratory, or (3) they may be sample spectra

collected previously at a similar source. In the last case it must

be demonstrated that the analytical results are correct and

reproducible. A record associated with each Audit spectrum documents

its method of preparation. The documentation must be sufficient to

enable an independent analyst to reproduce the Audit spectra.

9.2.2 Test Procedure. Audit spectra concentrations are measured

using the FTIR CEM analytical program. Analytical results must be

within 5 percent of the certified audit concentration

for each analyte (plus the uncertainty in the audit concentration).

If the condition is not met, demonstrate how the audit spectra are

unrepresentative of the sample spectra. If the audit spectra are

representative, modify the FTIR CEM analytical program until the

test requirement is met. Use the new analytical program in

subsequent FTIR CEM analyses of effluent samples.

9.3 Submit Spectra For Independent Analysis. This procedure

tests only the analytical program and not the FTIR CEM sampling

system. The analyst can submit FTIR CEM spectra for independent

analysis by EPA. Requirements for submission include: (1) Three

representative absorbance spectra (and stored interferograms) for

each test period to be reviewed, (2) corresponding CTS spectra, (3)

corresponding background spectra and interferograms, (4) spectra of

associated spiked samples if applicable, and (5) analytical results

for these sample spectra. The analyst will also submit documentation

of process times and conditions, sampling conditions associated with

each spectrum, file names and sampling times, method of analysis and

reference spectra used, optical configuration of FTIR CEM including

cell path length and temperature, spectral resolution and

apodization used for every spectrum. Independent analysis can also

be performed on site in conjunction with the FTIR CEM sampling and

analysis. Sample spectra are stored on the independent analytical

system as they are collected by the FTIR CEM system. The FTIR CEM

and the independent analyses are then performed separately. The two

analyses will agree to within 20 percent for each

analyte using the procedure in Section 12.3. This assumes both

analytical routines have properly accounted for differences in

optical path length, resolution, and temperature between the sample

spectra and the reference spectra.

10.0 Calibration/Standardization.

10.1 Calibration Transfer Standards. For CTS requirements see

Section 4.5 of the FTIR Protocol. A well characterized absorbance

band in the CTS gas is used to measure the path length and line

resolution of the instrument. The CTS measurements made at the

beginning of every 24 hour period must agree to within 5

percent after correction for differences in pressure. Verify that

the frequency response of the instrument and CTS absorbance

intensity are correct by comparing to other CTS spectra or by

referring to the literature.

10.2 Analyte Calibration. If EPA library reference spectra are

not available, use calibration standards to prepare reference

spectra according to Section 6 of the FTIR Protocol. A suitable set

of analyte reference data includes spectra of at least 2 independent

samples at each of at least 2 different concentrations. The

concentrations bracket a range that includes the expected analyte

absorbance intensities. The linear fit of the reference analyte band

areas must have a fractional calibration uncertainty (FCU in

Appendix F of the FTIR Protocol) of no greater than 10 percent. For

requirements of analyte standards refer to Section 4.6 of the FTIR

Protocol.

10.3 System Calibration. The calibration standard is introduced

at a point on the sampling probe. The sampling system is purged with

the calibration standard to verify that the absorbance measured in

this way is equal to the absorbance in the analyte calibration. Note

that the system calibration gives no indication of the ability of

the sampling system to transport the target analyte(s) under the

test conditions.

10.4 Analyte Spike. The target analyte(s) is spiked at the

outlet of the sampling probe, upstream of the particulate filter,

and combined with effluent at a ratio of about 1 part spike to 9

parts effluent. The measured absorbance of the spike is compared to

the expected absorbance of the spike plus the analyte concentration

already in the effluent. This measures sampling system bias, if any,

as distinguished from analyzer bias. It is important that spiked

sample pass through all of the sampling system components before

analysis.

10.5 Signal-to-Noise Ratio (S/N). The measure of S/N in this

performance specification is the root-mean-square (RMS) noise level

as given in Appendix C of the FTIR Protocol. The RMS noise level of

a contiguous segment of a spectrum is defined as the RMS difference

(RMSD) between the n contiguous absorbance values (Ai)

which form the segment and the mean value (AM) of that

segment.

[GRAPHIC] [TIFF OMITTED] TP27AU97.014

A decrease in the S/N may indicate a loss in optical throughput,

or detector or interferometer malfunction.

10.6 Background Deviation. The 100 percent baseline must be

between 95 and 105 percent transmittance (absorbance of 0.02 to

-0.02) in every analytical region. When background deviation exceeds

this range, a new background spectrum must be collected using

nitrogen or other zero gas.

10.7 Detector Linearity. Measure the background and CTS at

three instrument aperture settings; one at the aperture setting to

be used in the testing, and one each at settings one half and twice

the test aperture setting. Compare the three CTS spectra. CTS band

areas should agree to within the uncertainty of the cylinder

standard. If test aperture is the maximum aperture, collect CTS

spectrum at maximum aperture, then close the aperture to reduce the

IR through-put by half. Collect a second background and CTS at the

smaller aperture setting and compare the spectra as above. Instead

of changing the aperture neutral density filters can be used to

attenuate the infrared beam. Set up the FTIR system as it will be

used in the test measurements. Collect a CTS spectrum. Use a neutral

density filter to attenuate the infrared beam (either immediately

after the source or the interferometer) to approximately \1/2\ its

original intensity. Collect a second CTS spectrum. Use another

filter to attenuate the infrared beam to approximately \1/4\ its

original intensity. Collect a third background

[[Page 45375]]

and CTS spectrum. Compare the CTS spectra as above. Another check on

linearity is to observe the single beam background in frequency

regions where the optical configuration is known to have a zero

response. Verify that the detector response is ``flat'' and equal to

zero in these regions. If detector response is not linear, decrease

aperture, or attenuate the infrared beam. Repeat the linearity check

until system passes the requirement.

11.0 Analytical Procedure.

11.1 Initial Certification. First, perform the evaluation

procedures in Section 6.0 of the FTIR Protocol. The performance of

an FTIR CEM can be certified upon installation using EPA Method 301

type validation (40 CFR, Part 63, Appendix A), or by comparison to a

reference Method if one exists for the target analyte(s). Details of

each procedure are given below. Validation testing is used for

initial certification upon installation of a new system. Subsequent

performance checks can be performed with more limited analyte

spiking. Performance of the analytical program is checked initially,

and periodically as required by EPA, by analyzing audit spectra or

audit gases.

11.1.1 Validation. Use EPA Method 301 type sampling (reference

4, Section 5.3 of Method 301) to validate the FTIR CEM for measuring

the target analytes. The analyte spike procedure is as follows: (1)

A known concentration of analyte is mixed with a known concentration

of a non-reactive tracer gas, (2) the undiluted spike gas is sent

directly to the FTIR cell and a spectrum of this sample is

collected, (3) pre-heat the spiked gas to at least the sample line

temperature, (4) introduce spike gas at the back of the sample probe

upstream of the particulate filter, (5) spiked effluent is carried

through all sampling components downstream of the probe, (6) spike

at a ratio of roughly 1 part spike to 9 parts flue gas (or more

dilute), (7) the spike-to-flue gas ratio is estimated by comparing

the spike flow to the total sample flow, and (8) the spike ratio is

verified by comparing the tracer concentration in spiked flue gas to

the tracer concentration in undiluted spike gas. The analyte flue

gas concentration is unimportant as long as the spiked component can

be measured and the sample matrix (including interferences) is

similar to its composition under test conditions. Validation can be

performed using a single FTIR CEM analyzing sample spectra collected

sequentially. Since flue gas analyte (unspiked) concentrations can

vary, it is recommended that two separate sampling lines (and pumps)

are used; one line to carry unspiked flue gas and the other line to

carry spiked flue gas. Even with two sampling lines the variation in

unspiked concentration may be fast compared to the interval between

consecutive measurements. Alternatively, two FTIR CEMs can be

operated side-by-side, one measuring spiked sample, the other

unspiked sample. In this arrangement spiked and unspiked

measurements can be synchronized to minimize the affect of temporal

variation in the unspiked analyte concentration. In either sampling

arrangement, the interval between measured concentrations used in

the statistical analysis should be, at least, 5 cell volumes (5 * TC

in equation 1). A validation run consists of, at least, 24

independent analytical results, 12 spiked and 12 unspiked samples.

See Section 3.17 for definition of an ``independent'' analytical

result. The results are analyzed using Sections 12.1 and 12.2 to

determine if the measurements passed the validation requirements.

Several analytes can be spiked and measured in the same sampling

run, but a separate statistical analysis is performed for each

analyte. In lieu of 24 independent measurements, averaged results

can be used in the statistical analysis. In this procedure, a series

of consecutive spiked measurements are combined over a sampling

period to give a single average result. The related unspiked

measurements are averaged in the same way. The minimum 12 spiked and

12 unspiked result averages are obtained by averaging measurements

over subsequent sampling periods of equal duration. The averaged

results are grouped together and statistically analyzed using

Section 12.2.

11.1.1.1 Validation with a Single Analyzer and Sampling Line.

If one sampling line is used, connect the sampling system components

and purge the entire sampling system and cell with at least 10 cell

volumes of sample gas. Begin sampling by collecting spectra of 2

independent unspiked samples. Introduce the spike gas into the back

of the probe, upstream of the particulate filter. Allow 10 cell

volumes of spiked flue gas to purge the cell and sampling system.

Collect spectra of 2 independent spiked samples. Turn off the spike

flow and allow 10 cell volumes of unspiked flue gas to purge the

FTIR cell and sampling system. Repeat this procedure 6 times until

the 24 samples are collected. Spiked and unspiked samples can also

be measured in groups of 4 instead of in pairs. Analyze the results

using Sections 12.1 and 12.2. If the statistical analysis passes the

validation criteria, then the validation is completed. If the

results do not pass the validation, the cause may be that temporal

variations in the analyte sample gas concentration are fast relative

to the interval between measurements. The difficulty may be avoided

by: (1) Averaging the measurements over long sampling periods and

using the averaged results in the statistical analysis, (2)

modifying the sampling system to reduce TC by, for example, using a

smaller volume cell or increasing the sample flow rate, (3) using

two sample lines (4) use two analyzers to perform synchronized

measurements. This performance specification permits modifications

in the sampling system to minimize TC if the other requirements of

the validation sampling procedure are met.

11.1.1.2 Validation With a Single Analyzer and Two Sampling

Lines. An alternative sampling procedure uses two separate sample

lines, one carrying spiked flue gas, the other carrying unspiked

gas. A valve in the gas distribution manifold allows the operator to

choose either sample. A short heated line connects the FTIR cell to

the 3-way valve in the manifold. Both sampling lines are

continuously purged. Each sample line has a rotameter and a bypass

vent line after the rotameter, immediately upstream of the valve, so

that the spike and unspiked sample flows can each be continuously

monitored. Begin sampling by collecting spectra of 2 independent

unspiked samples. Turn the sampling valve to close off the unspiked

gas flow and allow the spiked flue gas to enter the FTIR cell.

Isolate and evacuate the cell and fill with the spiked sample to

ambient pressure. (While the evacuated cell is filling, prevent air

leaks into the cell by making sure that the spike sample rotameter

always indicates that a portion of the flow is directed out the by-

pass vent.) Open the cell outlet valve to allow spiked sample to

continuously flow through the cell. Measure spectra of 2 independent

spiked samples. Repeat this procedure until at least 24 samples are

collected.

11.1.1.3 Synchronized Measurements With Two Analyzers. Use two

FTIR analyzers, each with its own cell, to perform synchronized

spiked and unspiked measurements. If possible, use a similar optical

configuration for both systems. The optical configurations are

compared by measuring the same CTS gas with both analyzers. Each

FTIR system uses its own sampling system including a separate

sampling probe and sampling line. A common gas distribution manifold

can be used if the samples are never mixed. One sampling system and

analyzer measures spiked effluent. The other sampling system and

analyzer measures unspiked flue gas. The two systems are

synchronized so that so that each measures spectra at approximately

the same times. The sample flow rates are also synchronized so that

both sampling rates are approximately the same (TC1 TC2

in equation 1). Start both systems at the same time. Collect spectra

of at least 12 independent samples with each (spiked and unspiked)

system to obtain the minimum 24 measurements. Analyze the analytical

results using Sections 12.1 and 12.2. Run averages can be used in

the statistical analysis instead of individual measurements.

11.1.1.4 Compare to a Reference Method (RM). Obtain EPA

approval that the method qualifies as an RM for the analyte(s) and

the source to be tested. Follow the published procedures for the RM

in preparing and setting up equipment and sampling system,

performing measurements, and reporting results. Since FTIR CEMS have

multicomponent capability, it is possible to perform more than one

RM simultaneously, one for each target analyte. Conduct at least 9

runs where the FTIR CEM and the RM are sampling simultaneously. Each

Run is at least 30 minutes long and consists of spectra of at least

5 independent FTIR CEM samples and the corresponding RM

measurements. If more than 9 runs are conducted, the analyst may

eliminate up to 3 runs from the analysis if at least 9 runs are

used.

11.1.1.4.1 RMs Using Integrated Sampling. Perform the RM and

FTIR CEM sampling simultaneously. The FTIR CEM can measure spectra

as frequently as the analyst chooses (and should obtain measurements

as frequently as possible) provided that the measurements include

spectra of at least 5 independent measurements every 30 minutes.

Concentration results from all of the FTIR CEM spectra within a run

may be averaged for use in the statistical comparison

[[Page 45376]]

even if all of the measurements are not independent. When averaging

the FTIR CEM concentrations within a run, it is permitted to exclude

some measurements from the average provided the minimum of 5

independent measurements every 30 minutes are included: The Run

average of the FTIR CEM measurements depends on both the sample flow

rate and the measurement frequency (MF). The run average of the RM

using the integrated sampling method depends primarily on its

sampling rate. If the target analyte concentration fluctuates

significantly, the contribution to the run average of a large

fluctuation depends on the sampling rate and measurement frequency,

and on the duration and magnitude of the fluctuation. It is,

therefore, important to carefully select the sampling rate for both

the FTIR CEM and the RM and the measurement frequency for the FTIR

CEM. The minimum of 9 run averages can be compared according to the

relative accuracy test procedure in Performance Specification 2 for

SO2 and NOX CEMs (40 CFR part 60, Appendix B).

11.1.1.4.2 RMs Using a Grab Sampling Technique. Synchronize the

RM and FTIR CEM measurements as closely as possible. For a grab

sampling RM record the volume collected and the exact sampling

period for each sample. Synchronize the FTIR CEM so that the FTIR

measures a spectrum of a similar cell volume at the same time as the

RM grab sample was collected. Measure at least 5 independent samples

with both the FTIR CEM and the RM for each of the minimum 9 Runs.

Compare the Run concentration averages by using the relative

accuracy analysis procedure in 40 CFR part 60, Appendix B.

11.1.1.4.3 Continuous Emission Monitors (CEMs) as RMs. If the

RM is a CEM, synchronize the sampling flow rates of the RM and the

FTIR CEM. Each run is at least 1-hour long and consists of at least

10 FTIR CEM measurements and the corresponding 10 RM measurements

(or averages). For the statistical comparison use the relative

accuracy analysis procedure in 40 CFR part 60, Appendix B. If the RM

time constant is m--Mm--CS

Where

B=Bias at the spike level

Sm=Mean of the observed spiked sample concentrations

Mm=Mean of the observed unspiked sample concentrations

CS=Expected value of the spiked concentration. The CS is determined

by comparing the SF6 tracer concentration in undiluted

spike gas to the SF6 tracer concentrations in the spiked

samples;

[GRAPHIC] [TIFF OMITTED] TP27AU97.015

The expected concentration (CS) is the measured concentration of

the analyte in undiluted spike gas divided by the dilution factor

[GRAPHIC] [TIFF OMITTED] TP27AU97.016

where

[anal]dir=The analyte concentration in undiluted spike

gas measured directly by filling the FTIR cell with the spike gas.

If the bias is statistically significant (Section 12.2), Method 301

requires that a correction factor, CF, be multiplied by the

analytical results, and that 0.7 CF 1.3.

[GRAPHIC] [TIFF OMITTED] TP27AU97.017

12.2 Statistical Analysis of Validation Measurements. Arrange the

independent measurements (or measurement averages) as in Table 1.

More than 12 pairs of measurements can be analyzed. The statistical

analysis follows EPA Method 301, Section 6.3. Section 12.1 of this

performance specification shows the calculations for the bias,

expected spike concentration, and correction factor. This Sections

shows the determination of the statistical significance of the bias.

Determine the statistical significance of the bias at the 95 percent

confidence level by calculating the t-value for the set of

measurements. First, calculate the differences, di, for

each pair of spiked and each pair of unspiked measurements. Then

calculate the standard deviation of the spiked pairs of

measurements.

[GRAPHIC] [TIFF OMITTED] TP27AU97.018

Where

di=The differences between pairs of spiked measurements.

SDs=The standard deviation in the di values.

n=The number of spiked pairs, 2n=12 for the minimum of 12 spiked and

12 unspiked measurements.

Calculate the relative standard deviation, RSD, using

SDs and the mean of the spiked concentrations,

Sm. The RSD must be 50%.

[GRAPHIC] [TIFF OMITTED] TP27AU97.019

Repeat the calculations in equations 7 and 8 to determine

SDu and RSD, respectively, for the unspiked samples.

Calculate the standard deviation of the mean using

SDs and SDu from equation 7.

[GRAPHIC] [TIFF OMITTED] TP27AU97.020

The t-statistic is calculated as follows to test the bias for

statistical significance;

[GRAPHIC] [TIFF OMITTED] TP27AU97.021

Where the bias, B, and the correction factor, CF, are given in

Section 12.1.

For 11 degrees of freedom, and a one-tailed distribution, Method

301 requires that t 2.201. If the t-statistic indicates

the bias is statistically significant, then analytical measurements

must be multiplied by the correction factor. There is no limitation

on the number of measurements, but there must be at least 12

independent spiked and 12 independent unspiked measurements. Refer

to the t-distribution (Table 2) at the 95 percent confidence level

and appropriate degrees of freedom for the critical t-value.

13.0-15.0 [Reserved]

16.0 References.

1. Method 318, 40 CFR Part 63, Appendix A (Draft), ``Measurement

of Gaseous Formaldehyde, Phenol and Methanol Emissions by FTIR

Spectroscopy,'' EPA Contract No. 68D20163, Work Assignment 2-18,

February, 1995.

2. ``EPA Protocol for the Use of Extractive Fourier Transform

Infrared (FTIR) Spectrometry in Analyses of Gaseous Emissions from

Stationary Industrial Sources,'' February, 1995.

3. ``Measurement of Gaseous Organic and Inorganic Emissions by

Extractive FTIR Spectroscopy,'' EPA Contract No. 68-D2-0165, Work

Assignment 3-08.

4. ``Method 301--Field Validation of Pollutant Measurement

Methods from Various Waste Media,'' 40 Part CFR 63, Appendix A.

17.0 Tables, Diagrams, Flowcharts, and Validation Data.

Table 1.--Arrangement of Validation Measurements For Statistical Analysis.

--------------------------------------------------------------------------------------------------------------------------------------------------------

Measurement (or average) Time Spiked (ppm) di spiked Unspiked (ppm) di unspiked

--------------------------------------------------------------------------------------------------------------------------------------------------------

1................................... ........... S1 ........................ U1 .......................

2................................... ........... S2 S2-S1 U2 U2-U1

3................................... ........... S3 ........................ U3 .......................

4................................... ........... S4 S4-S3 U4 U4-U3

[[Page 45377]]

5................................... ........... S5 ........................ U5 .......................

6................................... ........... S6 S6-S5 U6 U6-U5

7................................... ........... S7 ........................ U7 .......................

8................................... ........... S8 S8-S7 U8 U8-U7

9................................... ........... S9 ........................ U9 .......................

10.................................. ........... S10 S10-S9 U10 U10-U9

11.................................. ........... S11 ........................ U11 .......................

12.................................. ........... S12 S12-S11 U12 U12-U11

Average->........................... ........... Sm ........................ Mm .......................

--------------------------------------------------------------------------------------------------------------------------------------------------------

Table 2.--t-Values

----------------------------------------------------------------------------------------------------------------

n-1a t-value n-1a t-value n-1a t-value n-1a t-value

----------------------------------------------------------------------------------------------------------------

11.......... 2.201 17 2.110 23 2.069 29 2.045

12.......... 2.179 18 2.101 24 2.064 30 2.042

13.......... 2.160 19 2.093 25 2.060 40 2.021

14.......... 2.145 20 2.086 26 2.056 60 2.000

15.......... 2.131 21 2.080 27 2.052 120 1.980

16.......... 2.120 22 2.074 28 2.048 1.960

----------------------------------------------------------------------------------------------------------------

(a) n is the number of independent pairs of measurements (a pair consists of one spiked and its corresponding

unspiked measurement). Either discreet (independent) measurements in a single run, or run averages can be

used.

[FR Doc. 97-22508 Filed 8-26-97; 8:45 am]

BILLING CODE 6560-50-P