Loading (50 kb)...'

(continued)

(3) Canceled designations will be deleted from the list maintained under §53.8(c). The requirements and procedures for cancellation set forth in §53.11 shall be inapplicable to cancellation of reference or equivalent method designations under this section.

(4) If the appendix to part 50 of this chapter in question is revised to specify a new measurement principle and calibration procedure on which the applicant's candidate method is based, the Administrator will take appropriate action under §53.5 to determine whether the candidate method is a reference method.

(5) Upon taking action under paragraph (e)(2) of this section, the Administrator will send notice of the action to all applicants for whose methods reference and equivalent method designations are canceled by such action.

(f) An applicant who has received notice of a determination under paragraph (d)(2) of this section may appeal the determination by taking one or more of the following actions:

(1) The applicant may submit new or additional information in support of the application.

(2) The applicant may request that the Administrator reconsider the data and information already submitted.

(3) The applicant may request that any test conducted by the Administrator that was a material factor in making the determination be repeated.

Table A–1 to Subpart A of Part 53—Summary of Applicable Requirements for Reference and Equivalent Methods for Air Monitoring of Criteria Pollutants
top


--------------------------------------------------------------------------------------------------------------------------------------------------------
Applicable Subparts of Part 53
Pollutant Ref. or Equivalent Manual or Automated Applicable Part -----------------------------------------------
50 Appendix A B C D E F
--------------------------------------------------------------------------------------------------------------------------------------------------------
SO2.................................. Reference.............. Manual................. A
Manual................. ....................... [bcheck] [bchec
k]
Equivalent............. Automated.............. ............... [bchec [bchec [bchec
k] k] k]
CO................................... Reference.............. Automated.............. C [bchec [bchec
k] k]
Manual................. ....................... [bcheck] ...... [bchec
k]
Equivalent............. Automated.............. ............... [bchec [bchec [bchec
k] k] k]
O3................................... Reference.............. Automated.............. D [bchec [bchec
k] k]
Manual................. ....................... [bcheck] ...... [bchec
k]
Equivalent............. Automated.............. ............... [bchec [bchec [bchec
k] k] k]
NO2.................................. Reference.............. Automated.............. F [bchec [bchec
k] k]
Manual................. ....................... [bcheck] ...... [bchec
k]
Equivalent............. Automated.............. ............... [bchec [bchec [bchec
k] k] k]
Pb................................... Reference.............. Manual................. G
Equivalent............. Manual................. ............... [bchec ...... [bchec
k] k]
PM10................................. Reference.............. Manual................. J [bchec ...... ...... [bchec
k] k]
Manual................. ....................... [bcheck] ...... [bchec [bchec
k] k]
Equivalent............. Automated.............. ............... [bchec ...... [bchec [bchec
k] k] k]
PM2.5................................ Reference.............. Manual................. L [bchec ...... ...... ...... [bchec
k] k]
Equivalent Class I..... Manual................. L [bchec ...... [bchec ...... [bchec
k] k] k]
Equivalent Class II.... Manual................. L [bchec ...... [bchec ...... [bchec [bchec
k] k] k] k]
Equivalent Class III... Manual or Automated.... ............... [bchec ...... [bchec ...... [bchec [bchec
k] k] \1\ k] \1\ k] \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Note: Because of the wide variety of potential devices possible, the specific requirements applicable to a Class III candidate equivalent method for
PM2.5 are not specified explicitly in this part but, instead, shall be determined on a case-by-case basis for each such candidate method.


Appendix A to Subpart A of Part 53—References
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(1) American National Standard Quality Systems-Model for Quality Assurance in Design, Development, Production, Installation, and Servicing, ANSI/ISO/ASQC Q9001-1994. Available from American Society for Quality Control, 611 East Wisconsin Avenue, Milwaukee, WI 53202.

(2) American National Standard—Specifications and Guidelines for Quality Systems for Environmental Data Collection and Environmental Technology Programs, ANSI/ASQC E41994. Available from American Society for Quality Control, 611 East Wisconsin Avenue, Milwaukee, WI 53202.

(3) Dimensioning and Tolerancing, ASME Y14.5M-1994. Available from the American Society of Mechanical Engineers, 345 East 47th Street, New York, NY 10017.

(4) Mathematical Definition of Dimensioning and Tolerancing Principles, ASME Y14.5.1M-1994. Available from the American Society of Mechanical Engineers, 345 East 47th Street, New York, NY 10017.

(5) ISO 10012, Quality Assurance Requirements for Measuring Equipment-Part 1: Meteorological confirmation system for measuring equipment):1992(E). Available from American Society for Quality Control, 611 East Wisconsin Avenue, Milwaukee, WI 53202.

(6) Copies of section 2.12 of the Quality Assurance Handbook for Air Pollution Measurement Systems, Volume II, Ambient Air Specific Methods, EPA/600/R-94/038b, are available from Department E (MD-77B), U.S. EPA, Research Triangle Park, NC 27711.

Subpart B—Procedures for Testing Performance Characteristics of Automated Methods SO2, CO, O3, and NO2
top
§ 53.20 General provisions.
top
(a) The test procedures given in this subpart shall be used to test the performance of candidate automated methods against the performance specifications given in table B–1. A test analyzer representative of the candidate automated method must exhibit performance better than, or equal to, the specified value for each such specification (except Range) to satisfy the requirements of this subpart. Except as provided in paragraph (b) of this section, the range of the candidate method must be the range specified in table B–1 to satisfy the requirements of this subpart.

(b) For a candidate method having more than one selectable range, one range must be that specified in table B–1 and a test analyzer representative of the method must pass the tests required by this subpart while operated in that range. The tests may be repeated for a broader range (i.e., one extending to higher concentrations) than that specified in table B–1 provided that the range does not extend to concentrations more than two times the upper range limit specified in table B–1. If the application is for a reference method determination, the tests may be repeated for a narrower range (one extending to lower concentrations) than that specified in table B–1.

If the tests are conducted or passed only for the specified range, any reference or equivalent method determination with respect to the method will be limited to that range. If the tests are passed for both the specified range and a broader range (or ranges), any such determination will include the broader range(s) as well as the specified range, provided that the tests required by subpart C of this part (if applicable) are met for the broader range(s). If the tests are passed for both the specified range and a narrower range, a reference method determination for the method will include the narrower range as well as the specified range. Appropriate test data shall be submitted for each range sought to be included in a reference or equivalent method determination under this paragraph (b).

(c) For each performance specification (except Range), the test procedure shall be initially repeated seven (7) times to yield 7 test results. Each result shall be compared with the corresponding specification in table B–1; a value higher than or outside that specified constitutes a failure. These 7 results for each parameter shall be interpreted as follows:

(1) Zero (0) failures: Candidate method passes the performance parameter.

(2) Three (3) or more failures: Candidate method fails the performance parameter.

(3) One (1) or two (2) failures: Repeat the test procedures for the parameter eight (8) additional times yielding a total of fifteen (15) test results. The combined total of 15 test results shall then be interpreted as follows:

(i) One (1) or two (2) failures: Candidate method passes the performance parameter.

(ii) Three (3) or more failures: Candidate method fails the performance parameter.


Table B-1_Performance Specifications for Automated Methods
----------------------------------------------------------------------------------------------------------------
Sulfur Photochemical Carbon Nitrogen Definitions and
Performance parameter Units \1\ dioxide oxidants monoxide dioxide test procedures
----------------------------------------------------------------------------------------------------------------
1. Range..................... Parts per 0-0.5 0-0.5 0-50 0-0.5 Sec. 53.23(a).
million.
2. Noise..................... ......do........ .005 .005 .50 .005 Sec. 53.23(b).
3. Lower detectable limit.... Parts per .01 .01 1.0 .01 Sec. 53.23(c).
million.
4. Interference equivalent... ................ ......... ............. ......... ......... Sec. 53.23(d).
Each interferant........... Parts per ±. ±.02 ±1 ±0
million. 02 .0 .02
Total interferant.......... ......do........ .06 .06 1.5 .04
5. Zero drift, 12 and 24 hour ......do........ ±. ±.02 ±1 ±. Sec. 52.23(e).
02 .0 02
6. Span drift, 24 hour....... ................ ......... ............. ......... ......... Do.
20 percent of upper range Percent......... ±2 ±20.0 ±1 ±2
limit. 0.0 0.0 0.0
80 percent of upper range ......do........ ±5 ±5.0 ±2 ±5
limit. .0 .5 .0
7. Lag time.................. Minutes......... 20 20 10 20 Do.
8. Rise time................. ......do........ 15 15 5 15 Do.
9. Fall time................. ......do........ 15 15 5 15 Do.
10. Precision................ ................ ......... ............. ......... ......... Do.
20 percent of upper range Parts per .01 .01 .5 .02
limit. million.
80 percent of upper range ......do........ .015 .01 .5 .03
limit.
----------------------------------------------------------------------------------------------------------------
\1\ To convert from parts per million to µg/m \3\ at 25 °C and 760 mm Hg, multiply by M/0.02447, where
M is the molecular weight of the gas.


(d) The tests for zero drift, span drift, lag time, rise time, fall time, and precision shall be combined into a single sequential procedure to be conducted at various line voltages and ambient temperatures specified in §53.23(e). The tests for noise, lower detectable limit, and interference equivalents shall be made at any temperature between 20 °C. and 30 °C. and at any normal line voltage between 105 and 125 volts, and shall be conducted such that not more than three (3) test results for each parameter are obtained per 24 hours.

(e) All response readings to be recorded shall first be converted to concentration units according to the calibration curve constructed in accordance with §53.21(b).

(f) All recorder chart tracings, records, test data and other documentation obtained from or pertinent to these tests shall be identified, dated, signed by the analyst performing the test, and submitted.

Note: Suggested formats for reporting the test results and calculations are provided in Figures B–2, B–3, B–4, B–5, and B–6 in appendix A. Symbols and abbreviations used in this subpart are listed in table B–5, appendix A.

[40 FR 7049, Feb. 18, 1975, as amended at 40 FR 18168, Apr. 25, 1975; 41 FR 52694, Dec. 1, 1976]

§ 53.21 Test conditions.
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(a) Set-up and start-up of the test analyzer shall be in strict accordance with the operating instructions specified in the manual referred to in §53.4(b)(3). Allow adequate warm-up or stabilization time as indicated in the operating instructions before beginning the tests. If the candidate method does not include an integral strip chart recorder, connect the output signal of the test analyzer to a suitable strip chart recorder of the servo, null-balance type. This recorder shall have a chart width of at least 25 centimeters, chart speeds up to 10 cm per hour, a response time of 1 second or less, a deadband of not more than 0.25 percent of full scale, and capability either of reading measurements at least 5 percent below zero or of offsetting the zero by at least 5 percent.

Note: Other data acquisition components may be used along with the chart recorder during conduct of these tests. Use of the chart recorder is intended only to facilitate evaluation of data submitted.

(b) Calibration of the test analyzer shall be as indicated in the manual referred to in §53.4(b)(3) and as follows: If the chart recorder does not have below zero capability, adjust either the controls of the test analyzer or the chart recorder to obtain a +5% offset zero reading on the recorder chart to facilitate observing negative response or drift. If the candidate method is not capable of negative response, the test analyzer (not recorder) shall be operated with an offset zero. Construct and submit a calibration curve showing a plot of recorder scale readings (ordinate) against pollutant concentrations (abscissa). A plot of output units (volts, millivolts, milliamps, etc.) against pollutant concentrations shall also be shown for methods not including an integral chart recorder. All such plots shall consist of at least seven (7) approximately equally spaced, identifiable points, including 0 and 90±5 percent of full scale.

(c) Once the test analyzer has been set up and calibrated and the tests started, manual adjustment or normal periodic maintenance is permitted only every 3 days. Automatic adjustments which the test analyzer performs by itself are permitted at any time. The submitted records shall show clearly when any manual adjustment or periodic maintenance was made and describe the operations performed.

(d) If the test analyzer should malfunction during any of the performance tests, the tests for that parameter shall be repeated. A detailed explanation of the malfunction, remedial action taken, and whether recalibration was necessary (along with all pertinent records and charts) shall be submitted. If more than one malfunction occurs, all performance test procedures for all parameters shall be repeated.

(e) Tests for all performance parameters shall be completed on the same test analyzer, except that use of multiple test analyzers to accelerate testing will be permitted when alternate ranges of a multi-range candidate method are being tested.

§ 53.22 Generation of test atmospheres.
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(a) Table B–2 specifies preferred methods for generating test atmospheres and suggested methods of verifying the concentrations. Only one means of establishing the concentration of a test atmosphere is normally required. If the method of generation can produce reproducible concentrations, verification is optional. If the method of generation is not reproducible, then establishment of the concentration by some verification method is required. However, when a method of generation other than that given in table B–2 is used, the test concentration shall be verified.

(b) The test atmosphere delivery system shall be designed and constructed so as not to significantly alter the test atmosphere composition or concentration during the period of the test. The delivery system shall be fabricated from borosilicate glass or FEP Teflon.

(c) The output of the test atmosphere generation system shall be sufficiently stable to obtain stable response during the required tests. If a permeation device is used for generation of a test atmosphere, the device, as well as the air passing over it, shall be controlled to ±0.1 °C.

(d) All diluent air shall be zero air free of contaminants likely to cause a detectable response on the test analyzer.


Table B-2_Test Atmospheres
----------------------------------------------------------------------------------------------------------------
Test gas Generation Verification
----------------------------------------------------------------------------------------------------------------
Ammonia............................... Permeation device. Similar to Indophenol method, reference 3.
system described in references 1
and 2.
Carbon dioxide........................ Cylinder of zero air or nitrogen Use NBS-certified standards whenever
containing CO2 as required to possible. If NBS standards are not
obtain the concentration available, obtain 2 standards from
specified in table B-3. independent sources which agree
within 2 percent; or obtain one
standard and submit it to an
independent laboratory for analysis
which must agree within 2 percent of
the supplier's nominal analysis.
Carbon monoxide....................... Cylinder of zero air or nitrogen Do.
containing CO as required to
obtain the concentration
specified in table B-3.
Ethane................................ Cylinder of zero air or nitrogen Do.
containing ethane as required to
obtain the concentration
specified in table B-3.
Ethylene.............................. Cylinder of prepurified nitrogen Do.
containing ethylene as required
to obtain the concentration
specified in table B-3.
Hydrogen chloride..................... Cylinder \1\ of prepurified Collect samples in bubbler containing
nitrogen containing distilled water and analyze by the
approximately 100 p/m of gaseous mercuric thiocyanate method, ASTM
HCl. Dilute with zero air to (D512), p. 29, reference 4.
concentration specified in table
B-3.
Hydrogen sulfide...................... Permeation device system Tentative method of analysis for H2 S
described in references 1 and 2. content of the atmosphere, p. 426,
reference 5.
Methane............................... Cylinder of zero air containing Use NBS-certified standards whenever
methane as required to obtain possible. If NBS standards are not
the concentration specified in available, obtain 2 standards from
table B-3. independent sources which agree
within 2 percent; or obtain one
standard and submit it to an
independent laboratory for an
analysis which must agree within 2
percent of the supplier's nominal
analysis.
Nitric oxide.......................... Cylinder \1\ of prepurified Gas-phase titration as described in
nitrogen containing reference 6, section 7.1.
approximately 100 p/m NO. Dilute
with zero air to required
concentration.
Nitrogen dioxide...................... 1. Gas phase titration as 1. Use an NO 2 analyzer calibrated
described in reference 6. with a gravimetrically calibrated
2. Permeation device, similar to permeation device.
system described in references 1 2. Use an NO 2 analyzer calibrated by
and 2. gas-phase titration as described in
reference 6.
Ozone................................. Calibrated ozone generator as Use an ozone analyzer calibrated by
described in reference 7, gas-phase titration as described in
appendix D. reference 6.
Sulfur dioxide........................ Permeation device Similar to P-rosaniline method. Reference 7,
system described in reference appendix A.
method for SO2, reference 7,
appendix A.
Water................................. Pass zero air through distilled Measure relative humidity by means of
water at a fixed known a dew-point indicator, calibrated
temperature between 20° and electrolytic or piezo electric
30 °C. such that the air hygrometer, or wet/dry bulb
stream becomes saturated. Dilute thermometer.
with zero air to concentration
specified in table B-3.
Xylene................................ Cylinder of prepurified nitrogen Use NBS-certified standards whenever
containing 100 p/m xylene. possible. If NBS standards are not
Dilute with zero air to available, obtain 2 standards from
concentration specified in table independent sources which agree
B-3. within 2 percent; or obtain one
standard and submit it to an
independent laboratory for an
analysis which must agree within 2
percent of the supplier's nominal
analysis.
Zero air.............................. 1. Ambient air purified by
appropriate scrubbers or other
devices such that it is free of
contaminants likely to cause a
detectable response on the
analyzer.
2. Cylinder of compressed zero
air certified by the supplier or
an independent laboratory to be
free of contaminants likely to
cause a detectable response on
the analyzer.
----------------------------------------------------------------------------------------------------------------
\1\ Use stainless steel pressure regulator dedicated to the pollutant measured.
Reference 1. O'Keeffe, A. E., and Ortaman, G. C. ``Primary Standards for Trace Gas Analysis,'' Anal. Chem. 38,
760 (1966).
Reference 2. Scaringelli, F. P., A. E., Rosenberg, E., and Bell, J. P., ``Primary Standards for Trace Gas
Analysis.'' Anal. Chem. 42, 871 (1970).
Reference 3. ``Tentative Method of Analysis for Ammonia in the Atmosphere (Indophenol Method)'', Health Lab
Sciences, vol. 10, No. 2, 115-118, April 1973.
Reference 4. 1973 Annual Book of ASTM Standards, American Society for Testing and Materials, 1916 Race St.,
Philadelphia, PA.
Reference 5. Methods for Air Sampling and Analysis, Intersociety Committee, 1972, American Public Health
Association, 1015.
Reference 6. Federal Register, vol. 38, No. 110, Tentative Method for the Continuous Measurement of Nitrogen
Dioxide (Chemiluminescent) addenda C. (June 8, 1973).
Reference 7. Federal Register, vol. 36, No. 228, National Primary and Secondary Ambient Air Quality Standards,
Nov. 25, 1971.


(e) The concentration of each test atmosphere shall be established and/or verified before or during each series of tests. Samples for verifying test concentrations shall be collected from the test atmosphere delivery system as close as possible to the sample intake port of the test analyzer.

(f) The accuracy of all flow measurements used to calculate test atmosphere concentrations shall be documented and referenced to a primary standard (such as a spirometer, bubble meter, etc.). Any corrections shall be clearly shown. All flow measurements given in volume units shall be standardized to 25 °C. and 760 mm Hg.

(g) Schematic drawings and other information showing complete procedural details of the test atmosphere generation, verification, and delivery system shall be provided. All pertinent calculations shall be clearly indicated.

[40 FR 7049, Feb. 18, 1975, as amended at 40 FR 18168, Apr. 25, 1975]

§ 53.23 Test procedures.
top
(a) Range—(1) Technical definition. Nominal minimum and maximum concentrations which a method is capable of measuring.

Note: The nominal range is specified at the lower and upper range limits in concentration units, for example, 0–0.5 p/m.

(2) Test procedure. Submit a suitable calibration curve, as specified in §53.21(b), showing the test analyzer's response over at least 95 percent of the required range.

Note: A single calibration curve will normally suffice.

(b) Noise—(1) Technical definition. Spontaneous, short duration deviations in output, about the mean output, which are not caused by input concentration changes. Noise is determined as the standard deviation about the mean and is expressed in concentration units.

(2) Test procedure. (i) Allow sufficient time for the test analyzer to warm up and stabilize. Determine at two concentrations, first using zero air and then a pollutant test gas concentration as indicated below. The noise specification in table B–1 shall apply to both of these tests.

(ii) Connect an integrating-type digital meter (DM) suitable for the test analyzer's output and accurate to three significant digits, to measure the analyzer's output signal.

Note: Use of a chart recorder in addition to the DM is optional.

(iii) Measure zero air for 60 minutes. During this 60-minute interval, record twenty-five (25) readings at 2-minute intervals. (See Figure B–2 in appendix A.)

(iv) Convert each DM reading to concentration units (p/m) by reference to the test analyzer's calibration curve as determined in §53.21(b). Label the converted DM readings r1, r2, r3 . . . ri . . . r25.

(v) Calculate the standard deviation, S, as follows:



where i indicates the i-th DM reading in ppm.


(vi) Let S at 0 ppm be identified as So; compare So to the noise specification given in table B–1.

(vii) Repeat steps (iii) through (vi) of this section using a pollutant test atmosphere concentration of 80±5 percent of the upper range limit (URL) instead of zero gas, and let S at 80 percent of the URL be identified as S80. Compare S80 to the noise specification given in table B–1.

(viii) Both S0 and S80 must be less than or equal to the specification for noise to pass the test for the noise parameter.

(c) Lower detectable limit—(1) Technical definition. The minimum pollutant concentration which produces a signal of twice the noise level.

(2) Test procedure. (i) Allow sufficient time for the test analyzer to warm up and stabilize. Measure zero air and record the stable reading in ppm as BZ. (See Figure B–3 in appendix A.)

(ii) Generate and measure a pollutant test atmosphere concentration equal to the value for the lower detectable limit specified in table B–1.

Note: If necessary, the test atmosphere concentration may be generated or verified at a higher concentration, then accurately diluted with zero air to the final required concentration.

(iii) Record the test analyzer's stable indicated reading, in ppm, as BL.

(iv) Determine the Lower Detectable Limit (LDL) as LDL = BL-BZ. Compare this LDL value with the noise level, S0, determined in §53.23(b), for 0 concentration test atmosphere. LDL must be equal to or higher than 2S0 to pass this test.

(d) Interference equivalent—(1) Technical definition. Positive or negative response caused by a substance other than the one being measured.

(2) Test procedure. The test analyzer shall be tested for all substances likely to cause a detectable response. The test analyzer shall be challenged, in turn, with each interfering agent specified in table B–3. In the event that there are substances likely to cause a significant interference which have not been specified in table B–3, these substances shall be tested at a concentration substantially higher than that normally found in the ambient air. The interference may be either positive or negative, depending on whether the test analyzer's response is increased or decreased by the presence of the interferent. Interference equivalents shall be determined by mixing each interferent, one at a time, with the pollutant at the concentrations specified in table B–3, and comparing the test analyzer's response to the response caused by the pollutant alone. Known gas-phase reactions that might occur between an interferent and the pollutant are designated by footnote 3 in table B–3. In these cases, the interference equivalent shall be determined in the absence of the pollutant.

(i) Allow sufficient time for warm-up and stabilization of the test analyzer.

(ii) For a candidate method using a prefilter or scrubber based upon a chemical reaction to derive part of its specificity, and which requires periodic service or maintenance, the test analyzer shall be “conditioned” prior to each interference test as follows:


Table B-3_Interferant Test Concentration,\1\ Parts Per Million
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Hydrochloric Hydrogen Sulfur Nitrogen Nitric Carbon M- Water Carbon
Pollutant Analyzer type \2\ acid Ammonia sulfide dioxide dioxide oxide dioxide Ethylene Ozone xylene vapor monoxide Methane Ethane
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
SO2..................... Flame photometric (FPD)..... ............ ....... 0.1 \1\ 0.14 ........ ....... 750 ........ ....... ....... \3\ 50 ....... .......
20,000
SO2..................... Gas chromatography (FPD).... ............ ....... .1 \4\.14 ........ ....... 750 ........ ....... ....... \3\ 50 ....... .......
20,000
SO2..................... Spectrophotometric-wet 0.2 \3\ 0.1 .1 \4\.14 0.5 ....... 750 ........ 0.5 ....... ........ ........ ....... .......
chemical (pararosaniline
reaction).
SO2..................... Electrochemical............. .2 \3\.1 .1 \4\.14 .5 0.5 ........ 0.2 .5 ....... \3\ ........ ....... .......
20,000
SO2..................... Conductivity................ .2 \3\.1 ........ \4\.14 .5 ....... 750 ........ ....... ....... ........ ........ ....... .......
SO2..................... Spectrophotometric-gas phase ............ ....... ........ \4\.14 .5 .5 ........ ........ .5 0.2 ........ ........ ....... .......
O3...................... Chemiluminescent............ ............ ....... \3\.1 ........ ........ ....... 750 ........ \4\.08 ....... \3\ ........ ....... .......
20,000
O3...................... Electrochemical............. ............ \3\.1 ........ .5 .5 ....... ........ ........ \4\.08 ....... \3\ ........ ....... .......
20,000
O3...................... Spectrophotometric-wet ............ \3\.1 ........ .5 .5 \3\.5 ........ ........ \4\.08 ....... ........ ........ ....... .......
chemical (potassium iodide
reaction).
O3...................... Spectrophotometric-gas phase ............ ....... ........ .5 .5 \3\.5 ........ ........ \4\.08 ....... ........ ........ ....... .......
CO...................... Infrared.................... ............ ....... ........ ........ ........ ....... 750 ........ ....... ....... 20,000 \4\ 10 ....... .......
CO...................... Gas chromatography with ............ ....... ........ ........ ........ ....... ........ ........ ....... ....... 20,000 \4\ 10 ....... 0.5
flame ionization detector.
CO...................... Electrochemical............. ............ ....... ........ ........ ........ .5 ........ .2 ....... ....... 20,000 \4\ 10 ....... .......
CO...................... Catalytic combustion-thermal ............ .1 ........ ........ ........ ....... 750 .2 ....... ....... 20,000 \4\ 10 5.0 .5
detection.
CO...................... IR fluorescence............. ............ ....... ........ ........ ........ ....... 750 ........ ....... ....... 20,000 \4\ 10 ....... .5
CO...................... Mercury replacement UV ............ ....... ........ ........ ........ ....... ........ .2 ....... ....... ........ \4\ 10 ....... .5
photometric.
NO2..................... Chemiluminescent............ ............ \3\.1 ........ .5 \4\.1 .5 ........ ........ ....... ....... 20,000 ........ ....... .......
NO2..................... Spectrophotometric-wet ............ ....... ........ .5 \4\.1 .5 750 ........ .5 ....... ........ ........ ....... .......
chemical (azo-dye reaction).
NO2..................... Electrochemical............. 0.2 \3\.1 ........ .5 \4\.1 .5 750 ........ .5 ....... 20,000 50 ....... .......
NO2..................... Spectrophotometric-gas phase ............ \3\.1 ........ .5 \4\.1 .5 ........ ........ .5 ....... 20,000 50 ....... .......
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Concentrations of interferant listed must be prepared and controlled to ±10 percent of the state value.
\2\ Analyzer types not listed will be considered by the administrator as special cases.
\3\ Do not mix with pollutant.
\4\ Concentration of pollutant used for test. These pollutant concentrations must be prepared to ±10 percent of the stated value.


(A) Service or perform the indicated maintenance on the scrubber or prefilter as directed in the manual referred to in §53.4(b)(3).

(B) Before testing for each interferent, allow the test analyzer to sample through the scrubber a test atmosphere containing the interferent at a concentration equal to the value specified in table B–3. Sampling shall be at the normal flow rate and shall be continued for 6 continuous hours prior to testing.

(iii) Generate three test atmosphere streams as follows:

(A) Test atmosphere P: Pollutant concentration.

(B) Test atmosphere I: Interference concentration.

(C) Test atmosphere Z: Zero air.

(iv) Adjust the individual flow rates and the pollutant or interferent generators for the three test atmospheres as follows:

(A) The flow rates of test atmospheres I and Z shall be identical.

(B) The concentration of pollutant in test atmosphere P shall be adjusted such that when P is mixed (diluted) with either test atmosphere I or Z, the resulting concentration of pollutant shall be as specified in table B–3.

(C) The concentration of interferent in test atmosphere I shall be adjusted such that when I is mixed (diluted) with test atmosphere P, the resulting concentration of interferent shall be equal to the value specified in table B–3.

(D) To minimize concentration errors due to flow rate differences between I and Z, it is recommended that, when possible, the flow rate of P be from 10 to 20 times larger than the flow rates of I and Z.

(v) Mix test atmospheres P and Z by passing the total flow of both atmospheres through a mixing flask.

(vi) Sample and measure the mixture of test atmospheres P and Z with the test analyzer. Allow for a stable reading, and record the reading, in concentration units, as R (see Figure B–3).

(vii) Mix test atmospheres P and I by passing the total flow of both atmospheres through a mixing flask.

(viii) Sample and measure this mixture. Record the stable reading, in concentration units, as RI.

(ix) Calculate the interference equivalent (IE) as:

IE = RI-R

IE must be equal to or less than the specification given in table B–1 for each interferent to pass the test.

(x) Follow steps (iii) through (ix) of this section, in turn, to determine the interference equivalent for each interferent.

(xi) For those interferents which cannot be mixed with the pollutant, as indicated by footnote (3) in table B–3, adjust the concentration of test atmosphere I to the specified value without being mixed or diluted by the pollutant test atmosphere. Determine IE as follows:

(A) Sample and measure test atmosphere Z (zero air). Allow for a stable reading and record the reading, in concentration units, as R.

(B) Sample and measure the interferent test atmosphere I. If the test analyzer is not capable of negative readings, adjust the analyzer (not the recorder) to give an offset zero. Record the stable reading in concentration units as RI, extrapolating the calibration curve, if necessary, to represent negative readings.

(C) Calculate IE=RI-R. IE must be equal to or less than the specification in table B–1 to pass the test.

(xii) Sum the absolute value of all the individual interference equivalents. This sum must be equal to or less than the total interferent specification given in table B–1 to pass the test.

(e) Zero drift, span drift, lag time, rise time, fall time, and precision—(1) Technical definitions—(i) Zero drift: The change in response to zero pollutant concentration, over 12- and 24-hour periods of continuous unadjusted operation.

(ii) Span drift: The percent change in response to an up-scale pollutant concentration over a 24-hour period of continuous unadjusted operation.

(iii) Lag time: The time interval between a step change in input concentration and the first observable corresponding change in response.

(iv) Rise time: The time interval between initial response and 95 percent of final response after a step increase in input concentration.

(v) Fall time: The time interval between initial response and 95 percent of final response after a step decrease in input concentration.

(vi) Precision: Variation about the mean of repeated measurements of the same pollutant concentration, expressed as one standard deviation about the mean.

(2) Tests for these performance parameters shall be accomplished over a period of seven (7) or more days. During this time, the line voltage supplied to the test analyzer and the ambient temperature surrounding the analyzer shall be varied from day to day. One test result for each performance parameter shall be obtained each test day, for seven (7) or fifteen (15) test days as necessary. The tests are performed sequentially in a single procedure.

(3) The 24-hour test day may begin at any clock hour. The first 12 hours out of each test day are required for testing 12-hour zero drift. Tests for the other parameters shall be conducted during the remaining 12 hours.

(4) Table B–4 specifies the line voltage and room temperature to be used for each test day. The line voltage and temperature shall be changed to the specified values at the start of each test day (i.e., at the start of the 12-hour zero test). Initial adjustments (day zero) shall be made at a line voltage of 115 volts (rms) and a room temperature of 25 °C.

(5) The tests shall be conducted in blocks consisting of 3 test days each until 7 or 15 test results have been obtained. (The final block may contain fewer than three test days.) If a test is interrupted by an occurrence other than a malfunction of the test analyzer, only the block during which the interruption occurred shall be repeated.

(6) During each block, manual adjustments to the electronics, gas, or reagent flows or periodic maintenance shall not be permitted. Automatic adjustments which the test analyzer performs by itself are permitted at any time.

(7) At least 4 hours prior to the start of the first test day of each block, the test analyzer may be adjusted and/or serviced according to the periodic maintenance procedures specified in the manual referred to in §53.4(b)(3). If a new block is to immediately follow a previous block, such adjustments or servicing may be done immediately after completion of the day's tests for the last day of the previous block and at the voltage and temperature specified for that day, but only on test days 3, 6, 9, and 12.

Note: If necessary, the beginning of the test days succeeding such maintenance or adjustment may be delayed as necessary to complete the service or adjustment operation.

(8) All response readings to be recorded shall first be converted to concentration units according to the calibration curve. Whenever a test atmosphere is to be measured but a stable reading is not required, the test atmosphere shall be measured long enough to cause a change in response of at least 10% of full scale. Identify all readings and other pertinent data on the strip chart. (See Figure B–1 illustrating the pattern of the required readings.) (continued)