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(continued)


Table B-4_Line Voltage and Room Temperature Test Conditions
------------------------------------------------------------------------
Line Room
Test day voltage,\1\ temperature,\2\ Comments
rms °C
------------------------------------------------------------------------
0................... 115 25 Initial set-up and
adjustments.
1................... 125 20
2................... 105 20
3................... 125 30 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
4................... 105 30
5................... 125 20
6................... 105 20 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
7................... 125 30 Examine test results
to ascertain if
further testing is
required.
8................... 105 30
9................... 125 20 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
10.................. 105 20
11.................. 125 30
12.................. 105 30 Adjustments and/or
periodic
maintenance
permitted at end of
tests.
13.................. 125 20
14.................. 105 20
15.................. 125 30
------------------------------------------------------------------------
\1\ Voltage specified shall be controlled to ±1 volt.
\2\ Temperature specified shall be controlled to ±1 °C.




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(9) Test procedure. (i) Arrange to generate pollutant test atmospheres as follows:



------------------------------------------------------------------------
Pollutant concentration
Test atmosphere (percent)
------------------------------------------------------------------------
A0........................................ Zero air.
A20....................................... 20±5 of the upper
range limit.
A30....................................... 30±5 of the upper
range limit.
A80....................................... 80±5 of the upper
range limit.
A90....................................... 90±5 of the upper
range limit.
------------------------------------------------------------------------


Test atmospheres A0, A20, and A80 shall be consistent during the tests and from day to day.

(ii) For steps (xxv) through (xxxi) of this section, a chart speed of at least 10 centimeters per hour shall be used. The actual chart speed, chart speed changes, and time checks shall be clearly marked on the chart.

(iii) Allow sufficient time for test analyzer to warm up and stabilize at a line voltage of 115 volts and a room temperature of 25 °C. Recalibrate, if necessary, and adjust the zero baseline to 5 percent of chart. No further adjustments shall be made to the analyzer until the end of the tests on the third day.

(iv) Measure test atmosphere A0 until a stable reading is obtained, and record this reading (in ppm) as Z'n, where n = 0 (see Figure B–4 in appendix A).

(v) Measure test atmosphere A20. Allow for a stable reading and record it as M'n, where n = 0.

(vi) Measure test atmosphere A80. Allow for a stable reading and record it as S'n, where n = 0.

(vii) The above readings for Z'0, M'0, and S'0 should be taken at least four (4) hours prior to the beginning of test day 1.

(viii) At the beginning of each test day, adjust the line voltage and room temperature to the values given in table B–4.

(ix) Measure test atmosphere A0 continuously for at least twelve (12) continuous hours during each test day.

(x) After the 12-hour zero drift test (step ix), sample test atmosphere A0. A stable reading is not required.

(xi) Measure test atmosphere A20 and record the stable reading (in ppm) as P1. (See Figure B–4 in appendix A.)

(xii) Sample test atmosphere A30; a stable reading is not required.

(xiii) Measure test atmosphere A20 and record the stable reading as P2.

(xiv) Sample test atmosphere A0; a stable reading is not required.

(xv) Measure test atmosphere A20 and record the stable reading as P3.

(xvi) Sample test atmosphere A30; a stable reading is not required.

(xvii) Measure test atmosphere A20 and record the stable reading as P4.

(xviii) Sample test atmosphere A0; a stable reading is not required.

(xix) Measure test atmosphere A20 and record the stable reading as P5.

(xx) Sample test atmosphere A30; a stable reading is not required.

(xxi) Measure test atmosphere A20 and record the stable reading as P6.

(xxii) Measure test atmosphere A30 and record the stable reading as P7.

(xxiii) Sample test atmosphere A90; a stable reading is not required.

(xxiv) Measure test atmosphere A80 and record the stable reading as P8. Increase chart speed to at least 10 centimeters per hour.

(xxv) Measure test atmosphere A0. Record the stable reading as L1.

(xxvi) Quickly switch the test analyzer to measure test atmosphere A80 and mark the recorder chart to show the exact time when the switch occurred.

(xxvii) Measure test atmosphere A90 and record the stable reading as P80.

(xxviii) Sample test atmosphere A90; a stable reading is not required.

(xxix) Measure test atmosphere A80 and record the stable reading as P10.

(xxx) Measure test atmosphere A0 and record the stable reading as L2.

(xxxi) Measure test atmosphere A80 and record the stable reading as P11.

(xxxii) Sample test atmosphere A90; a stable reading is not required.

(xxxiii) Measure test atmosphere A80 and record the stable reading as P12.

(xxxiv) Repeat steps (viii) through (xxxiii) of this section, each test day.

(xxxv) If zero and span adjustments are made after the readings are taken on test days 3, 6, 9, or 12, complete all adjustments; then measure test atmospheres A0, A80, and A20. Allow for a stable reading on each, and record the readings as Z'nS'n, and Mn respectively, where n = the test day number.

(10) Determine the results of each day's tests as follows. Mark the recorder chart to show readings and determinations.

(i) Zero drift. (A) 12-hour. Examine the strip chart pertaining to the 12-hour continuous zero air test. Determine the minimum (Cmin.) and maximum (Cmax.) readings (in p/m) during this period of 12 consecutive hours, extrapolating the calibration curve to negative concentration units if necessary. Determine the 12-hour zero drift (12ZD) as 12ZD = Cmax.-Cmin.. (See Figure B–5 in appendix A.)

(B) Calculate the 24-hour zero drift (24ZD) for the n-th test day as 24ZDn = Zn-Zn-1, or 24ZDn = Zn-Z'n-1 if zero adjustment was made on the previous day, where Zn = 1/2(L1+L2) for L1 and L2 taken on the n-th test day.

(C) Compare 12ZD and 24ZD to the zero drift specification in table B–1. Both 12ZD and 24ZD must be equal to or less than the specified value to pass the test for zero drift.

(ii) Span drift. (A) Span drift at 20 percent of URL (MSD)


If span adjustment was made on the previous day, where


n indicates the n-th test day, and i indicates the i-th reading on the n-th day.

(B) Span drift at 80 percent of URL (USD):


or


If span adjustment was made on the previous day, where


n indicates the n-th test day, and i indicates the i-th reading on the n-th test day.

(C) Both USD and MSD must be equal to or less than the respective specifications given in table B–1 to pass the test for span draft.

(iii) Lag time. Determine, from the strip chart, the elapsed time in minutes between the mark made in step (xxvi) and the first observable (two times the noise level) response. This time must be equal to or less than the time specified in table B–1 to pass the test for lag time.

(iv) Rise time. Calculate 95 percent of reading P9 and determine from the recorder chart, the elapsed time between the first observable (two times noise level) response and a response equal to 95 percent of the P9 reading. This time must be equal to or less than the rise time specified in table B–1 to pass the test for rise time.

(v) Fall time. Calculate five percent of (P10-L2) and determine, from the strip chart, the elapsed time in minutes between the first observable decrease in response following reading P10 and a response equal to five percent of (P10-L2). This time must be equal to or less than the fall time specification in table B–1 to pass the test for fall time.

(vi) Precision. Calculate precision (P20 and P80) for each day's test as follows:

(A)


(B)


(C) Both P20 and P80 must be equal to or less than the specification given in table B–1 to pass the test for precision.

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

Appendix A to Subpart B of Part 53—Optional Forms for Reporting Test Results
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Table B-5_Symbols and Abbreviations



BL............................ Analyzer reading at specified LDL
concentration.
Bz............................ Analyzer reading at 0 concentration for
LDL test.
DM............................ Digital meter.
Cmax.......................... Maximum analyzer reading during 12ZD
test.
Cmin.......................... Minimum analyzer reading during 12ZD
test.
i............................. Subscript indicating the i-th quantity
in a series.
IE............................ Interference equivalent.
L1............................ First analyzer zero reading for 24ZD
test.
L2............................ Second analyzer zero reading for 24ZD
test.
Mn............................ Average of P1 . . . P6 for the n-th test
day.
M[prime]n..................... Adjusted span reading at 20 percent of
URL on the n-th test day.
MSD........................... Span drift at 20 percent of URL.
n............................. Subscript indicating the test day
number.
P............................. Analyzer reading for precision test.
Pi............................ The i-th analyzer reading for precision
test.
P20........................... Precision at 20 percent of URL.
P80........................... Precision at 80 percent of URL.
R............................. Analyzer reading of pollutant alone for
IE test.
RI............................ Analyzer reading with interferent added
for IE test.
ri............................ The i-th DM reading for noise test.
S............................. Standard deviation of noise readings.
S0............................ Noise value (S) measured at 0
concentration.
S80........................... Noise value (S) measured at 80 percent
of URL.
Sn............................ Average of P7 . . . P12 for the n-th
test day.
S[prime]n..................... Adjusted span reading at 80 percent of
URL on the n-th test day.
URL........................... Upper range limit.
USD........................... Span drift at 80 percent o
Z............................. Average of L1 and L2.
Zn............................ Average of L1 and L2 on the n-th test
day.
Z[prime]n..................... Adjusted zero reading on the n-th test
day.
ZD............................ Zero drift.
12ZD.......................... 12-hour zero drift.
24ZD.......................... 24-hour zero drift.





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[40 FR 7049, Feb. 18, 1975, as amended at 40 FR 18169, Apr. 25, 1975]

Subpart C—Procedures for Determining Comparability Between Candidate Methods and Reference Methods
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Source: 62 FR 38792, July 18, 1997, unless otherwise noted.

§ 53.30 General provisions.
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(a) Determination of comparability. The test procedures prescribed in this subpart shall be used to determine if a candidate method is comparable to a reference method when both methods measure pollutant concentrations in ambient air.

(1) Comparability is shown for SO2, CO, O3, and NO2 methods when the differences between:

(i) Measurements made by a candidate manual method or by a test analyzer representative of a candidate automated method.

(ii) Measurements made simultaneously by a reference method, are less than or equal to the values specified in the last column of table C–1 of this subpart.

(2) Comparability is shown for lead methods when the differences between:

(i) Measurements made by a candidate method.

(ii) Measurements made by the reference method on simultaneously collected lead samples (or the same sample, if applicable), are less than or equal to the value specified in table C–3 of this subpart.

(3) Comparability is shown for PM10 and PM2.5 methods when the relationship between:

(i) Measurements made by a candidate method.

(ii) Measurements made by a reference method on simultaneously collected samples (or the same sample, if applicable) at each of two test sites, is such that the linear regression parameters (slope, intercept, and correlation coefficient) describing the relationship meet the values specified in table C–4 of this subpart.

(b) Selection of test sites—(1) All methods. Each test site shall be in a predominately urban area which can be shown to have at least moderate concentrations of various pollutants. The site shall be clearly identified and shall be justified as an appropriate test site with suitable supporting evidence such as maps, population density data, vehicular traffic data, emission inventories, pollutant measurements from previous years, concurrent pollutant measurements, and meteorological data. If approval of a proposed test site is desired prior to conducting the tests, a written request for approval of the test site or sites must be submitted prior to conducting the tests and must include the supporting and justification information required. The Administrator may exercise discretion in selecting a different site (or sites) for any additional tests the Administrator decides to conduct.

(2) Methods for SO2, CO, O3, and NO2. All test measurements are to be made at the same test site. If necessary, the concentration of pollutant in the sampled ambient air may be augmented with artificially generated pollutant to facilitate measurements in the specified ranges described under paragraph (d)(2) of this section.

(3) Methods for Pb. Test measurements may be made at any number of test sites. Augmentation of pollutant concentrations is not permitted, hence an appropriate test site or sites must be selected to provide lead concentrations in the specified range.

(4) Methods for PM10. Test measurements must be made, or derived from particulate samples collected, at not less than two test sites, each of which must be located in a geographical area characterized by ambient particulate matter that is significantly different in nature and composition from that at the other test site(s). Augmentation of pollutant concentrations is not permitted, hence appropriate test sites must be selected to provide PM10 concentrations in the specified range. The tests at the two sites may be conducted in different calendar seasons, if appropriate, to provide PM10 concentrations in the specified ranges.

(5) Methods for PM2.5. Augmentation of pollutant concentrations is not permitted, hence appropriate test sites must be selected to provide PM2.5 concentrations and PM2.5/PM10 ratios (if applicable) in the specified ranges.

(i) Where only one test site is required, as specified in table C–4 of this subpart, the site need only meet the PM2.5 ambient concentration levels required by §53.34(c)(3).

(ii) Where two sites are required, as specified in table C–4 of this subpart, each site must be selected to provide the ambient concentration levels required by §53.34(c)(3). In addition, one site must be selected such that all acceptable test sample sets, as defined in §53.34(c)(3), have a PM2.5/PM10 ratio of more than 0.75; the other site must be selected such that all acceptable test sample sets, as defined in §53.34(c)(3), have a PM2.5/PM10 ratio of less than 0.40. At least two reference method PM10 samplers shall be collocated with the candidate and reference method PM2.5 samplers and operated simultaneously with the other samplers at each test site to measure concurrent ambient concentrations of PM10 to determine the PM2.5/PM10 ratio for each sample set. The PM2.5/PM10 ratio for each sample set shall be the average of the PM2.5 concentration, as determined in §53.34(c)(1), divided by the average PM10 concentration, as measured by the PM10 samplers. The tests at the two sites may be conducted in different calendar seasons, if appropriate, to provide PM2.5 concentrations and PM2.5/PM10 ratios in the specified ranges.

(c) Test atmosphere. Ambient air sampled at an appropriate test site or sites shall be used for these tests. Simultaneous concentration measurements shall be made in each of the concentration ranges specified in tables C–1, C–3, or C–4 of this subpart, as appropriate.

(d) Sample collection—(1) All methods. All test concentration measurements or samples shall be taken in such a way that both the candidate method and the reference method receive air samples that are homogenous or as nearly identical as practical.

(2) Methods for SO2, CO, O3, and NO2. Ambient air shall be sampled from a common intake and distribution manifold designed to deliver homogenous air samples to both methods. Precautions shall be taken in the design and construction of this manifold to minimize the removal of particulates and trace gases, and to ensure that identical samples reach the two methods. If necessary, the concentration of pollutant in the sampled ambient air may be augmented with artificially-generated pollutant. However, at all times the air sample measured by the candidate and reference methods under test shall consist of not less than 80 percent ambient air by volume. Schematic drawings, physical illustrations, descriptions, and complete details of the manifold system and the augmentation system (if used) shall be submitted.

(3) Methods for Pb, PM10 and PM2.5. The ambient air intake points of all the candidate and reference method collocated samplers for lead, PM10 or PM2.5 shall be positioned at the same height above the ground level, and between 2 and 4 meters apart. The samplers shall be oriented in a manner that will minimize spatial and wind directional effects on sample collection.

(4) PM10 methods employing the same sampling procedure as the reference method but a different analytical method. Candidate methods for PM10 which employ a sampler and sample collection procedure that are identical to the sampler and sample collection procedure specified in the reference method, but use a different analytical procedure, may be tested by analyzing common samples. The common samples shall be collected according to the sample collection procedure specified by the reference method and shall be analyzed in accordance with the analytical procedures of both the candidate method and the reference method.

(e) Submission of test data and other information. All recorder charts, calibration data, records, test results, procedural descriptions and details, and other documentation obtained from (or pertinent to) these tests shall be identified, dated, signed by the analyst performing the test, and submitted. For candidate methods for PM2.5, all submitted information must meet the requirements of the ANSI/ASQC E4 Standard, sections 3.3.1, paragraphs 1 and 2 (reference 1 of appendix A of this subpart).

§ 53.31 Test conditions.
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(a) All methods. All test measurements made or test samples collected by means of a sample manifold as specified in §53.30(d)(2) shall be at a room temperature between 20 °C and 30 °C, and at a line voltage between 105 and 125 volts. All methods shall be calibrated as specified in paragraph (c) of this section prior to initiation of the tests.

(b) Samplers and automated methods. (1) Setup and start-up of the test analyzer, test sampler(s), and reference method (if applicable) shall be in strict accordance with the applicable operation manual(s). If the test analyzer does not have an integral strip chart or digital data recorder, connect the analyzer output to a suitable strip chart or digital data recorder. This recorder shall have a chart width of at least 25 centimeters, a response time of 1 second or less, a deadband of not more than 0.25 percent of full scale, and capability of either reading measurements at least 5 percent below zero or offsetting the zero by at least 5 percent. Digital data shall be recorded at appropriate time intervals such that trend plots similar to a strip chart recording may be constructed with a similar or suitable level of detail.

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

(3) Allow adequate warmup or stabilization time as indicated in the applicable operation manual(s) before beginning the tests.

(c) Calibration. The reference method shall be calibrated according to the appropriate appendix to part 50 of this chapter (if it is a manual method) or according to the applicable operation manual(s) (if it is an automated method). A candidate manual method (or portion thereof) shall be calibrated, according to the applicable operation manual(s), if such calibration is a part of the method.

(d) Range. (1) Except as provided in paragraph (d)(2) of this section, each method shall be operated in the range specified for the reference method in the appropriate appendix to part 50 of this chapter (for manual reference methods), or specified in table B–1 of subpart B of this part (for automated reference methods).

(2) For a candidate method having more than one selectable range, one range must be that specified in table B–1 of subpart B of this part and a test analyzer representative of the method must pass the tests required by this subpart while operated on that range. The tests may be repeated for a broader range (i.e., one extending to higher concentrations) than the one specified in table B–1 of subpart B of this part, provided that the range does not extend to concentrations more than two times the upper range limit specified in table B–1 of subpart B of this part and that the test analyzer has passed the tests required by subpart B of this part (if applicable) for the broader range. If the tests required by this subpart are conducted or passed only for the range specified in table B–1 of subpart B of this part, any 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. Appropriate test data shall be submitted for each range sought to be included in such a determination.

(e) Operation of automated methods. (1) Once the test analyzer has been set up and calibrated and tests started, manual adjustment or normal periodic maintenance as specified in the manual referred to in §53.4(b)(3) 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 manual adjustments were made and describe the operations performed.

(2) All test measurements shall be made with the same test analyzer; use of multiple test analyzers is not permitted. The test analyzer shall be operated continuously during the entire series of test measurements.

(3) If a test analyzer should malfunction during any of these tests, the entire set of measurements shall be repeated, and a detailed explanation of the malfunction, remedial action taken, and whether recalibration was necessary (along with all pertinent records and charts) shall be submitted.

§ 53.32 Test procedures for methods for SO2, CO, O3, and NO2.
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(a) Conduct the first set of simultaneous measurements with the candidate and reference methods:

(1) Table C–1 of this subpart specifies the type (1- or 24-hour) and number of measurements to be made in each of the three test concentration ranges.

(2) The pollutant concentration must fall within the specified range as measured by the reference method.

(3) The measurements shall be made in the sequence specified in table C–2 of this subpart, except for the 1-hour SO2 measurements, which are all in the high range.

(b) For each pair of measurements, determine the difference (discrepancy) between the candidate method measurement and reference method measurement. A discrepancy which exceeds the discrepancy specified in table C–1 of this subpart constitutes a failure. Figure C–1 of this subpart contains a suggested format for reporting the test results.

(c) The results of the first set of measurements shall be interpreted as follows:

(1) Zero failures. The candidate method passes the test for comparability.

(2) Three or more failures. The candidate method fails the test for comparability.

(3) One or two failures. Conduct a second set of simultaneous measurements as specified in table C–1 of this subpart. The results of the combined total of first-set and second-set measurements shall be interpreted as follows:

(i) One or two failures. The candidate method passes the test for comparability.

(ii) Three or more failures. The candidate method fails the test for comparability.

(4) For SO2, the 1-hour and 24-hour measurements shall be interpreted separately, and the candidate method must pass the tests for both 1- and 24-hour measurements to pass the test for comparability.

(d) A 1-hour measurement consists of the integral of the instantaneous concentration over a 60-minute continuous period divided by the time period. Integration of the instantaneous concentration may be performed by any appropriate means such as chemical, electronic, mechanical, visual judgment, or by calculating the mean of not less than 12 equally spaced instantaneous readings. Appropriate allowances or corrections shall be made in cases where significant errors could occur due to characteristic lag time or rise/fall time differences between the candidate and reference methods. Details of the means of integration and any corrections shall be submitted.

(e) A 24-hour measurement consists of the integral of the instantaneous concentration over a 24-hour continuous period divided by the time period. This integration may be performed by any appropriate means such as chemical, electronic, mechanical, or by calculating the mean of 24 sequential 1-hour measurements.

(f) For ozone and carbon monoxide, no more than six 1-hour measurements shall be made per day. For sulfur dioxide, no more than four 1-hour measurements or one 24-hour measurement shall be made per day. One-hour measurements may be made concurrently with 24-hour measurements if appropriate.

(g) For applicable methods, control or calibration checks may be performed once per day without adjusting the test analyzer or method. These checks may be used as a basis for a linear interpolation-type correction to be applied to the measurements to correct for drift. If such a correction is used, it shall be applied to all measurements made with the method, and the correction procedure shall become a part of the method.

§ 53.33 Test procedure for methods for lead.
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(a) Sample collection. Collect simultaneous 24-hour samples (filters) of lead at the test site or sites with both the reference and candidate methods until at least 10 filter pairs have been obtained. If the conditions of §53.30(d)(4) apply, collect at least 10 common samples (filters) in accordance with §53.30(d)(4) and divide each to form the filter pairs.

(b) Audit samples. Three audit samples must be obtained from the address given in §53.4(a). The audit samples are 3/4×8-inch glass fiber strips containing known amounts of lead at the following nominal levels: 100 µg/strip; 300 µg/strip; 750 µg/strip. The true amount of lead, in total µg/strip, will be provided with each audit sample.

(c) Filter analysis. (1) For both the reference method samples and the audit samples, analyze each filter extract three times in accordance with the reference method analytical procedure. The analysis of replicates should not be performed sequentially, i.e., a single sample should not be analyzed three times in sequence. Calculate the indicated lead concentrations for the reference method samples in µg/m 3 for each analysis of each filter. Calculate the indicated total lead amount for the audit samples in µg/strip for each analysis of each strip. Label these test results as R1A, R1B, R1C, R2A, R2B, ..., Q1A, Q1B, Q1C, ..., where R denotes results from the reference method samples; Q denotes results from the audit samples; 1, 2, 3 indicate the filter number, and A, B, C indicate the first, second, and third analysis of each filter, respectively.

(2) For the candidate method samples, analyze each sample filter or filter extract three times and calculate, in accordance with the candidate method, the indicated lead concentrates in µg/m 3 for each analysis of each filter. Label these test results as C1A, C1B, C2C, ..., where C denotes results from the candidate method. For candidate methods which provide a direct measurement of lead concentrations without a separable procedure, C1A = C1B = C1C, C2A = C2B = C2C, etc.

(d) Average lead concentration. For the reference method, calculate the average lead concentration for each filter by averaging the concentrations calculated from the three analyses:

Equation 1

where:

i is the filter number.


(e) Acceptable filter pairs. Disregard all filter pairs for which the lead concentration as determined in the previous paragraph (d) of this section by the average of the three reference method determinations, falls outside the range of 0.5 to 4.0 µg/m 3 . All remaining filter pairs must be subjected to both of the following tests for precision and comparability. At least five filter pairs must be within the 0.5 to 4.0 µg/m 3 range for the tests to be valid.

(f) Test for precision. (1) Calculate the precision (P) of the analysis (in percent) for each filter and for each method, as the maximum minus the minimum divided by the average of the three concentration values, as follows:

Equation 2
or

Equation 3

where:

i indicates the filter number.


(2) If any reference method precision value (PRi) exceeds 15 percent, the precision of the reference method analytical procedure is out of control. Corrective action must be taken to determine the source(s) of imprecision and the reference method determinations must be repeated according to paragraph (c) of this section, or the entire test procedure (starting with paragraph (a) of this section) must be repeated.

(3) If any candidate method precision value (PCi) exceeds 15 percent, the candidate method fails the precision test.

(4) The candidate method passes this test if all precision values (i.e., all PRi's and all PCi's) are less than 15 percent.

(g) Test for accuracy. (1)(i) For the audit samples calculate the average lead concentration for each strip by averaging the concentrations calculated from the three analyses:

Equation 4

where:

i is audit sample number.


(ii) Calculate the percent difference (Dq) between the indicated lead concentration for each audit sample and the true lead concentration (Tq) as follows:

Equation 5
(2) If any difference value (Dqi) exceeds ±5 percent, the accuracy of the reference method analytical procedure is out of control. Corrective action must be taken to determine the source of the error(s) (e.g., calibration standard discrepancies, extraction problems, etc.) and the reference method and audit sample determinations must be repeated according to paragraph (c) of this section, or the entire test procedure (starting with paragraph (a) of this section) must be repeated.

(h) Test for comparability. (1) For each filter pair, calculate all nine possible percent differences (D) between the reference and candidate methods, using all nine possible combinations of the three determinations (A, B, and C) for each method, as:

Equation 6

where:

i is the filter number, and n numbers from 1 to 9 for the nine possible difference combinations for the three determinations for each method (j = A, B, C, candidate; k = A, B, C, reference).


(2) If none of the percent differences (D) exceeds ±20 percent, the candidate method passes the test for comparability.

(3) If one or more of the percent differences (D) exceeds ±20 percent, the candidate method fails the test for comparability.

(i) The candidate method must pass both the precision test (paragraph (f) of this section) and the comparability test (paragraph (h) of this section) to qualify for designation as an equivalent method.

§ 53.34 Test procedure for methods for PM10 and PM2.5.
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(a) Collocated measurements. Set up three reference method samplers collocated with three candidate method samplers or analyzers at each of the number of test sites specified in table C–4 of this subpart. At each site, obtain as many sets of simultaneous PM10 or PM2.5 measurements as necessary (see paragraph (c)(3) of this section), each set consisting of three reference method and three candidate method measurements, all obtained simultaneously. For PM2.5 candidate Class II equivalent methods, at least two collocated PM10 reference method samplers are also required to obtain PM2.5/PM10 ratios for each sample set. Candidate PM10 method measurements shall be 24-hour integrated measurements; PM2.5 measurements may be either 24- or 48-hour integrated measurements. All collocated measurements in a sample set must cover the same 24- or 48-hour time period. For samplers, retrieve the samples promptly after sample collection and analyze each sample according to the reference method or candidate method, as appropriate, and determine the PM10 or PM2.5 concentration in µg/m 3 . If the conditions of §53.30(d)(4) apply, collect sample sets only with the three reference method samplers. Guidance for quality assurance procedures for PM2.5 methods is found in section 2.12 of the Quality Assurance Handbook (reference 6 of appendix A to subpart A of this part).

(b) Sequential samplers. For sequential samplers, the sampler shall be configured for the maximum number of sequential samples and shall be set for automatic collection of all samples sequentially such that the test samples are collected equally, to the extent possible, among all available sequential channels or utilizing the full available sequential capability.

(c) Test for comparability and precision. (1) For each of the measurement sets, calculate the average PM10 or PM2.5 concentration obtained with the reference method samplers:

Equation 7

where:

R denotes results from the reference method;

i is the sampler number; and

j is the set.


(2)(i) For each of the measurement sets, calculate the precision of the reference method PM10 or PM2.5 measurements as:

Equation 8
If the corresponding R j is below:


80 µg/m 3 for PM10 methods.

40 µg/m 3 for 24-hour PM2.5 at single test sites for Class I candidate methods.

40 µg/m 3 for 24-hour PM2.5 at sites having PM2.5/PM10 ratios >0.75.

30 µg/m 3 for 48-hour PM2.5 at single test sites for Class I candidate methods.

30 µg/m 3 for 48-hour PM2.5 at sites having PM2.5/PM10 ratios >0.75.

30 µg/m 3 for 24-hour PM2.5 at sites having PM2.5/PM10 ratios <0.40.

20 µg/m 3 for 48-hour PM2.5 at sites having PM2.5/PM10 ratios >0.75.


(ii) Otherwise, calculate the precision of the reference method PM10 or PM2.5 measurements as:

Equation 9
(3) If R j falls outside the acceptable concentration range specified in table C–4 of this subpart for any set, or if Pj RPj as applicable, exceeds the value specified in table C–4 of this subpart for any set, that set of measurements shall be discarded. For each site, table C–4 of this subpart specifies the minimum number of sample sets required for various conditions, and §53.30(b)(5) specifies the PM2.5/PM10 ratio requirements applicable to Class II candidate equivalent methods. Additional measurement sets shall be collected and analyzed, as necessary, to provide a minimum of 10 acceptable measurement sets for each test site. If more than 10 measurement sets are collected that meet the above criteria, all such measurement sets shall be used to demonstrate comparability.

(4) For each of the acceptable measurement sets, calculate the average PM10 or PM2.5 concentration obtained with the candidate method samplers:

Equation 10

where:

C denotes results from the candidate method;

i is the sampler number; and

j is the set.


(5) For each site, plot the average PM10 or PM2.5 measurements obtained with the candidate method (R j) against the corresponding average PM10 or PM2.5 measurements obtained with the reference method (R j). For each site, calculate and record the linear regression slope and intercept, and the correlation coefficient.

(6) If the linear regression parameters calculated under paragraph (c)(5) of this section meet the values specified in table C–4 of this subpart for all test sites, the candidate method passes the test for comparability.

[62 FR 38792, July 19, 1997; 63 FR 7714, Feb. 17, 1998]

Table C–1 to Subpart C of Part 53—Test Concentration Ranges, Number of Measurements Required, and Maximum Discrepancy Specification
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--------------------------------------------------------------------------------------------------------------------------------------------------------
Simultaneous Measurements Required Maximum
------------------------------------------------ Discrepancy
Pollutant Concentration Range Parts per Million 1-hr 24-hr Specification,
------------------------------------------------ Parts per
First Set Second Set First Set Second Set Million
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ozone...................................... Low 0.06 to 0.10......................... 5 6 .......... .......... 0.02
Med 0.15 to 0.25......................... 5 6 .......... .......... .03
High 0.35 to 0.45........................ 4 6 .......... .......... .04
-----------------------------------------------------------------
Total.................................. 14 18
=================================================================
Carbon Monoxide............................ Low 7 to 11.............................. 5 6 .......... .......... 1.5
Med 20 to 30............................. 5 6 .......... .......... 2.0
High 35 to 45............................ 4 6 .......... .......... 3.0
-----------------------------------------------------------------
Total.................................. 14 18
=================================================================
Sulfur Dioxide............................. Low 0.02 to 0.05......................... .......... .......... 3 3 0.02
Med 0.10 to 0.15......................... .......... .......... 2 3 .03
High 0.30 to 0.50........................ 7 8 2 2 .04
-----------------------------------------------------------------
Total................................. 7 8 7 8
=================================================================
Nitrogen Dioxide........................... Low 0.02 to 0.08......................... .......... .......... 3 3 0.02
Med 0.10 to 0.20......................... .......... .......... 2 3 .03
High 0.25 to 0.35........................ .......... .......... 2 2 .03
-----------------------------------------------------------------
Total.................................. .......... .......... 7 8
--------------------------------------------------------------------------------------------------------------------------------------------------------


Table C–2 to Subpart C of Part 53—Sequence of Test Measurements
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------------------------------------------------------------------------
Concentration Range
Measurement ---------------------------------
First Set Second Set
------------------------------------------------------------------------
1..................................... Low Medium
2..................................... High High
3..................................... Medium Low
4..................................... High High
5..................................... Low Medium
6..................................... Medium Low
7..................................... Low Medium
8..................................... Medium Low
9..................................... High High
10.................................... Medium Low
11.................................... High Medium
12.................................... Low High
13.................................... Medium Medium
14.................................... Low High
15.................................... ............... Low
16.................................... ............... Medium
17.................................... ............... Low
18.................................... ............... High
------------------------------------------------------------------------


Table C–3 to Subpart C of Part 53—Test Specifications for Lead Methods
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------------------------------------------------------------------------

------------------------------------------------------------------------
Concentration range, µg/m\3\............................ 0.5-4.0
Minimum number of 24-hr measurements.......................... 5
Maximum analytical precision, percent......................... 5
Maximum analytical accuracy, percent.......................... ±
5
Maximum difference, percent of reference method............... ±
20
------------------------------------------------------------------------


Table C–4 to Subpart C of Part 53—Test Specifications for PM10 and PM2.5 Methods
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------------------------------------------------------------------------
PM2.5
Specification PM10 -------------------------
Class I Class II
------------------------------------------------------------------------
Acceptable concentration range 30-300 10-200 10-200
(Rj), µg/m\3\.............
Minimum number of test sites..... 2 1 2
Number of candidate method 3 3 3
samplers per site...............
Number of reference method 3 3 3
samplers per site...............
Minimum number of acceptable
sample sets per site for PM10:
Rj < 80 µg/m\3\..... 3
Rj > 80 µg/m\3\..... 3
Total.................... 10
Minimum number of acceptable
sample sets per site for PM2.5:
Single test site for Class I
candidate equivalent
methods:
Rj < 40 µg/m\3\ ........... 3
for 24-hr or Rj < 30
µg/m\3\ for 48-hr
samples.................
Rj > 40 µg/m\3\ ........... 3
for 24-hr or Rj > 30
µg/m\3\ for 48-hr
samples.................
Sites at which the PM2.5/PM10
ratio must be > 0.75:
Rj < 40 µg/m\3\ ........... ........... 3
for 24-hr or Rj < 30
µg/m\3\ for 48-hr
samples.................
Rj > 40 µg/m\3\ ........... ........... 3
for 24-hr or Rj > 30
µg/m\3\ for 48-hr
samples.................
Sites at which the PM2.5/PM10
ratio must be < 0.40:
Rj < 30 µg/m\3\ ........... ........... 3
for 24-hr or Rj < 20
µg/m\3\ for 48-hr
samples.................
Rj > 30 µg/m\3\ ........... ........... 3
for 24-hr or Rj > 20
µg/m\3\ for 48-hr
samples.................
Total, each site................. ........... 10 10
Precision of replicate reference 5 µg/ 2 µg/ 2 µg/
method measurements, Pj or RPj m\3\ or 7% m\3\ or 5% m\3\ or 5%
respectively, maximum...........
Slope of regression relationship. 1±0. 1±0. 1±0.
1 05 05
Intercept of regression 0±5 0±1 0±1
relationship, µg/m\3\.....
Correlation of reference method >=0.97 >=0.97 >=0.97
and candidate method
measurements....................
------------------------------------------------------------------------


[62 FR 38792, July 18, 1997; 63 FR 7714, Feb. 17, 1998]

Figure C–1 to Subpart C of Part 53—Suggested Format for Reporting Test Results
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Candidate Method ________________________
Reference Method ________________________
Applicant _______________________
[squ] First Set [squ] Second Set [squ] Type [squ] 1 Hour [squ] 24 Hour
---------------------------------------------------------------------------------------------------------------- (continued)