# 40 CFR § 60.106 - Test methods and procedures.

§ 60.106 Test methods and procedures.

(a) In conducting the performance tests required in § 60.8, the owner or operator shall use as reference methods and procedures the test methods in appendix A of this part or other methods and procedures as specified in this section, except as provided in § 60.8(b).

(b) The owner or operator shall determine compliance with the particulate matter (PM) standards in § 60.102(a) as follows:

(1) The emission rate (E) of PM shall be computed for each run using the following equation:

$E=\frac{c,{Q}_{\mathrm{rd}}}{{\mathrm{KR}}_{c}}$

Where:
E = Emission rate of PM, kg/Mg (lb/ton) of coke burn-off.
cs = Concentration of PM, g/dscm (gr/dscf).
Qsd = Volumetric flow rate of effluent gas, dscm/hr (dscf/hr).
Rc = Coke burn-off rate, Mg/hr (ton/hr) coke.
K = Conversion factor, 1,000 g/kg (7,000 gr/lb).

(2) Method 5B or 5F is to be used to determine particulate matter emissions and associated moisture content from affected facilities without wet FGD systems; only Method 5B is to be used after wet FGD systems. The sampling time for each run shall be at least 60 minutes and the sampling rate shall be at least 0.015 dscm/min (0.53 dscf/min), except that shorter sampling times may be approved by the Administrator when process variables or other factors preclude sampling for at least 60 minutes.

(3) The coke burn-off rate (Rc) shall be computed for each run using the following equation:

Rc = K1Qr (%CO2 + %CO) + K2Qa−K3Qr (%CO/2 + %CO2 + %O2) + K3Qoxy (%Ooxy)
Where:
Rc = Coke burn-off rate, kilograms per hour (kg/hr) (lb/hr).
Qr = Volumetric flow rate of exhaust gas from fluid catalytic cracking unit regenerator before entering the emission control system, dscm/min (dscf/min).
Qa = Volumetric flow rate of air to fluid catalytic cracking unit regenerator, as determined from the fluid catalytic cracking unit control room instrumentation, dscm/min (dscf/min).
Qoxy = Volumetric flow rate of O2 enriched air to fluid catalytic cracking unit regenerator, as determined from the fluid catalytic cracking unit control room instrumentation, dscm/min (dscf/min).
%CO2 = Carbon dioxide concentration in fluid catalytic cracking unit regenerator exhaust, percent by volume (dry basis).
%CO = CO concentration in FCCU regenerator exhaust, percent by volume (dry basis).
%O2 = O2 concentration in fluid catalytic cracking unit regenerator exhaust, percent by volume (dry basis).
%Ooxy = O2 concentration in O2 enriched air stream inlet to the fluid catalytic cracking unit regenerator, percent by volume (dry basis).
K1 = Material balance and conversion factor, 0.2982 (kg-min)/(hr-dscm-%) [0.0186 (lb-min)/(hr-dscf-%)].
K2 = Material balance and conversion factor, 2.088 (kg-min)/(hr-dscm) [0.1303 (lb-min)/(hr-dscf)].
K3 = Material balance and conversion factor, 0.0994 (kg-min)/(hr-dscm-%) [0.00624 (lb-min)/(hr-dscf-%)].

(i) Method 2 shall be used to determine the volumetric flow rate (Qr).

(ii) The emission correction factor, integrated sampling and analysis procedure of Method 3B shall be used to determine CO2, CO, and O2 concentrations.

(4) Method 9 and the procedures of § 60.11 shall be used to determine opacity.

(c) If auxiliary liquid or solid fossil-fuels are burned in an incinerator-waste heat boiler, the owner or operator shall determine the emission rate of PM permitted in § 60.102(b) as follows:

(1) The allowable emission rate (Es) of PM shall be computed for each run using the following equation:

Es = F + A (H/Rc)
Where:
Es = Emission rate of PM allowed, kg/Mg (lb/ton) of coke burn-off in catalyst regenerator.
F = Emission standard, 1.0 kg/Mg (2.0 lb/ton) of coke burn-off in catalyst regenerator.
A = Allowable incremental rate of PM emissions, 43 g/GJ (0.10 lb/million Btu).
H = Heat input rate from solid or liquid fossil fuel, GJ/hr (million Btu/hr).
Rc = Coke burn-off rate, Mg coke/hr (ton coke/hr).

(2) Procedures subject to the approval of the Administrator shall be used to determine the heat input rate.

(3) The procedure in paragraph (b)(3) of this section shall be used to determine the coke burn-off rate (Rc).

(d) The owner or operator shall determine compliance with the CO standard in § 60.103(a) by using the integrated sampling technique of Method 10 to determine the CO concentration (dry basis). The sampling time for each run shall be 60 minutes.

(e)

(1) The owner or operator shall determine compliance with the H2S standard in § 60.104(a)(1) as follows: Method 11, 15, 15A, or 16 shall be used to determine the H2S concentration. The gases entering the sampling train should be at about atmospheric pressure. If the pressure in the refinery fuel gas lines is relatively high, a flow control valve may be used to reduce the pressure. If the line pressure is high enough to operate the sampling train without a vacuum pump, the pump may be eliminated from the sampling train. The sample shall be drawn from a point near the centroid of the fuel gas line.

(i) For Method 11, the sampling time and sample volume shall be at least 10 minutes and 0.010 dscm (0.35 dscf). Two samples of equal sampling times shall be taken at about 1-hour intervals. The arithmetic average of these two samples shall constitute a run. For most fuel gases, sampling times exceeding 20 minutes may result in depletion of the collection solution, although fuel gases containing low concentrations of H2S may necessitate sampling for longer periods of time.

(ii) For Method 15 or 16, at least three injects over a 1-hour period shall constitute a run.

(iii) For Method 15A, a 1-hour sample shall constitute a run.

(2) Where emissions are monitored by § 60.105(a)(3), compliance with § 60.104(a)(1) shall be determined using Method 6 or 6C and Method 3 or 3A. The method ANSI/ASME PTC 19.10-1981, “Flue and Exhaust Gas Analyses,” (incorporated by reference - see § 60.17) is an acceptable alternative to EPA Method 6. A 1-hour sample shall constitute a run. Method 6 samples shall be taken at a rate of approximately 2 liters/min. The ppm correction factor (Method 6) and the sampling location in paragraph (f)(1) of this section apply. Method 4 shall be used to determine the moisture content of the gases. The sampling point for Method 4 shall be adjacent to the sampling point for Method 6 or 6C.

(f) The owner or operator shall determine compliance with the SO2 and the H2S and reduced sulfur standards in § 60.104(a)(2) as follows:

(1) Method 6 shall be used to determine the SO2 concentration. The concentration in mg/dscm obtained by Method 6 or 6C is multiplied by 0.3754 to obtain the concentration in ppm. The sampling point in the duct shall be the centroid of the cross section if the cross-sectional area is less than 5.00 m 2 (53.8 ft 2) or at a point no closer to the walls than 1.00 m (39.4 in.) if the cross-sectional area is 5.00 m 2 or more and the centroid is more than 1 m from the wall. The sampling time and sample volume shall be at least 10 minutes and 0.010 dscm (0.35 dscf) for each sample. Eight samples of equal sampling times shall be taken at about 30-minute intervals. The arithmetic average of these eight samples shall constitute a run. For Method 6C, a run shall consist of the arithmetic average of four 1-hour samples. Method 4 shall be used to determine the moisture content of the gases. The sampling point for Method 4 shall be adjacent to the sampling point for Method 6 or 6C. The sampling time for each sample shall be equal to the time it takes for two Method 6 samples. The moisture content from this sample shall be used to correct the corresponding Method 6 samples for moisture. For documenting the oxidation efficiency of the control device for reduced sulfur compounds, Method 15 shall be used following the procedures of paragraph (f)(2) of this section.

(2) Method 15 shall be used to determine the reduced sulfur and H2 S concentrations. Each run shall consist of 16 samples taken over a minimum of 3 hours. The sampling point shall be the same as that described for Method 6 in paragraph (f)(1) of this section. To ensure minimum residence time for the sample inside the sample lines, the sampling rate shall be at least 3.0 lpm (0.10 cfm). The SO2 equivalent for each run shall be calculated after being corrected for moisture and oxygen as the arithmetic average of the SO2 equivalent for each sample during the run. Method 4 shall be used to determine the moisture content of the gases as the paragraph (f)(1) of this section. The sampling time for each sample shall be equal to the time it takes for four Method 15 samples.

(3) The oxygen concentration used to correct the emission rate for excess air shall be obtained by the integrated sampling and analysis procedure of Method 3 or 3A. The samples shall be taken simultaneously with the SO2, reduced sulfur and H2S, or moisture samples. The SO2, reduced sulfur, and H2S samples shall be corrected to zero percent excess air using the equation in paragraph (h)(6) of this section.

(g) Each performance test conducted for the purpose of determining compliance under § 60.104(b) shall consist of all testing performed over a 7-day period using Method 6 or 6C and Method 3 or 3A. To determine compliance, the arithmetic mean of the results of all the tests shall be compared with the applicable standard.

(h) For the purpose of determining compliance with § 60.104(b)(1), the following calculation procedures shall be used:

(1) Calculate each 1-hour average concentration (dry, zero percent oxygen, ppmv) of sulfur dioxide at both the inlet and the outlet to the add-on control device as specified in § 60.13(h). These calculations are made using the emission data collected under § 60.105(a).

(2) Calculate a 7-day average (arithmetic mean) concentration of sulfur dioxide for the inlet and for the outlet to the add-on control device using all of the 1-hour average concentration values obtained during seven successive 24-hour periods.

(3) Calculate the 7-day average percent reduction using the following equation:

Rso2 = 100(Cso2(i) − Cso2(o)) / Cso2(i)
where:
Rso2 = 7-day average sulfur dioxide emission reduction, percent
Cso2(i) = sulfur dioxide emission concentration determined in § 60.106(h)(2) at the inlet to the add-on control device, ppmv
Cso2(o) = sulfur dioxide emission concentration determined in § 60.106(h)(2) at the outlet to the add-on control device, ppmv
100 = conversion factor, decimal to percent

(4) Outlet concentrations of sulfur dioxide from the add-on control device for compliance with the 50 ppmv standard, reported on a dry, O2-free basis, shall be calculated using the procedures outlined in § 60.106(h)(1) and (2) above, but for the outlet monitor only.

(5) If supplemental sampling data are used for determining the 7-day averages under paragraph (h) of this section and such data are not hourly averages, then the value obtained for each supplemental sample shall be assumed to represent the hourly average for each hour over which the sample was obtained.

(6) For the purpose of adjusting pollutant concentrations to zero percent oxygen, the following equation shall be used:

where:
Cadj = pollutant concentration adjusted to zero percent oxygen, ppm or g/dscm
Cmeas = pollutant concentration measured on a dry basis, ppm or g/dscm
20.9c = 20.9 percent oxygen−0.0 percent oxygen (defined oxygen correction basis), percent
20.9 = oxygen concentration in air, percent
%O2 = oxygen concentration measured on a dry basis, percent

(i) For the purpose of determining compliance with § 60.104(b)(2), the following reference methods and calculation procedures shall be used except as provided in paragraph (i)(12) of this section:

(1) One 3-hour test shall be performed each day.

(2) For gases released to the atmosphere from the fluid catalytic cracking unit catalyst regenerator:

(i) Method 8 as modified in § 60.106(i)(3) for moisture content and for the concentration of sulfur oxides calculated as sulfur dioxide,

(ii) Method 1 for sample and velocity traverses,

(iii) Method 2 calculation procedures (data obtained from Methods 3 and 8) for velocity and volumetric flow rate, and

(iv) Method 3 for gas analysis.

(3) Method 8 shall be modified by the insertion of a heated glass fiber filter between the probe and first impinger. The probe liner and glass fiber filter temperature shall be maintained above 160 °C (320 °F). The isopropanol impinger shall be eliminated. Sample recovery procedures described in Method 8 for container No. 1 shall be eliminated. The heated glass fiber filter also shall be excluded; however, rinsing of all connecting glassware after the heated glass fiber filter shall be retained and included in container No. 2. Sampled volume shall be at least 1 dscm.

(4) For Method 3, the integrated sampling technique shall be used.

(5) Sampling time for each run shall be at least 3 hours.

(6) All testing shall be performed at the same location. Where the gases discharged by the fluid catalytic cracking unit catalyst regenerator pass through an incinerator-waste heat boiler in which auxiliary or supplemental gaseous, liquid, or solid fossil fuel is burned, testing shall be conducted at a point between the regenerator outlet and the incinerator-waste heat boiler. An alternative sampling location after the waste heat boiler may be used if alternative coke burn-off rate equations, and, if requested, auxiliary/supplemental fuel SOX credits, have been submitted to and approved by the Administrator prior to sampling.

(7) Coke burn-off rate shall be determined using the procedures specified under paragraph (b)(3) of this section, unless paragraph (i)(6) of this section applies.

(8) Calculate the concentration of sulfur oxides as sulfur dioxide using equation 8-3 in Section 6.5 of Method 8 to calculate and report the total concentration of sulfur oxides as sulfur dioxide (Cso x).

(9) Sulfur oxides emission rate calculated as sulfur dioxide shall be determined for each test run by the following equation:

${E}_{{so}_{x}}={C}_{{so}_{x}}{Q}_{sd}/K$

Where:
ESOx = sulfur oxides emission rate calculated as sulfur dioxide, kg/hr (lb/hr)
CSOx = sulfur oxides emission concentration calculated as sulfur dioxide, g/dscm (gr/dscf)
Qsd = dry volumetric stack gas flow rate corrected to standard conditions, dscm/hr (dscf/hr)
K = 1,000 g/kg (7,000 gr/lb)

(10) Sulfur oxides emissions calculated as sulfur dioxide shall be determined for each test run by the following equation:

${R}_{{so}_{x}}=\left({E}_{{so}_{x}}}{{R}_{c}}\right)$

Where:
RSOx = Sulfur oxides emissions calculated as kg sulfur dioxide per Mg (lb/ton) coke burn-off.
ESOx = Sulfur oxides emission rate calculated as sulfur dioxide, kg/hr (lb/hr).
Rc = Coke burn-off rate, Mg/hr (ton/hr).

(11) Calculate the 7-day average sulfur oxides emission rate as sulfur dioxide per Mg (ton) of coke burn-off by dividing the sum of the individual daily rates by the number of daily rates summed.

(12) An owner or operator may, upon approval by the Administrator, use an alternative method for determining compliance with § 60.104(b)(2), as provided in § 60.8(b). Any requests for approval must include data to demonstrate to the Administrator that the alternative method would produce results adequate for the determination of compliance.

(j) For the purpose of determining compliance with § 60.104(b)(3), the following analytical methods and calculation procedures shall be used:

(1) One fresh feed sample shall be collected once per 8-hour period.

(2) Fresh feed samples shall be analyzed separately by using any one of the following applicable analytical test methods: ASTM D129-64, 78, or 95, ASTM D1552-83 or 95, ASTM D2622-87, 94, or 98, or ASTM D1266-87, 91, or 98. (These methods are incorporated by reference: see § 60.17.) The applicable range of some of these ASTM methods is not adequate to measure the levels of sulfur in some fresh feed samples. Dilution of samples prior to analysis with verification of the dilution ratio is acceptable upon prior approval of the Administrator.

(3) If a fresh feed sample cannot be collected at a single location, then the fresh feed sulfur content shall be determined as follows:

(i) Individual samples shall be collected once per 8-hour period for each separate fresh feed stream charged directly into the riser or reactor of the fluid catalytic cracking unit. For each sample location the fresh feed volumetric flow rate at the time of collecting the fresh feed sample shall be measured and recorded. The same method for measuring volumetric flow rate shall be used at all locations.

(ii) Each fresh feed sample shall be analyzed separately using the methods specified under paragraph (j)(2) of this section.

(iii) Fresh feed sulfur content shall be calculated for each 8-hour period using the following equation:

${S}_{f}=\sum _{i=1}^{n}\frac{{S}_{i}{Q}_{i}}{{Q}_{f}}$

where:
Sf = fresh feed sulfur content expressed in percent by weight of fresh feed.
n = number of separate fresh feed streams charged directly to the riser or reactor of the fluid catalytic cracking unit.
Qf = total volumetric flow rate of fresh feed charged to the fluid catalytic cracking unit.
Si = fresh feed sulfur content expressed in percent by weight of fresh feed for the “ith” sampling location.
Qi = volumetric flow rate of fresh feed stream for the “ith” sampling location.

(4) Calculate a 7-day average (arithmetic mean) sulfur content of the fresh feed using all of the fresh feed sulfur content values obtained during seven successive 24-hour periods.

(k) The test methods used to supplement continuous monitoring system data to meet the minimum data requirements in § 60.104(d) will be used as described below or as otherwise approved by the Administrator.

(1) Methods 6, 6B, or 8 are used. The sampling location(s) are the same as those specified for the monitor.

(2) For Method 6, the minimum sampling time is 20 minutes and the minimum sampling volume is 0.02 dscm (0.71 dscf) for each sample. Samples are taken at approximately 60-minute intervals. Each sample represents a 1-hour average. A minimum of 18 valid samples is required to obtain one valid day of data.

(3) For Method 6B, collection of a sample representing a minimum of 18 hours is required to obtain one valid day of data.

(4) For Method 8, the procedures as outlined in this section are used. The equivalent of 16 hours of sampling is required to obtain one valid day of data.

[39 FR 9315, Mar. 8, 1974, as amended at 43 FR 10869, Mar. 15, 1978; 51 FR 42842, Nov. 26, 1986; 52 FR 20392, June 1, 1987; 53 FR 41333, Oct. 21, 1988; 54 FR 34028, Aug. 17, 1989; 55 FR 40176, Oct. 2, 1990; 56 FR 4176, Feb. 4, 1991; 65 FR 61754, Oct. 17, 2000; 71 FR 55127, Sept. 21, 2006; 73 FR 35867, June 24, 2008; 77 FR 56463, Sep. 12, 2012]