Title 40—Protection of Environment--Volume 1
PART 1065—ENGINE-TESTING PROCEDURES
§ 1065.660   THC, NMHC, NMNEHC, CH4, and C2H6determination.
(a) THC determination and initial THC/CH 4 contamination corrections. (1) If we require you to determine THC emissions, calculate x THC[THC-FID]cor using the initial THC contamination concentration x THC[THC-FID]init from § 1065.520 as follows:
Example:
(2) For the NMHC determination described in paragraph (b) of this section, correct x THC[THC-FID] for initial THC contamination using Eq. 1065.660-1. You may correct x THC[NMC-FID] for initial contamination of the CH 4 sample train using Eq. 1065.660-1, substituting in CH 4 concentrations for THC.
(3) For the NMNEHC determination described in paragraph (c) of this section, correct x THC[THC-FID] for initial THC contamination using Eq. 1065.660-1. You may correct x THC[NMC-FID] for initial contamination of the CH 4 sample train using Eq. 1065.660-1, substituting in CH 4 concentrations for THC.
(4) For the CH 4 determination described in paragraph (d) of this section, you may correct x THC[NMC-FID] for initial THC contamination of the CH 4 sample train using Eq. 1065.660-1, substituting in CH 4 concentrations for THC.
(5) You may calculate THC as the sum of NMHC and CH 4 if you determine CH 4 with an FTIR as described in paragraph (d)(2) of this section and NMHC with an FTIR using the additive method from paragraph (b)(4) of this section.
(6) You may calculate THC as the sum of NMNEHC, C 2 H 6 , and CH 4 if you determine CH 4 with an FTIR as described in paragraph (d)(2) of this section, C 2 H 6 with an FTIR as described in paragraph (e) of this section, and NMNEHC with an FTIR using the additive method from paragraph (c)(3) of this section.
(b) NMHC determination. Use one of the following to determine NMHC concentration, x NMHC :
(1) If you do not measure CH 4 , you may omit the calculation of NMHC concentrations and calculate the mass of NMHC as described in § 1065.650(c)(5).
(2) For an NMC, calculate x NMHC using the NMC's penetration fractions, response factors, and/or combined penetration fractions and response factors as described in § 1065.365, the THC FID's CH 4 response factor, RF CH4[THC-FID], from § 1065.360, the initial THC contamination and dry-to-wet corrected THC concentration, x THC[THC-FID]cor, as determined in paragraph (a) of this section, and the dry-to-wet corrected CH 4 concentration, x THC[NMC-FID]cor, optionally corrected for initial THC contamination as determined in paragraph (a) of this section.
(i) Use the following equation for an NMC configured as described in § 1065.365(d):
Eq. 1065.660-2
Where:
Example:
(ii) Use the following equation for penetration fractions determined using an NMC configuration as outlined in § 1065.365(e):
Example:
(iii) Use the following equation for an NMC configured as described in § 1065.365(f):
Example:
(3) For a GC-FID or FTIR, calculate x NMHC using the THC analyzer's CH 4 response factor, RF CH4[THC-FID], from § 1065.360, and the initial THC contamination and dry-to-wet corrected THC concentration, x THC[THC-FID]cor, as determined in paragraph (a) of this section as follows:
Example:
x THC[THC-FID]cor = 145.6 µmol/mol
RF CH4[THC-FID] = 0.970
x CH4 = 18.9 µmol/mol
x NMHC = 145.6—0.970 · 18.9
x NMHC = 127.3 µmol/mol
(4) For an FTIR, calculate x NMHC by summing the hydrocarbon species listed in § 1065.266(c) as follows:
Example:
(c) NMNEHC determination. Use one of the following methods to determine NMNEHC concentration, x NMNEHC :
(1) Calculate x NMNEHC based on the test fuel's ethane content as follows:
(i) If the content of your test fuel contains less than 0.010 mol/mol of ethane, you may omit the calculation of NMNEHC concentration and calculate the mass of NMNEHC as described in § 1065.650(c)(6)(i).
(ii) If the content of your fuel test contains at least 0.010 mol/mol of C 2 H 6 , you may omit the calculation of NMNEHC concentration and calculate the mass of NMNEHC as described in § 1065.650(c)(6)(ii).
(2) For a GC-FID, NMC FID, or FTIR, calculate x NMNEHC using the THC analyzer's CH 4 response factor, RF CH4[THC-FID], and C 2 H 6 response factor, RF C2H6[THC-FID], from § 1065.360, the initial contamination and dry-to-wet corrected THC concentration, x THC[THC-FID]cor, as determined in paragraph (a) of this section, the dry-to-wet corrected CH 4 concentration, x CH4, as determined in paragraph (d) of this section, and the dry-to-wet corrected C 2 H 6 concentration, x C2H6, as determined in paragraph (e) of this section as follows:
Example:
(3) For an FTIR, calculate x NMNEHC by summing the hydrocarbon species listed in § 1065.266(c) as follows:
Example:
(d) CH 4 determination. Use one of the following methods to determine methane (CH 4 ) concentration, x CH4 :
(1) For an NMC, calculate x CH4 using the NMC's penetration fractions, response factors, and/or combined penetration fractions and response factors as described in § 1065.365, the THC FID's CH 4 response factor, RF CH4[THC-FID], from § 1065.360, the initial THC contamination and dry-to-wet corrected THC concentration, x THC[THC-FID]cor, as determined in paragraph (a) of this section, and the dry-to-wet corrected CH 4 concentration, x THC[NMC-FID]cor, optionally corrected for initial THC contamination as determined in paragraph (a) of this section.
(i) Use the following equation for an NMC configured as described in § 1065.365(d):
Example:
(ii) Use the following equation for an NMC configured as described in § 1065.365(e):
Example:
(iii) Use the following equation for an NMC configured as described in § 1065.365(f):
Example:
(2) For a GC-FID or FTIR, x CH4 is the actual dry-to-wet corrected CH 4 concentration as measured by the analyzer.
(e) C 2 H 6 determination. For a GC-FID or FTIR, x C2H6 is the C 1 -equivalent, dry-to-wet corrected C 2 H 6 concentration as measured by the analyzer.
§ 1065.665   THCE and NMHCE determination.
(a) If you measured an oxygenated hydrocarbon's mass concentration, first calculate its molar concentration in the exhaust sample stream from which the sample was taken (raw or diluted exhaust), and convert this into a C 1 -equivalent molar concentration. Add these C 1 -equivalent molar concentrations to the molar concentration of non-oxygenated total hydrocarbon (NOTHC). The result is the molar concentration of total hydrocarbon equivalent (THCE). Calculate THCE concentration using the following equations, noting that Eq. 1065.665-3 is required only if you need to convert your oxygenated hydrocarbon (OHC) concentration from mass to moles:
(b) If we require you to determine nonmethane hydrocarbon equivalent (NMHCE), use the following equation:
(c) The following example shows how to determine NMHCE emissions based on ethanol (C 2 H 5 OH), methanol (CH 3 OH), acetaldehyde (C 2 H 4 O), and formaldehyde (CH 2 O) as C 1 -equivalent molar concentrations:
§ 1065.667   Dilution air background emission correction.
(a) To determine the mass of background emissions to subtract from a diluted exhaust sample, first determine the total flow of dilution air, n dil, over the test interval. This may be a measured quantity or a calculated quantity. Multiply the total flow of dilution air by the mean mole fraction ( i.e., concentration) of a background emission. This may be a time-weighted mean or a flow-weighted mean ( e.g., a proportionally sampled background). Finally, multiply by the molar mass, M, of the associated gaseous emission constituent. The product of n dil and the mean molar concentration of a background emission and its molar mass, M, is the total background emission mass, m. In the case of PM, where the mean PM concentration is already in units of mass per mole of exhaust, multiply it by the total amount of dilution air flow, and the result is the total background mass of PM, m PM. Subtract total background mass from total mass to correct for background emissions.
(b) You may determine the total flow of dilution air by a direct flow measurement.
(c) You may determine the total flow of dilution air by subtracting the calculated raw exhaust molar flow as described in § 1065.655(g) from the measured dilute exhaust flow. This may be done by totaling continuous calculations or by using batch results.
(d) You may determine the total flow of dilution air from the measured dilute exhaust flow and a chemical balance of the fuel, DEF, intake air, and dilute exhaust as described in § 1065.655. For this paragraph (d), the molar flow of dilution air is calculated by multiplying the dilute exhaust flow by the mole fraction of dilution gas to dilute exhaust, χ dil/ex , from the dilute chemical balance. This may be done by totaling continuous calculations or by using batch results. For example, to use batch results, the total flow of dilution air is calculated by multiplying the total flow of diluted exhaust, n dexh , by the flow-weighted mean mole fraction of dilution air in diluted exhaust, χ dil/exh . Calculate χ dil/exh using flow-weighted mean concentrations of emissions in the chemical balance, as described in § 1065.655. The chemical balance in § 1065.655 assumes that your engine operates stoichiometrically, even if it is a lean-burn engine, such as a compression-ignition engine. Note that for lean-burn engines this assumption could result in an error in emission calculations. This error could occur because the chemical balance in § 1065.655 treats excess air passing through a lean-burn engine as if it was dilution air. If an emission concentration expected at the standard is about 100 times its dilution air background concentration, this error is negligible. However, if an emission concentration expected at the standard is similar to its background concentration, this error could be significant. If this error might affect your ability to show that your engines comply with applicable standards in this chapter, we recommend that you either determine the total flow of dilution air using one of the more accurate methods in paragraph (b) or (c) of this section, or remove background emissions from dilution air by HEPA filtration, chemical adsorption, or catalytic scrubbing. You might also consider using a partial-flow dilution technique such as a bag mini-diluter, which uses purified air as the dilution air.
(e) The following is an example of using the flow-weighted mean fraction of dilution air in diluted exhaust, x dil/exh , and the total mass of background emissions calculated using the total flow of diluted exhaust, n dexh , as described in § 1065.650(c):
(f) The following is an example of using the fraction of dilution air in diluted exhaust, x dil/exh , and the mass rate of background emissions calculated using the flow rate of diluted exhaust, n dexh , as described in § 1065.650(c):
§ 1065.670   NOXintake-air humidity and temperature corrections.
See the standard-setting part to determine if you may correct NO X emissions for the effects of intake-air humidity or temperature. Use the NO X intake-air humidity and temperature corrections specified in the standard-setting part instead of the NO X intake-air humidity correction specified in this part 1065. If the standard-setting part does not prohibit correcting NO X emissions for intake-air humidity according to this part 1065, correct NO X concentrations for intake-air humidity as described in this section. See § 1065.650(c)(1) for the proper sequence for applying the NO X intake-air humidity and temperature corrections. You may use a time-weighted mean intake air humidity to calculate this correction if your intake air humidity remains within a tolerance of ±0.0025 mol/mol of the mean value over the test interval. For intake-air humidity correction, use one of the following approaches:
(a) For compression-ignition engines operating on carbon-containing fuels and lean-burn combustion engines operating on fuels other than carbon-containing fuels, correct for intake-air humidity using the following equation:
(b) For spark-ignition engines operating on carbon-containing fuels and stoichiometric combustion engines operating on fuels other than carbon-containing fuels, correct for intake-air humidity using the following equation:
(c) Develop your own correction, based on good engineering judgment.
§ 1065.672   Drift correction.
(a) Scope and frequency. Perform the calculations in this section to determine if gas analyzer drift invalidates the results of a test interval. If drift does not invalidate the results of a test interval, correct that test interval's gas analyzer responses for drift according to this section. Use the drift-corrected gas analyzer responses in all subsequent emission calculations. Note that the acceptable threshold for gas analyzer drift over a test interval is specified in § 1065.550 for both laboratory testing and field testing.
(b) Correction principles. The calculations in this section utilize a gas analyzer's responses to reference zero and span concentrations of analytical gases, as determined sometime before and after a test interval. The calculations correct the gas analyzer's responses that were recorded during a test interval. The correction is based on an analyzer's mean responses to reference zero and span gases, and it is based on the reference concentrations of the zero and span gases themselves. Validate and correct for drift as follows:
(c) Drift validation. After applying all the other corrections—except drift correction—to all the gas analyzer signals, calculate emissions according to § 1065.650. Then correct all gas analyzer signals for drift according to this section. Recalculate emissions using all of the drift-corrected gas analyzer signals. Validate and report the emission results before and after drift correction according to § 1065.550.
(d) Drift correction. Correct all gas analyzer signals as follows:
(1) Correct each recorded concentration, x i , for continuous sampling or for batch sampling, x .
(2) Correct for drift using the following equation:
(3) For any pre-test interval concentrations, use the last concentration determined before the test interval. For some test intervals, the last pre-zero or pre-span might have occurred before one or more earlier test intervals.
(4) For any post-test interval concentrations, use the first concentration determined after the test interval. For some test intervals, the first post-zero or post-span might occur after one or more later test intervals.
(5) If you do not record any pre-test interval analyzer response to the span gas concentration, x prespan , set x prespan equal to the reference concentration of the span gas:
(6) If you do not record any pre-test interval analyzer response to the zero gas concentration, x prezero , set x prezero equal to the reference concentration of the zero gas:
(7) Usually the reference concentration of the zero gas, x refzero , is zero: x refzero = 0 µmol/mol. However, in some cases you might know that x refzero has a non-zero concentration. For example, if you zero a CO 2 analyzer using ambient air, you may use the default ambient air concentration of CO 2 , which is 375 µmol/mol. In this case, x refzero = 375 µmol/mol. Note that when you zero an analyzer using a non-zero x refzero , you must set the analyzer to output the actual x refzero concentration. For example, if x refzero = 375 µmol/mol, set the analyzer to output a value of 375 µmol/mol when the zero gas is flowing to the analyzer.
§ 1065.675   CLD quench verification calculations.
Perform CLD quench-check calculations as follows:
(a) Perform a CLD analyzer quench verification test as described in § 1065.370.
(b) Estimate the maximum expected mole fraction of water during emission testing, x H2Oexp. Make this estimate where the humidified NO span gas was introduced in § 1065.370(e)(6). When estimating the maximum expected mole fraction of water, consider the maximum expected water content in intake air, fuel combustion products, and dilution air (if applicable). If you introduced the humidified NO span gas into the sample system upstream of a sample dryer during the verification test, you need not estimate the maximum expected mole fraction of water and you must set x H2Oexp equal to x H2Omeas.
(c) Estimate the maximum expected CO 2 concentration during emission testing, x CO2exp . Make this estimate at the sample system location where the blended NO and CO 2 span gases are introduced according to § 1065.370(d)(10). When estimating the maximum expected CO 2 concentration, consider the maximum expected CO 2 content in fuel combustion products and dilution air.
(d) Calculate quench as follows:
§ 1065.680   Adjusting emission levels to account for infrequently regenerating aftertreatment devices.
This section describes how to calculate and apply emission adjustment factors for engines using aftertreatment technology with infrequent regeneration events that may occur during testing. These adjustment factors are typically calculated based on measurements conducted for the purposes of engine certification, and then used to adjust the results of testing related to demonstrating compliance with emission standards. For this section, “regeneration” means an intended event during which emission levels change while the system restores aftertreatment performance. For example, exhaust gas temperatures may increase temporarily to remove sulfur from an adsorber or SCR catalyst or to oxidize accumulated particulate matter in a trap. The duration of this event extends until the aftertreatment performance and emission levels have returned to normal baseline levels. Also, “infrequent” refers to regeneration events that are expected to occur on average less than once over a transient or ramped-modal duty cycle, or on average less than once per mode in a discrete-mode test.
(a) Apply adjustment factors based on whether there is active regeneration during a test segment. The test segment may be a test interval or a full duty cycle, as described in paragraph (b) of this section. For engines subject to standards over more than one duty cycle, you must develop adjustment factors under this section for each separate duty cycle. You must be able to identify active regeneration in a way that is readily apparent during all testing. All adjustment factors for regeneration are additive.
(1) If active regeneration does not occur during a test segment, apply an upward adjustment factor, UAF, that will be added to the measured emission rate for that test segment. Use the following equation to calculate UAF:
(2) If active regeneration occurs or starts to occur during a test segment, apply a downward adjustment factor, DAF, that will be subtracted from the measured emission rate for that test segment. Use the following equation to calculate DAF:
(3) Note that emissions for a given pollutant may be lower during regeneration, in which case EF L would be greater than EF H, and both UAF and DAF would be negative.
(4) Calculate the average emission factor, EF A, as follows:
(5) The frequency of regeneration, F, generally characterizes how often a regeneration event occurs within a series of test segments. Determine F using the following equation, subject to the provisions of paragraph (a)(6) of this section:
(6) Use good engineering judgment to determine i r and i f , as follows:
(i) For engines that are programmed to regenerate after a specific time interval, you may determine the duration of a regeneration event and the time between regeneration events based on the engine's design parameters. For other engines, determine these values based on measurements from in-use operation or from running repetitive duty cycles in a laboratory.
(ii) For engines subject to standards over multiple duty cycles, such as for transient and steady-state testing, apply this same calculation to determine a value of F for each duty cycle.
(iii) Consider an example for an engine that is designed to regenerate its PM filter 500 minutes after the end of the last regeneration event, with the regeneration event lasting 30 minutes. If the RMC takes 28 minutes, i rRMC = 2 (30 ÷ 28 = 1.07, which rounds up to 2), and i fRMC = 500 ÷ 28 = 17.86.
(b) Develop adjustment factors for different types of testing as follows:
(1) Discrete-mode testing. Develop separate adjustment factors for each test mode (test interval) of a discrete-mode test. When measuring EF H , if a regeneration event has started but is not complete when you reach the end of the sampling time for a test interval, extend the sampling period for that test interval until the regeneration event is complete.
(2) Ramped-modal and transient testing. Develop a separate set of adjustment factors for an entire ramped-modal cycle or transient duty cycle. When measuring EF H , if a regeneration event has started but is not complete when you reach the end of the duty cycle, start the next repeat test as soon as possible, allowing for the time needed to complete emission measurement and installation of new filters for PM measurement; in that case EF H is the average emission level for the test segments that included regeneration.
(3) Accounting for cold-start measurements. For engines subject to cold-start testing requirements, incorporate cold-start operation into your analysis as follows:
(i) Determine the frequency of regeneration, F , in a way that incorporates the impact of cold-start operation in proportion to the cold-start weighting factor specified in the standard-setting part. You may use good engineering judgment to determine the effect of cold-start operation analytically.
(ii) Treat cold-start testing and hot-start testing together as a single test segment for adjusting measured emission results under this section. Apply the adjustment factor to the composite emission result.
(iii) You may apply the adjustment factor only to the hot-start test result if your aftertreatment technology does not regenerate during cold operation as represented by the cold-start transient duty cycle. If we ask for it, you must demonstrate this by engineering analysis or by test data.
(c) If an engine has multiple regeneration strategies, determine and apply adjustment factors under this section separately for each type of regeneration.
§ 1065.690   Buoyancy correction for PM sample media.
(a) General. Correct PM sample media for their buoyancy in air if you weigh them on a balance. The buoyancy correction depends on the sample media density, the density of air, and the density of the calibration weight used to calibrate the balance. The buoyancy correction does not account for the buoyancy of the PM itself, because the mass of PM typically accounts for only (0.01 to 0.10)% of the total weight. A correction to this small fraction of mass would be at the most 0.010%.
(b) PM sample media density. Different PM sample media have different densities. Use the known density of your sample media, or use one of the densities for some common sampling media, as follows:
(1) For PTFE-coated borosilicate glass, use a sample media density of 2300 kg/m 3 .
(2) For PTFE membrane (film) media with an integral support ring of polymethylpentene that accounts for 95% of the media mass, use a sample media density of 920 kg/m 3 .
(3) For PTFE membrane (film) media with an integral support ring of PTFE, use a sample media density of 2144 kg/m 3 .
(c) Air density. Because a PM balance environment must be tightly controlled to an ambient temperature of (22 ±1) °C and humidity has an insignificant effect on buoyancy correction, air density is primarily a function of atmospheric pressure. Therefore you may use nominal constant values for temperature and humidity when determining the air density of the balance environment in Eq. 1065.690-2.
(d) Calibration weight density. Use the stated density of the material of your metal calibration weight. The example calculation in this section uses a density of 8000 kg/m 3 , but you should know the density of your weight from the calibration weight supplier or the balance manufacturer if it is an internal weight.
(e) Correction calculation. Correct the PM sample media for buoyancy using the following equations:
§ 1065.695   Data requirements.
(a) To determine the information we require from engine tests, refer to the standard-setting part and request from your EPA Program Officer the format used to apply for certification or demonstrate compliance. We may require different information for different purposes, such as for certification applications, approval requests for alternate procedures, selective enforcement audits, laboratory audits, production-line test reports, and field-test reports.
(b) See the standard-setting part and § 1065.25 regarding recordkeeping.
(c) We may ask you the following about your testing, and we may ask you for other information as allowed under the Act:
(1) What approved alternate procedures did you use? For example:
(i) Partial-flow dilution for proportional PM.
(ii) CARB test procedures.
(iii) ISO test procedures.
(2) What laboratory equipment did you use? For example, the make, model, and description of the following:
(i) Engine dynamometer and operator demand.
(ii) Probes, dilution, transfer lines, and sample preconditioning components.
(iii) Batch storage media (such as the bag material or PM filter material).
(3) What measurement instruments did you use? For example, the make, model, and description of the following:
(i) Speed and torque instruments.
(ii) Flow meters.
(iii) Gas analyzers.
(iv) PM balance.
(4) When did you conduct calibrations and performance checks and what were the results? For example, the dates and results of the following:
(i) Linearity verification.
(ii) Interference checks.
(iii) Response checks.
(iv) Leak checks.
(v) Flow meter checks.
(5) What engine did you test? For example, the following:
(i) Manufacturer.
(ii) Family name on engine label.
(iii) Model.
(iv) Model year.
(v) Identification number.
(6) How did you prepare and configure your engine for testing? Consider the following examples:
(i) Dates, hours, duty cycle and fuel used for service accumulation.
(ii) Dates and description of scheduled and unscheduled maintenance.
(iii) Allowable pressure range of intake restriction.
(iv) Allowable pressure range of exhaust restriction.
(v) Charge air cooler volume.
(vi) Charge air cooler outlet temperature, specified engine conditions and location of temperature measurement.
(vii) Fuel temperature and location of measurement.
(viii) Any aftertreatment system configuration and description.
(ix) Any crankcase ventilation configuration and description (e.g., open, closed, PCV, crankcase scavenged).
(x) Number and type of preconditioning cycles.
(7) How did you test your engine? For example:
(i) Constant speed or variable speed.
(ii) Mapping procedure (step or sweep).
(iii) Continuous or batch sampling for each emission.
(iv) Raw or dilute sampling; any dilution-air background sampling.
(v) Duty cycle and test intervals.
(vi) Cold-start, hot-start, warmed-up running.
(vii) Absolute pressure, temperature, and dewpoint of intake and dilution air.
(viii) Simulated engine loads, curb idle transmission torque value.
(ix) Warm-idle speed value.
(x) Simulated vehicle signals applied during testing.
(xi) Bypassed governor controls during testing.
(xii) Date, time, and location of test (e.g., dynamometer laboratory identification).
(xiii) Cooling medium for engine and charge air.
(xiv) Operating temperatures of coolant, head, and block.
(xv) Natural or forced cool-down and cool-down time.
(xvi) Canister loading.
(8) How did you validate your testing? For example, results from the following:
(i) Duty cycle regression statistics for each test interval.
(ii) Proportional sampling.
(iii) Drift.
(iv) Reference PM sample media in PM-stabilization environment.
(v) Carbon balance error verification, if performed.
(9) How did you calculate results? For example, results from the following:
(i) Drift correction.
(ii) Noise correction.
(iii) “Dry-to-wet” correction.
(iv) NMHC, CH 4 , and contamination correction.
(v) Chemical balance method—carbon-based or hydrogen-based chemical balance method.
(vi) NO X humidity correction.
(vii) Brake-specific emission formulation—total mass divided by total work, mass rate divided by power, or ratio of mass to work.
(viii) Rounding emission results.
(10) What were the results of your testing? For example:
(i) Maximum mapped power and speed at maximum power.
(ii) Maximum mapped torque and speed at maximum torque.
(iii) For constant-speed engines: no-load governed speed.
(iv) For constant-speed engines: test torque.
(v) For variable-speed engines: maximum test speed.
(vi) Speed versus torque map.
(vii) Speed versus power map.
(viii) Brake-specific emissions over the duty cycle and each test interval.
(ix) Brake-specific fuel consumption.
(11) What fuel did you use? For example:
(i) Fuel that met specifications of subpart H of this part.
(ii) Alternate fuel.
(iii) Oxygenated fuel.
(12) How did you field test your engine? For example:
(i) Data from paragraphs (c)(1), (3), (4), (5), and (9) of this section.
(ii) Probes, dilution, transfer lines, and sample preconditioning components.
(iii) Batch storage media (such as the bag material or PM filter material).
(iv) Continuous or batch sampling for each emission.
(v) Raw or dilute sampling; any dilution air background sampling.
(vi) Cold-start, hot-start, warmed-up running.
(vii) Intake and dilution air absolute pressure, temperature, dewpoint.
(viii) Curb idle transmission torque value.
(ix) Warm idle speed value, any enhanced-idle speed value.
(x) Date, time, and location of test (e.g., identify the testing laboratory).
(xi) Proportional sampling validation.
(xii) Drift validation.
(xiii) Operating temperatures of coolant, head, and block.
(xiv) Vehicle make, model, model year, identification number.
§ 1065.701   General requirements for test fuels.
(a) General. For all emission measurements, use test fuels that meet the specifications in this subpart, unless the standard-setting part directs otherwise. Section 1065.10(c)(1) does not apply with respect to test fuels. Note that the standard-setting parts generally require that you design your emission controls to function properly when using commercially available fuels, even if they differ from the test fuel. Where we specify multiple grades of a certain fuel type (such as diesel fuel with different sulfur concentrations), see the standard-setting part to determine which grade to use.
(b) Fuels meeting alternate specifications. We may allow you to use a different test fuel (such as California LEV III gasoline) if it does not affect your ability to show that your engines would comply with all applicable emission standards in this chapter using the test fuel specified in this subpart.
(c) Fuels not specified in this subpart. If you produce engines that run on a type of fuel (or mixture of fuels) that we do not specify in this subpart, you must get our written approval to establish the appropriate test fuel. See the standard-setting part for provisions related to fuels and fuel mixtures not specified in this subpart.
(1) For engines designed to operate on a single fuel, we will generally allow you to use the fuel if you show us all the following things are true:
(i) Show that your engines will use only the designated fuel in service.
(ii) Show that this type of fuel is commercially available.
(iii) Show that operating the engines on the fuel we specify would be inappropriate, as in the following examples:
(A) The engine will not run on the specified fuel.
(B) The engine or emission controls will not be durable or work properly when operating with the specified fuel.
(C) The measured emission results would otherwise be substantially unrepresentative of in-use emissions.
(2) For engines that are designed to operate on different fuel types, the provisions of paragraphs (c)(1)(ii) and (iii) of this section apply with respect to each fuel type.
(3) For engines that are designed to operate on different fuel types as well as continuous mixtures of those fuels, we may require you to test with either the worst-case fuel mixture or the most representative fuel mixture, unless the standard-setting part specifies otherwise.
(d) Fuel specifications. Specifications in this section apply as follows:
(1) Measure and calculate values as described in the appropriate reference procedure. Record and report final values expressed to at least the same number of decimal places as the applicable limit value. The right-most digit for each limit value is significant unless specified otherwise. For example, for a specified distillation temperature of 60 °C, determine the test fuel's value to at least the nearest whole number.
(2) The fuel parameters specified in this subpart depend on measurement procedures that are incorporated by reference. For any of these procedures, you may instead rely upon the procedures identified in 40 CFR part 1090 for measuring the same parameter. For example, we may identify different reference procedures for measuring gasoline parameters in 40 CFR 1090.1360.
(e) Two-stroke fuel/oil mixing. For two-stroke engines, use a fuel/oil mixture meeting the manufacturer's specifications.
(f) Service accumulation and field testing fuels. If we do not specify a service-accumulation or field-testing fuel in the standard-setting part, use an appropriate commercially available fuel such as those meeting minimum specifications from the following table:
Table 1 of § 1065.701—Examples of Service-Accumulation and Field-Testing Fuels
a Incorporated by reference; see § 1065.1010.
§ 1065.703   Distillate diesel fuel.
(a) Distillate diesel fuels for testing must be clean and bright, with pour and cloud points adequate for proper engine operation.
(b) There are three grades of #2 diesel fuel specified for use as a test fuel. See the standard-setting part to determine which grade to use. If the standard-setting part does not specify which grade to use, use good engineering judgment to select the grade that represents the fuel on which the engines will operate in use. The three grades are specified in Table 1 of this section.
Table 1 of § 1065.703—Test Fuel Specifications for Distillate Diesel Fuel
a Incorporated by reference, see § 1065.1010. See § 1065.701(d) for other allowed procedures.
(c) You may use the following nonmetallic additives with distillate diesel fuels:
(1) Cetane improver.
(2) Metal deactivator.
(3) Antioxidant, dehazer.
(4) Rust inhibitor.
(5) Pour depressant.
(6) Dye.
(7) Dispersant.
(8) Biocide.
§ 1065.705   Residual and intermediate residual fuel.
This section describes the specifications for fuels meeting the definition of residual fuel in 40 CFR 1090.80, including fuels marketed as intermediate fuel. Residual fuels for service accumulation and any testing must meet the following specifications:
(a) The fuel must be a commercially available fuel that is representative of the fuel that will be used by the engine in actual use.
(b) The fuel must be free of used lubricating oil. Demonstrate this by showing that the fuel meets at least one of the following specifications.
(1) Zinc is at or below 15 mg per kg of fuel based on the procedures specified in IP—470, IP—501, or ISO 8217 (incorporated by reference, see § 1065.1010).
(2) Phosphorus is at or below 15 mg per kg of fuel based on the procedures specified in IP—500, IP—501, or ISO 8217 (incorporated by reference, see § 1065.1010).
(3) Calcium is at or below 30 mg per kg of fuel based on the procedures specified in IP—470, IP—501, or ISO 8217 (incorporated by reference, see § 1065.1010).
(c) The fuel must meet the specifications for one of the categories in the following table:
§ 1065.710   Gasoline.
(a) This section specifies test fuel properties for gasoline with ethanol (low-level blend only) and for gasoline without ethanol. Note that the “fuel type” for the fuels specified in paragraphs (b) and (c) of this section is considered to be gasoline. In contrast, fuels with higher ethanol concentrations, such as fuel containing 82 percent ethanol, are considered to be ethanol fuels rather than gasoline. We specify some test fuel parameters that apply uniquely for low-temperature testing and for testing at altitudes above 1,219 m. For all other testing, use the test fuel parameters specified for general testing. Unless the standard-setting part specifies otherwise, use the fuel specified in paragraph (c) of this section for general testing.
(b) The following specifications apply for a blended gasoline test fuel that has nominally 10% ethanol (commonly called E10 test fuel):
(1) Prepare the blended test fuel from typical refinery gasoline blending components. You may not use pure compounds, except as follows:
(i) You may use neat ethanol as a blendstock.
(ii) You may adjust the test fuel's vapor pressure by adding butane.
(iii) You may adjust the test fuel's benzene content by adding benzene.
(iv) You may adjust the test fuel's sulfur content by adding sulfur compounds that are representative of those found with in-use fuels.
(2) Table 1 of this section identifies limit values consistent with the units in the reference procedure for each fuel property. These values are generally specified in international units. Values presented in parentheses are for information only. Table 1 follows:
(3) The ethanol-blended specification in Table 1 of this section is based on the volume % ethanol content of the fuel as determined during blending by the fuel supplier and as stated by the supplier at the time of fuel delivery. Use good engineering judgment to determine the volume % of ethanol based on the volume of each blendstock. We recommend using a flow-based or gravimetric procedure that has an accuracy and repeatability of ±0.1%.
(c) The specifications of this paragraph (c) apply for testing with neat gasoline. This is sometimes called indolene or E0 test fuel. Gasoline for testing must have octane values that represent commercially available fuels for the appropriate application. Test fuel specifications apply as follows:
Table 2 of § 1065.710—Test Fuel Specifications for Neat (E0) Gasoline
a Incorporated by reference; see § 1065.1010. See § 1065.701(d) for other allowed procedures.
b For testing at altitudes above 1219 m, the specified initial boiling point range is (23.9 to 40.6) °C and the specified volatility range is (52.0 to 55.2) kPa.
c ASTM D6550 prescribes measurement of olefin concentration in mass %. Multiply this result by 0.857 and round to the first decimal place to determine the olefin concentration in volume %.
d Calculate dry vapor pressure equivalent, DVPE , based on the measured total vapor pressure, p T , in kPa using the following equation: DVPE (kPa) = 0.956· p T − 2.39 or DVPE (psi) = 0.956· p T − 0.347. DVPE is intended to be equivalent to Reid Vapor Pressure using a different test method.
e For testing unrelated to evaporative emissions, the specified range is (55.2 to 63.4) kPa.
(d) Use the high-octane gasoline specified in paragraph (b) of this section only for engines or vehicles for which the manufacturer conditions the warranty on the use of premium gasoline.
§ 1065.715   Natural gas.
(a) Except as specified in paragraph (b) of this section, natural gas for testing must meet the specifications in the following table:
Table 1 of § 1065.715—Test Fuel Specifications for Natural Gas
a Demonstrate compliance with fuel specifications based on the reference procedures in ASTM D1945 (incorporated by reference, see § 1065.1010), or on other measurement procedures using good engineering judgment.
(b) In certain cases you may use test fuel not meeting the specifications in paragraph (a) of this section, as follows:
(1) You may use fuel that your in-use engines normally use, such as pipeline natural gas.
(2) You may use fuel meeting alternate specifications if the standard-setting part allows it.
(3) You may ask for approval to use fuel that does not meet the specifications in paragraph (a) of this section, but only if using the fuel would not adversely affect your ability to demonstrate compliance with the applicable standards in this chapter.
(c) When we conduct testing using natural gas, we will use fuel that meets the specifications in paragraph (a) of this section.
(d) At ambient conditions, natural gas must have a distinctive odor detectable down to a concentration in air not more than one-fifth the lower flammable limit.
§ 1065.720   Liquefied petroleum gas.
(a) Except as specified in paragraph (b) of this section, liquefied petroleum gas for testing must meet the specifications in the following table:
Table 1 to Paragraph ( a ) of § 1065.720—Test Fuel Specifications for Liquefied Petroleum Gas
a Incorporated by reference; see § 1065.1010. See § 1065.701(d) for other allowed procedures.
b If these two test methods yield different results, use the results from ASTM D1267.
c The test fuel must not yield a persistent oil ring when you add 0.3 ml of solvent residue mixture to a filter paper in 0.1 ml increments and examine it in daylight after two minutes.
(b) In certain cases you may use test fuel not meeting the specifications in paragraph (a) of this section, as follows:
(1) You may use fuel that your in-use engines normally use, such as commercial-quality liquefied petroleum gas.
(2) You may use fuel meeting alternate specifications if the standard-setting part allows it.
(3) You may ask for approval to use fuel that does not meet the specifications in paragraph (a) of this section, but only if using the fuel would not adversely affect your ability to demonstrate compliance with the applicable standards in this chapter.
(c) When we conduct testing using liquefied petroleum gas, we will use fuel that meets the specifications in paragraph (a) of this section.
(d) At ambient conditions, liquefied petroleum gas must have a distinctive odor detectable down to a concentration in air not more than one-fifth the lower flammable limit.
§ 1065.725   High-level ethanol-gasoline blends.
For testing vehicles capable of operating on a high-level ethanol-gasoline blend, create a test fuel as follows:
(a) Add ethanol to an E10 fuel meeting the specifications described in § 1065.710 until the ethanol content of the blended fuel is between 80 and 83 volume %.
(b) You may alternatively add ethanol to a gasoline base fuel with no ethanol if you can demonstrate that such a base fuel blended with the proper amount of ethanol would meet all the specifications for E10 test fuel described in § 1065.710, other than the ethanol content.
(c) The ethanol used for blending must be either denatured fuel ethanol meeting the specifications in 40 CFR 1090.270, or fuel-grade ethanol with no denaturant. Account for the volume of any denaturant when calculating volumetric percentages.
(d) The blended test fuel must have a dry vapor pressure equivalent between 41.5 and 45.1 kPa (6.0 and 6.5 psi) when measured using the procedure specified in § 1065.710. You may add commercial grade butane as needed to meet this specification.
§ 1065.735   Diesel exhaust fluid.
(a) Use commercially available diesel exhaust fluid that represents the product that will be used in your in-use engines.
(b) Diesel exhaust fluid for testing must generally conform to the specifications referenced in the definition of “diesel exhaust fluid” in § 1065.1001. Use marine-grade diesel exhaust fluid only for marine engines.
§ 1065.740   Lubricants.
(a) Use commercially available lubricating oil that represents the oil that will be used in your engine in use.
(b) You may use lubrication additives, up to the levels that the additive manufacturer recommends.
§ 1065.745   Coolants.
(a) You may use commercially available antifreeze mixtures or other coolants that will be used in your engine in use.
(b) For laboratory testing of liquid-cooled engines, you may use water with or without rust inhibitors.
(c) For coolants allowed in paragraphs (a) and (b) of this section, you may use rust inhibitors and additives required for lubricity, up to the levels that the additive manufacturer recommends.
§ 1065.750   Analytical gases.
Analytical gases must meet the accuracy and purity specifications of this section, unless you can show that other specifications would not affect your ability to show that you comply with all applicable emission standards.
(a) Subparts C, D, F, and J of this part refer to the following gas specifications:
(1) Use purified gases to zero measurement instruments and to blend with calibration gases. Use gases with contamination no higher than the highest of the following values in the gas cylinder or at the outlet of a zero-gas generator:
(i) 2% contamination, measured relative to the flow-weighted mean concentration expected at the standard. For example, if you would expect a flow-weighted CO concentration of 100.0 µmol/mol, then you would be allowed to use a zero gas with CO contamination less than or equal to 2.000 µmol/mol.
(ii) Contamination as specified in the following table:
Table 1 to Paragraph ( a )(1)( ii ) of § 1065.750-General Specifications for Purified Gases a
a We do not require these levels of purity to be NIST-traceable.
b The N 2 O limit applies only if the standard-setting part requires you to report N 2 O or certify to an N 2 O standard.
c The H 2 limit only applies for testing with H 2 fuel.
d The NH 3 limit only applies for testing with NH 3 fuel.
e The H 2 O limit only applies for water measurement according to § 1065.257.
(2) Use the following gases with a FID analyzer:
(i) FID fuel. Use FID fuel with a stated H 2 concentration of (0.39 to 0.41) mol/mol, balance He or N 2 , and a stated total hydrocarbon concentration of 0.05 µmol/mol or less. For GC-FIDs that measure methane (CH 4 ) using a FID fuel that is balance N 2 , perform the CH 4 measurement as described in SAE J1151 (incorporated by reference, see § 1065.1010).
(ii) FID burner air. Use FID burner air that meets the specifications of purified air in paragraph (a)(1) of this section. For field testing, you may use ambient air.
(iii) FID zero gas. Zero flame-ionization detectors with purified gas that meets the specifications in paragraph (a)(1) of this section, except that the purified gas O 2 concentration may be any value. Note that FID zero balance gases may be any combination of purified air and purified nitrogen. We recommend FID analyzer zero gases that contain approximately the expected flow-weighted mean concentration of O 2 in the exhaust sample during testing.
(iv) FID propane span gas. Span and calibrate THC FID with span concentrations of propane, C 3 H 8 . Calibrate on a carbon number basis of one (C 1 ). For example, if you use a C 3 H 8 span gas of concentration 200 µmol/mol, span a FID to respond with a value of 600 µmol/mol. Note that FID span balance gases may be any combination of purified air and purified nitrogen. We recommend FID analyzer span gases that contain approximately the flow-weighted mean concentration of O 2 expected during testing. If the expected O 2 concentration in the exhaust sample is zero, we recommend using a balance gas of purified nitrogen.
(v) FID CH 4 span gas. If you always span and calibrate a CH 4 FID with a nonmethane cutter, then span and calibrate the FID with span concentrations of CH 4 . Calibrate on a carbon number basis of one (C 1 ). For example, if you use a CH 4 span gas of concentration 200 µmol/mol, span a FID to respond with a value of 200 µmol/mol. Note that FID span balance gases may be any combination of purified air and purified nitrogen. We recommend FID analyzer span gases that contain approximately the expected flow-weighted mean concentration of O 2 in the exhaust sample during testing. If the expected O 2 concentration in the exhaust sample is zero, we recommend using a balance gas of purified nitrogen.
(3) Use the following gas mixtures, with gases traceable within ±1% of the NIST-accepted gas standard value or other gas standards we approve:
(i) CH 4 , balance purified air and/or N 2 (as applicable).
(ii) C 2 H 6 , balance purified air and/or N 2 (as applicable).
(iii) C 3 H 8 , balance purified air and/or N 2 (as applicable).
(iv) CO, balance purified N 2 .
(v) CO 2 , balance purified N 2 .
(vi) NO, balance purified N 2 .
(vii) NO 2 , balance purified air.
(viii) O 2 , balance purified N 2 .
(ix) C 3 H 8 , CO, CO 2 , NO, balance purified N 2 .
(x) C 3 H 8 , CH 4 , CO, CO 2 , NO, balance purified N 2 .
(xi) N 2 O, balance purified air and/or N 2 (as applicable).
(xii) CH 4 , C 2 H 6 , balance purified air and/or N 2 (as applicable).
(xiii) CH 4 , CH 2 O 2 , C 2 H 2 , C 2 H 4 , C 2 H 4 O, C 2 H 6 , C 3 H 8 , C 3 H 6 , CH 4 O, and C 4 H 10 . You may omit individual gas constituents from this gas mixture. If your gas mixture contains oxygenated hydrocarbons, your gas mixture must be in balance purified N 2 , otherwise you may use balance purified air.
(4) You may use gases for species other than those listed in paragraph (a)(3) of this section (such as methanol in air, which you may use to determine response factors), as long as they are traceable to within ±3% of the NIST-accepted value or other similar standards we approve, and meet the stability requirements of paragraph (b) of this section.
(5) You may generate your own calibration gases using a precision blending device, such as a gas divider, to dilute gases with purified N 2 or purified air. If your gas divider meets the specifications in § 1065.248, and the gases being blended meet the requirements of paragraphs (a)(1) and (3) of this section, the resulting blends are considered to meet the requirements of this paragraph (a).
(6) If you measure H 2 O using an FTIR analyzer, generate H 2 O calibration gases with a humidity generator using one of the options in this paragraph (a)(6). Use good engineering judgment to prevent condensation in the transfer lines, fittings, or valves from the humidity generator to the FTIR analyzer. Design your system so the wall temperatures in the transfer lines, fittings, and valves from the point where the mole fraction of H 2 O in the humidified calibration gas, x H2Oref , is measured to the analyzer are at a temperature of (110 to 202)  °C. Calibrate the humidity generator upon initial installation, within 370 days before verifying the H 2 O measurement of the FTIR, and after major maintenance. Use the uncertainties from the calibration of the humidity generator's measurements and follow NIST Technical Note 1297 (incorporated by reference, see § 1065.1010) to verify that the amount of H 2 O in the calibration gas, x H2Oref , is determined within ±3% uncertainty, U xH2O . If the humidity generator requires assembly before use, after assembly follow the instrument manufacturer's instructions to check for leaks. You may generate the H 2 O calibration gas using one of the following options:
(i) Bubble gas that meets the requirements of paragraph (a)(1) of this section through distilled H 2 O in a sealed vessel. Adjust the amount of H 2 O in the calibration gas by changing the temperature of the H 2 O in the sealed vessel. Determine absolute pressure, p abs , and dewpoint, T dew , of the humidified gas leaving the sealed vessel. Calculate the amount of H 2 O in the calibration gas as described in § 1065.645(a) and (b). Calculate the uncertainty of the amount of H 2 O in the calibration gas, U xH2O , using the following equations:
Example:
Using Eq. 1065.645-1,
(ii) Use a device that introduces a measured flow of distilled H 2 O as vapor into a measured flow of gas that meets the requirements of paragraph (a)(1) of this section. Determine the molar flows of gas and H 2 O that are mixed to generate the calibration gas.
(A) Calculate the amount of H 2 O in the calibration gas as follows:
(B) Calculate the uncertainty of the amount of H 2 O in the generated calibration gas, U xH2O, using the following equations:
(C) The following example is a solution for using the equations in paragraph (a)(6)(ii)(B) of this section:
(b) Record the concentration of any calibration gas standard and its expiration date specified by the gas supplier.
(1) Do not use any calibration gas standard after its expiration date, except as allowed by paragraph (b)(2) of this section.
(2) Calibration gases may be relabeled and used after their expiration date as follows:
(i) Alcohol/carbonyl calibration gases used to determine response factors according to subpart I of this part may be relabeled as specified in subpart I of this part.
(ii) Other gases may be relabeled and used after the expiration date only if we approve it in advance.
(c) Transfer gases from their source to analyzers using components that are dedicated to controlling and transferring only those gases. For example, do not use a regulator, valve, or transfer line for zero gas if those components were previously used to transfer a different gas mixture. We recommend that you label regulators, valves, and transfer lines to prevent contamination. Note that even small traces of a gas mixture in the dead volume of a regulator, valve, or transfer line can diffuse upstream into a high-pressure volume of gas, which would contaminate the entire high-pressure gas source, such as a compressed-gas cylinder.
(d) To maintain stability and purity of gas standards, use good engineering judgment and follow the gas standard supplier's recommendations for storing and handling zero, span, and calibration gases. For example, it may be necessary to store bottles of condensable gases in a heated environment.
§ 1065.790   Mass standards.
(a) PM balance calibration weights. Use PM balance calibration weights that are certified as NIST-traceable within ±0.1% uncertainty. Make sure your highest calibration weight has no more than ten times the mass of an unused PM-sample medium.
(b) Dynamometer, fuel mass scale, and DEF mass scale calibration weights. Use dynamometer and mass scale calibration weights that are certified as NIST-traceable within ±0.1% uncertainty.
§ 1065.801   Applicability.
(a) This subpart applies for testing with oxygenated fuels. Unless the standard-setting part specifies otherwise, the requirements of this subpart do not apply for fuels that contain less than 25% oxygenated compounds by volume. For example, you generally do not need to follow the requirements of this subpart for tests performed using a fuel containing 10% ethanol and 90% gasoline, but you must follow these requirements for tests performed using a fuel containing 85% ethanol and 15% gasoline.
(b) Section 1065.805 applies for all other testing that requires measurement of any alcohols or carbonyls.
(c) This subpart specifies sampling procedures and calculations that are different than those used for non-oxygenated fuels. All other test procedures of this part 1065 apply for testing with oxygenated fuels.
§ 1065.805   Sampling system.
(a) Dilute engine exhaust, and use batch sampling to collect proportional flow-weighted dilute samples of the applicable alcohols and carbonyls. You may not use raw sampling for alcohols and carbonyls.
(b) You may collect background samples for correcting dilution air for background concentrations of alcohols and carbonyls.
(c) Maintain sample temperatures within the dilution tunnel, probes, and sample lines high enough to prevent aqueous condensation up to the point where a sample is collected to prevent loss of the alcohols and carbonyls by dissolution in condensed water. Use good engineering judgment to ensure that surface reactions of alcohols and carbonyls do not occur, as surface decomposition of methanol has been shown to occur at temperatures greater than 120 °C in exhaust from methanol-fueled engines.
(d) You may bubble a sample of the exhaust through water to collect alcohols for later analysis. You may also use a photoacoustic analyzer to quantify ethanol and methanol in an exhaust sample as described in § 1065.269.
(e) Sample the exhaust through cartridges impregnated with 2,4-dinitrophenylhydrazine to collect carbonyls for later analysis. If the standard-setting part specifies a duty cycle that has multiple test intervals (such as multiple engine starts or an engine-off soak phase), you may proportionally collect a single carbonyl sample for the entire duty cycle. For example, if the standard-setting part specifies a six-to-one weighting of hot-start to cold-start emissions, you may collect a single carbonyl sample for the entire duty cycle by using a hot-start sample flow rate that is six times the cold-start sample flow rate.
(f) You may sample alcohols or carbonyls using “California Non-Methane Organic Gas Test Procedures” (incorporated by reference, see § 1065.1010). If you use this method, follow its calculations to determine the mass of the alcohol/carbonyl in the exhaust sample, but follow subpart G of this part for all other calculations (40 CFR part 1066, subpart G, for vehicle testing).
(g) Use good engineering judgment to sample other oxygenated hydrocarbon compounds in the exhaust.
§ 1065.845   Response factor determination.
Since FID analyzers generally have an incomplete response to alcohols and carbonyls, determine each FID analyzer's alcohol/carbonyl response factor ( RF OHCi[THC-FID] ) after FID optimization to subtract those responses from the FID reading. Use the most recently determined alcohol/carbonyl response factors to compensate for alcohol/carbonyl response. You are not required to determine the response factor for a compound unless you will subtract its response to compensate for a response.
(a) You may generate response factors as described in paragraph (b) of this section, or you may use the following default response factors, consistent with good engineering judgment:
Table 1 of § 1065.845—Default Values for THC FID Response Factor Relative to Propane on a C 1 -Equivalent Basis
(b) Determine the alcohol/carbonyl response factors as follows:
(1) Select a C 3 H 8 span gas that meets the specifications of § 1065.750. Note that FID zero and span balance gases may be any combination of purified air or purified nitrogen that meets the specifications of § 1065.750. We recommend FID analyzer zero and span gases that contain approximately the flow-weighted mean concentration of O 2 expected during testing. Record the C 3 H 8 concentration of the gas.
(2) Select or prepare an alcohol/carbonyl calibration gas that meets the specifications of § 1065.750 and has a concentration typical of the peak concentration expected at the hydrocarbon standard. Record the calibration concentration of the gas.
(3) Start and operate the FID analyzer according to the manufacturer's instructions.
(4) Confirm that the FID analyzer has been calibrated using C 3 H 8 . Calibrate on a carbon number basis of one (C 1 ). For example, if you use a C 3 H 8 span gas of concentration 200 µmol/mol, span the FID to respond with a value of 600 µmol/mol.
(5) Zero the FID. Note that FID zero and span balance gases may be any combination of purified air or purified nitrogen that meets the specifications of § 1065.750. We recommend FID analyzer zero and span gases that contain approximately the flow-weighted mean concentration of O 2 expected during testing.
(6) Span the FID with the C 3 H 8 span gas that you selected under paragraph (a)(1) of this section.
(7) Introduce at the inlet of the FID analyzer the alcohol/carbonyl calibration gas that you selected under paragraph (a)(2) of this section.
(8) Allow time for the analyzer response to stabilize. Stabilization time may include time to purge the analyzer and to account for its response.
(9) While the analyzer measures the alcohol/carbonyl concentration, record 30 seconds of sampled data. Calculate the arithmetic mean of these values.
(10) Divide the mean measured concentration by the recorded span concentration of the alcohol/carbonyl calibration gas on a C 1 -equivalent basis. The result is the FID analyzer's response factor for alcohol/carbonyl, RF OHCi[THC-FID] on a C 1 -equivalent basis.
(c) Alcohol/carbonyl calibration gases must remain within ±2% of the labeled concentration. You must demonstrate the stability based on a quarterly measurement procedure with a precision of ±2% percent or another method that we approve. Your measurement procedure may incorporate multiple measurements. If the true concentration of the gas changes deviates by more than ±2%, but less than ±10%, the gas may be relabeled with the new concentration.
§ 1065.850   Calculations.
Use the calculations specified in § 1065.665 to determine THCE or NMHCE and the calculations specified in 40 CFR 1066.635 to determine NMOG.
§ 1065.901   Applicability.
(a) Field testing. This subpart specifies procedures for field-testing engines to determine brake-specific emissions and mass rate emissions using portable emission measurement systems (PEMS). These procedures are designed primarily for in-field measurements of engines that remain installed in vehicles or equipment the field. Field-test procedures apply to your engines only as specified in the standard-setting part.
(b) Laboratory testing. You may use PEMS for any testing in a laboratory or similar environment without restriction or prior approval if the PEMS meets all applicable specifications for laboratory testing. You may also use PEMS for any testing in a laboratory or similar environment if we approve it in advance, subject to the following provisions:
(1) Follow the laboratory test procedures specified in this part 1065, according to § 1065.905(e).
(2) Do not apply any PEMS-related field-testing adjustments or measurement allowances to laboratory emission results or standards.
(3) Do not use PEMS for laboratory measurements if it prevents you from demonstrating compliance with the applicable standards in this chapter. Some of the PEMS requirements in this part 1065 are less stringent than the corresponding laboratory requirements. Depending on actual PEMS performance, you might therefore need to account for some additional measurement uncertainty when using PEMS for laboratory testing. If we ask, you must show us by engineering analysis that any additional measurement uncertainty due to your use of PEMS for laboratory testing is offset by the extent to which your engine's emissions are below the applicable standards in this chapter. For example, you might show that PEMS versus laboratory uncertainty represents 5% of the standard, but your engine's deteriorated emissions are at least 20% below the standard for each pollutant.
§ 1065.905   General provisions.
(a) General. Unless the standard-setting part specifies deviations from the provisions of this subpart, field testing and laboratory testing with PEMS must conform to the provisions of this subpart. Use good engineering judgment when testing with PEMS to ensure proper function of the instruments under test conditions. For example, this may require additional maintenance or calibration for field testing or may require verification after moving the PEMS unit.
(b) Field-testing scope. Field testing conducted under this subpart may include any normal in-use operation of an engine.
(c) Field testing and the standard-setting part. This subpart J specifies procedures for field-testing various categories of engines. See the standard-setting part for specific provisions for a particular type of engine. Before using this subpart's procedures for field testing, read the standard-setting part to answer at least the following questions:
(1) How many engines must I test in the field?
(2) How many times must I repeat a field test on an individual engine?
(3) How do I select vehicles for field testing?
(4) What maintenance steps may I take before or between tests?
(5) What data are needed for a single field test on an individual engine?
(6) What are the limits on ambient conditions for field testing? Note that the ambient condition limits in § 1065.520 do not apply for field testing. Field testing may occur at any ambient temperature, pressure, and humidity unless otherwise specified in the standard-setting part.
(7) Which exhaust constituents do I need to measure?
(8) How do I account for crankcase emissions?
(9) Which engine and ambient parameters do I need to measure?
(10) How do I process the data recorded during field testing to determine if my engine meets field-testing standards? How do I determine individual test intervals? Note that “test interval” is defined in subpart K of this part 1065.
(11) Should I warm up the test engine before measuring emissions, or do I need to measure cold-start emissions during a warm-up segment of in-use operation?
(12) Do any unique specifications apply for test fuels?
(13) Do any special conditions invalidate parts of a field test or all of a field test?
(14) Does any special measurement allowance apply to field-test emission results or standards, based on using PEMS for field-testing versus using laboratory equipment and instruments for laboratory testing?
(15) Do results of initial field testing trigger any requirement for additional field testing or laboratory testing?
(16) How do I report field-testing results?
(d) Field testing and this part 1065. Use the following specifications for field testing:
(1) Use the applicability and general provisions of subpart A of this part.
(2) Use equipment specifications in § 1065.101 and in the sections from § 1065.140 to the end of subpart B of this part, with the exception of §§ 1065.140(e)(1) and (4), 1065.170(c)(1)(vi), and 1065.195(c). Section 1065.910 identifies additional equipment that is specific to field testing.
(i) For PM samples, configure dilution systems as follows:
(A) Use good engineering judgment to control dilution air temperature. If you choose to directly and actively control dilution air temperature, set the temperature to 25 °C.
(B) Control sample temperature to a (32 to 62) °C tolerance, as measured anywhere within 20 cm upstream or downstream of the PM storage media (such as a filter or oscillating crystal), where the tolerance applies only during sampling.
(C) Maintain filter face velocity to a (5 to 100) cm/s tolerance for flow-through media. Compliance with this provision can be verified by engineering analysis. This provision does not apply for non-flow-through media.
(ii) For inertial PM balances, there is no requirement to control the stabilization environment temperature or dewpoint.
(3) Use measurement instruments in subpart C of this part, except as specified in § 1065.915.
(4) Use calibrations and verifications in subpart D of this part, except as specified in § 1065.920. Section 1065.920 also specifies additional calibrations and verifications for field testing.
(5) Use the provisions of the standard-setting part for selecting and maintaining engines in the field instead of the specifications in subpart E of this part.
(6) Use the procedures in §§ 1065.930 and 1065.935 to start and run a field test. If you use a gravimetric balance for PM, weigh PM samples according to §§ 1065.590 and 1065.595.
(7) Use the calculations in subpart G of this part to calculate emissions over each test interval. Note that “test interval” is defined in subpart K of this part 1065, and that the standard setting part indicates how to determine test intervals for your engine.
Section 1065.940 specifies additional calculations for field testing. Use any calculations specified in the standard-setting part to determine if your engines meet the field-testing standards. The standard-setting part may also contain additional calculations that determine when further field testing is required.
(8) Use a typical in-use fuel meeting the specifications of § 1065.701(d).
(9) Use the lubricant and coolant specifications in §§ 1065.740 and 1065.745.
(10) Use the analytical gases and other calibration standards in § 1065.750 and § 1065.790.
(11) If you are testing with oxygenated fuels, use the procedures specified for testing with oxygenated fuels in subpart I of this part.
(12) Apply the definitions and reference materials in subpart K of this part.
(e) Laboratory testing using PEMS. You may use PEMS for testing in a laboratory as described in § 1065.901(b). Use the following procedures and specifications when using PEMS for laboratory testing:
(1) Use the applicability and general provisions of subpart A of this part.
(2) Use equipment specifications in subpart B of this part. Section 1065.910 specifies additional equipment specific to testing with PEMS.
(3) Use measurement instruments in subpart C of this part, except as specified in § 1065.915.
(4) Use calibrations and verifications in subpart D of this part, except as specified in § 1065.920. Section 1065.920 also specifies additional calibration and verifications for PEMS.
(5) Use the provisions of § 1065.401 for selecting engines for testing. Use the provisions of subpart E of this part for maintaining engines, except as specified in the standard-setting part.
(6) Use the procedures in subpart F of this part and in the standard-setting part to start and run a laboratory test.
(7) Use the calculations in subpart G of this part to calculate emissions over the applicable duty cycle. Section 1065.940 specifies additional calculations for testing with PEMS.
(8) Use a fuel meeting the specifications of subpart H of this part, as specified in the standard-setting part.
(9) Use the lubricant and coolant specifications in §§ 1065.740 and 1065.745.
(10) Use the analytical gases and other calibration standards in §§ 1065.750 and 1065.790.
(11) If you are testing with oxygenated fuels, use the procedures specified for testing with oxygenated fuels in subpart I of this part.
(12) Apply the definitions and reference materials in subpart K of this part.
(f) Summary . The following table summarizes the requirements of paragraphs (d) and (e) of this section:
Table 1 of § 1065.905—Summary of Testing Requirements Specified Outside of This Subpart
a Refer to paragraphs (d) and (e) of this section for complete specifications.
§ 1065.910   PEMS auxiliary equipment for field testing.
For field testing you may use various types of auxiliary equipment to attach PEMS to a vehicle or engine and to power PEMS.
(a) When you use PEMS, you may route engine intake air or exhaust through a flow meter. Route the engine intake air or exhaust as follows:
(1) Flexible connections. Use short flexible connectors where necessary.
(i) You may use flexible connectors to enlarge or reduce the pipe diameters to match that of your test equipment.
(ii) We recommend that you use flexible connectors that do not exceed a length of three times their largest inside diameter.
(iii) We recommend that you use four-ply silicone-fiberglass fabric with a temperature rating of at least 315 °C for flexible connectors. You may use connectors with a spring-steel wire helix for support and you may use Nomex TM coverings or linings for durability. You may also use any other nonreactive material with equivalent permeation-resistance and durability, as long as it seals tightly.
(iv) Use stainless-steel hose clamps to seal flexible connectors, or use clamps that seal equivalently.
(v) You may use additional flexible connectors to connect to flow meters.
(2) Tubing . We recommend using rigid 300 series stainless steel tubing to connect between flexible connectors. Tubing may be straight or bent to accommodate vehicle geometry. You may use “T” or “Y” fittings to join multiple connections, or you may cap or plug redundant flow paths if the engine manufacturer recommends it.
(3) Flow restriction. Use flow meters, connectors, and tubing that do not increase flow restriction so much that it exceeds the manufacturer's maximum specified value. You may verify this at the maximum exhaust flow rate by measuring pressure at the manufacturer-specified location with your system connected. You may also perform an engineering analysis to verify an acceptable configuration, taking into account the maximum exhaust flow rate expected, the field test system's flexible connectors, and the tubing's characteristics for pressure drops versus flow.
(b) Locate the PEMS to minimize the effects of the following parameters or place the PEMS in an environmental enclosure that minimizes the effect of these parameters on the emission measurement:
(1) Ambient temperature changes.
(2) Electromagnetic radiation.
(3) Mechanical shock and vibration.
(c) Use mounting hardware as required for securing flexible connectors, ambient sensors, and other equipment. Use structurally sound mounting points such as vehicle frames, trailer hitch receivers, walk spaces, and payload tie-down fittings. We recommend mounting hardware such as clamps, suction cups, and magnets that are specifically designed for your application. We also recommend considering mounting hardware such as commercially available bicycle racks, trailer hitches, and luggage racks where applicable.
(d) Field testing may require portable electrical power to run your test equipment. Power your equipment, as follows:
(1) You may use electrical power from the vehicle, equipment, or vessel, up to the highest power level, such that all the following are true:
(i) The power system is capable of safely supplying power, such that the power demand for testing does not overload the power system.
(ii) The engine emissions do not change significantly as a result of the power demand for testing.
(iii) The power demand for testing does not increase output from the engine by more than 1% of its maximum power.
(2) You may install your own portable power supply. For example, you may use batteries, fuel cells, a portable generator, or any other power supply to supplement or replace your use of vehicle power. You may connect an external power source directly to the vehicle's, vessel's, or equipment's power system; however, you must not supply power to the vehicle's power system in excess of 1% of the engine's maximum power.
§ 1065.915   PEMS instruments.
(a) Instrument specifications . We recommend that you use PEMS that meet the specifications of subpart C of this part. For unrestricted use of PEMS in a laboratory or similar environment, use a PEMS that meets the same specifications as each lab instrument it replaces. For field testing or for testing with PEMS in a laboratory or similar environment, under the provisions of § 1065.905(b), the specifications in the following table apply instead of the specifications in Table 1 of § 1065.205:
Table 1 of § 1065.915—Recommended Minimum PEMS Measurement Instrument Performance
a Accuracy, repeatability, and noise are all determined with the same collected data, as described in § 1065.305, and based on absolute values. “pt.” refers to the overall flow-weighted mean value expected at the standard; “max.” refers to the peak value expected at the standard over any test interval, not the maximum of the instrument's range; “meas” refers to the actual flow-weighted mean measured over any test interval.
(b) Redundant measurements. For all PEMS described in this subpart, you may use data from multiple instruments to calculate test results for a single test. If you use redundant systems, use good engineering judgment to use multiple measured values in calculations or to disregard individual measurements. Note that you must keep your results from all measurements, as described in § 1065.25. This requirement applies whether or not you actually use the measurements in your calculations.
(c) Field-testing ambient effects on PEMS. We recommend that you use PEMS that are only minimally affected by ambient conditions such as temperature, pressure, humidity, physical orientation, mechanical shock and vibration, electromagnetic radiation, and ambient hydrocarbons. Follow the PEMS manufacturer's instructions for proper installation to isolate PEMS from ambient conditions that affect their performance. If a PEMS is inherently affected by ambient conditions that you cannot control, you may monitor those conditions and adjust the PEMS signals to compensate for the ambient effect. The standard-setting part may also specify the use of one or more field-testing adjustments or measurement allowances that you apply to results or standards to account for ambient effects on PEMS.
(d) ECM signals. You may use signals from the engine's electronic control module (ECM) in place of values measured by individual instruments within a PEMS, subject to the following provisions:
(1) Recording ECM signals. If your ECM updates a broadcast signal more or less frequently than 1 Hz, process data as follows:
(i) If your ECM updates a broadcast signal more frequently than 1 Hz, use PEMS to sample and record the signal's value more frequently. Calculate and record the 1 Hz mean of the more frequently updated data.
(ii) If your ECM updates a broadcast signal less frequently than 1 Hz, use PEMS to sample and record the signal's value at the most frequent rate. Linearly interpolate between recorded values and record the interpolated values at 1 Hz.
(iii) Optionally, you may use PEMS to electronically filter the ECM signals to meet the rise time and fall time specifications in Table 1 of this section. Record the filtered signal at 1 Hz.
(2) Omitting ECM signals. Replace any discontinuous or irrational ECM data with linearly interpolated values from adjacent data.
(3) Aligning ECM signals with other data. You must perform time-alignment and dispersion of ECM signals, according to PEMS manufacturer instructions and using good engineering judgment.
(4) ECM signals for determining test intervals. You may use any combination of ECM signals, with or without other measurements, to determine the start-time and end-time of a test interval.
(5) ECM signals for determining brake-specific emissions. You may use any combination of ECM signals, with or without other measurements, to estimate engine speed, torque, brake-specific fuel consumption (BSFC, in units of mass of fuel per kW-hr), and fuel rate for use in brake-specific emission calculations. We recommend that the overall performance of any speed, torque, or BSFC estimator should meet the performance specifications in Table 1 of this section. We recommend using one of the following methods:
(i) Speed. Use the engine speed signal directly from the ECM. This signal is generally accurate and precise. You may develop your own speed algorithm based on other ECM signals.
(ii) Torque. Use one of the following:
(A) ECM torque. Use the engine-torque signal directly from the ECM, if broadcast. Determine if this signal is proportional to indicated torque or brake torque. If it is proportional to indicated torque, subtract friction torque from indicated torque and record the result as brake torque. Friction torque may be a separate signal broadcast from the ECM or you may have to determine it from laboratory data as a function of engine speed.
(B) ECM %-load. Use the %-load signal directly from the ECM, if broadcast. Determine if this signal is proportional to indicated torque or brake torque. If it is proportional to indicated torque, subtract the minimum %-load value from the %-load signal. Multiply this result by the maximum brake torque at the corresponding engine speed. Maximum brake torque versus speed information is commonly published by the engine manufacturer.
(C) Your algorithms. You may develop and use your own combination of ECM signals to determine torque.
(iii) BSFC. Use one of the following:
(A) Use ECM engine speed and ECM fuel flow signals to interpolate brake-specific fuel consumption data, which might be available from an engine laboratory as a function of ECM engine speed and ECM fuel signals.
(B) Use a single BSFC value that approximates the BSFC value over a test interval (as defined in subpart K of this part). This value may be a nominal BSFC value for all engine operation determined over one or more laboratory duty cycles, or it may be any other BSFC that you determine. If you use a nominal BSFC, we recommend that you select a value based on the BSFC measured over laboratory duty cycles that best represent the range of engine operation that defines a test interval for field-testing. You may use the methods of this paragraph (d)(5)(iii)(B) only if it does not adversely affect your ability to demonstrate compliance with applicable standards.
(C) You may develop and use your own combination of ECM signals to determine BSFC.
(iv) ECM fuel rate. Use the fuel rate signal directly from the ECM and chemical balance to determine the molar flow rate of exhaust. Use § 1065.655(d) to determine the carbon mass fraction of fuel. You may alternatively develop and use your own combination of ECM signals to determine fuel mass flow rate.
(v) Other ECM signals. You may ask to use other ECM signals for determining brake-specific emissions, such as ECM air flow. We must approve the use of such signals in advance.
(6) Permissible deviations. ECM signals may deviate from the specifications of this part 1065, but the expected deviation must not prevent you from demonstrating that you meet the applicable standards in this chapter. For example, your emission results may be sufficiently below an applicable standard, such that the deviation would not significantly change the result. As another example, a very low engine-coolant temperature may define a logical statement that determines when a test interval may start. In this case, even if the ECM's sensor for detecting coolant temperature was not very accurate or repeatable, its output would never deviate so far as to significantly affect when a test interval may start.
§ 1065.920   PEMS calibrations and verifications.
(a) Subsystem calibrations and verifications. Use all the applicable calibrations and verifications in subpart D of this part, including the linearity verifications in § 1065.307, to calibrate and verify PEMS. Note that a PEMS does not have to meet the system-response and updating-recording verifications of § 1065.308 and § 1065.309 if it meets the overall verification described in paragraph (b) of this section or if it measures PM using any method other than that described in § 1065.170(c)(1). This section does not apply to ECM signals. Note that because the regulations of this part require you to use good engineering judgment, it may be necessary to perform additional verifications and analysis. It may also be necessary to limit the range of conditions under which the PEMS can be used or to include specific additional maintenance to ensure that it functions properly under the test conditions. As provided in 40 CFR 1068.5, we will deem your system to not meet the requirements of this section if we determine that you did not use good engineering judgment to verify the measurement equipment. We may also deem your system to meet these requirements only under certain test conditions. If we ask for it, you must send us a summary of your verifications. We may also ask you to provide additional information or analysis to support your conclusions.
(b) Overall verification. This paragraph (b) specifies methods and criteria for verifying the overall performance of systems not fully compliant with requirements that apply for laboratory testing. Maintain records to show that the particular make, model, and configuration of your PEMS meets this verification. You may rely on data and other information from the PEMS manufacturer. However, we recommend that you generate your own records to show that your specific PEMS meets this verification. If you upgrade or change the configuration of your PEMS, your record must show that your new configuration meets this verification. The verification required by this section consists of operating an engine over a duty cycle in the laboratory and statistically comparing data generated and recorded by the PEMS with data simultaneously generated and recorded by laboratory equipment as follows:
(1) Mount an engine on a dynamometer for laboratory testing. Prepare the laboratory and PEMS for emission testing, as described in this part, to get simultaneous measurements. We recommend selecting an engine with emission levels close to the applicable duty-cycle standards, if possible.
(2) Select or create a duty cycle that has all the following characteristics:
(i) Engine operation that represents normal in-use speeds, loads, and degree of transient activity. Consider using data from previous field tests to generate a cycle.
(ii) A duration of (6 to 9) hours.
(3) Starting with a warmed-up engine, run a valid emission test with the duty cycle from paragraph (b)(2) of this section. The laboratory and PEMS must both meet applicable validation requirements, such as drift validation, hydrocarbon contamination validation, and proportional validation.
(4) Determine the brake-specific emissions and mass rate emissions, as applicable, for each test interval for both laboratory and the PEMS measurements, as follows:
(i) For both laboratory and PEMS measurements, use identical values to determine the beginning and end of each test interval.
(ii) For both laboratory and PEMS measurements, use identical values to determine total work over each test interval.
(iii) If the standard-setting part specifies the use of a measurement allowance for field testing, also apply the measurement allowance during calibration using good engineering judgment. If the measurement allowance is normally added to the standard, this means you must subtract the measurement allowance from measured PEMS emission results.
(iv) Round results to the same number of significant digits as the standard.
(5) For each test interval and emission, subtract the lab result from the PEMS result.
(6) The PEMS passes the verification of this paragraph (b) if any one of the following are true for each constituent:
(i) 91% or more of the differences are zero or less than zero.
(ii) The entire set of test-interval results passes the 95% confidence alternate-procedure statistics for field testing ( t -test and F -test) specified in § 1065.12.
§ 1065.925   PEMS preparation for field testing.
Take the following steps to prepare PEMS for field testing:
(a) Verify that ambient conditions at the start of the test are within the limits specified in the standard-setting part. Continue to monitor these values to determine if ambient conditions exceed the limits during the test.
(b) Install a PEMS and any accessories needed to conduct a field test.
(c) Power the PEMS and allow pressures, temperatures, and flows to stabilize to their operating set points.
(d) Bypass or purge any gaseous sampling PEMS instruments with ambient air until sampling begins to prevent system contamination from excessive cold-start emissions.
(e) Conduct calibrations and verifications.
(f) Operate any PEMS dilution systems at their expected flow rates using a bypass.
(g) If you use a gravimetric balance to determine whether an engine meets an applicable PM standard, follow the procedures for PM sample preconditioning and tare weighing as described in § 1065.590. Operate the PM-sampling system at its expected flow rates using a bypass.
(h) Verify the amount of contamination in the PEMS HC sampling system before the start of the field test as follows:
(1) Select the HC analyzer range for measuring the maximum concentration expected at the HC standard.
(2) Zero the HC analyzers using a zero gas or ambient air introduced at the analyzer port. When zeroing a FID, use the FID's burner air that would be used for in-use measurements (generally either ambient air or a portable source of burner air).
(3) Span the HC analyzer using span gas introduced at the analyzer port.
(4) Overflow zero or ambient air at the HC probe inlet or into a tee near the probe outlet.
(5) Measure the HC concentration in the sampling system:
(i) For continuous sampling, record the mean HC concentration as overflow zero air flows.
(ii) For batch sampling, fill the sample medium and record its mean concentration.
(6) Record this value as the initial HC concentration, x THCinit , and use it to correct measured values as described in § 1065.660.
(7) If the initial HC concentration exceeds the greater of the following values, determine the source of the contamination and take corrective action, such as purging the system or replacing contaminated portions:
(i) 2% of the flow-weighted mean concentration expected at the standard or measured during testing.
(ii) 2 µmol/mol.
(8) If corrective action does not resolve the deficiency, you may use a contaminated HC system if it does not prevent you from demonstrating compliance with the applicable emission standards.
§ 1065.930   Engine starting, restarting, and shutdown.
Unless the standard-setting part specifies otherwise, start, restart, and shut down the test engine for field testing as follows:
(a) Start or restart the engine as described in the owners manual.
(b) If the engine does not start after 15 seconds of cranking, stop cranking and determine the reason it failed to start. However, you may crank the engine longer than 15 seconds, as long as the owners manual or the service-repair manual describes the longer cranking time as normal.
(c) Respond to engine stalling with the following steps:
(1) If the engine stalls during a required warm-up before emission sampling begins, restart the engine and continue warm-up.
(2) If the engine stalls at any other time after emission sampling begins, restart the engine and continue testing.
(d) Shut down and restart the engine according to the manufacturer's specifications, as needed during normal operation in-use, but continue emission sampling until the field test is complete.
§ 1065.935   Emission test sequence for field testing.
(a) Time the start of field testing as follows:
(1) If the standard-setting part requires only hot-stabilized emission measurements, operate the engine in-use until the engine coolant, block, or head absolute temperature is within ±10% of its mean value for the previous 2 min or until an engine thermostat controls engine temperature with coolant or air flow.
(2) If the standard-setting part requires hot-start emission measurements, shut down the engine after at least 2 min at the temperature tolerance specified in paragraph (a)(1) of this section. Start the field test within 20 min of engine shutdown.
(3) If the standard-setting part requires cold-start emission measurements, proceed to the steps specified in paragraph (b) of this section.
(b) Take the following steps before emission sampling begins:
(1) For batch sampling, connect clean storage media, such as evacuated bags or tare-weighed PM sample media.
(2) Operate the PEMS according to the instrument manufacturer's instructions and using good engineering judgment.
(3) Operate PEMS heaters, dilution systems, sample pumps, cooling fans, and the data-collection system.
(4) Pre-heat or pre-cool PEMS heat exchangers in the sampling system to within their tolerances for operating temperatures.
(5) Allow all other PEMS components such as sample lines, filters, and pumps to stabilize at operating temperature.
(6) Verify that no significant vacuum-side leak exists in the PEMS, as described in § 1065.345.
(7) Adjust PEMS flow rates to desired levels, using bypass flow if applicable.
(8) Zero and span all PEMS gas analyzers using NIST-traceable gases that meet the specifications of § 1065.750.
(c) Start testing as follows:
(1) Before the start of the first test interval, zero or re-zero any PEMS electronic integrating devices, as needed.
(2) If the engine is already running and warmed up and starting is not part of field testing, start the field test by simultaneously starting to sample exhaust, record engine and ambient data, and integrate measured values using a PEMS.
(3) If engine starting is part of field testing, start field testing by simultaneously starting to sample from the exhaust system, record engine and ambient data, and integrate measured values using a PEMS. Then start the engine.
(d) Continue the test as follows:
(1) Continue to sample exhaust, record data and integrate measured values throughout normal in-use operation of the engine.
(2) Between each test interval, zero or re-zero any electronic integrating devices, and reset batch storage media, as needed.
(3) The engine may be stopped and started, but continue to sample emissions throughout the entire field test.
(4) Conduct periodic verifications such as zero and span verifications on PEMS gas analyzers and use these to correct for drift according to paragraph (g) of this section. Do not include data recorded during verifications in emission calculations. Conduct the verifications as follows:
(i) For PEMS gas analyzers used to determine NTE emission values, perform verifications as recommended by the PEMS manufacturer or as indicated by good engineering judgment.
(ii) For PEMS gas analyzers used to determine bin emission values, perform zero verifications at least hourly using purified air. Perform span verification at the end of the shift-day or more frequently as recommended by the PEMS manufacturer or as indicated by good engineering judgment.
(5) You may periodically condition and analyze batch samples in-situ, including PM samples; for example you may condition an inertial PM balance substrate if you use an inertial balance to measure PM.
(6) You may have personnel monitoring and adjusting the PEMS during a test, or you may operate the PEMS unattended.
(e) Stop testing as follows:
(1) Continue sampling as needed to get an appropriate amount of emission measurement, according to the standard setting part. If the standard-setting part does not describe when to stop sampling, develop a written protocol before you start testing to establish how you will stop sampling. You may not determine when to stop testing based on emission results.
(2) At the end of the field test, allow the sampling systems' response times to elapse and then stop sampling. Stop any integrators and indicate the end of the test cycle on the data-collection medium.
(3) You may shut down the engine before or after you stop sampling.
(f) For any proportional batch sample, such as a bag sample or PM sample, verify for each test interval whether or not proportional sampling was maintained according to § 1065.545. Void the sample for any test interval that did not maintain proportional sampling according to § 1065.545.
(g) Take the following steps after emission sampling is complete:
(1) As soon as practical after emission sampling, analyze any gaseous batch samples.
(2) If you used dilution air, either analyze background samples or assume that background emissions were zero. Refer to § 1065.140 for dilution-air specifications.
(3) After quantifying all exhaust gases, record mean analyzer values after stabilizing a zero gas to each analyzer, then record mean analyzer values after stabilizing the span gas to the analyzer. Stabilization may include time to purge an analyzer of any sample gas and any additional time to account for analyzer response. Use these recorded values, including pre-test verifications and any zero verifications during testing, to correct for drift as described in § 1065.550.
(4) Verify PEMS gas analyzers used to determine NTE emission values as follows:
(i) Invalidate any data that does not meet the range criteria in § 1065.550. Note that it is acceptable that analyzers exceed 100% of their ranges when measuring emissions between test intervals, but not during test intervals. You do not have to retest an engine if the range criteria are not met.
(ii) Invalidate any data that does not meet the drift criterion in § 1065.550. For HC, invalidate any data if the difference between the uncorrected and the corrected brake-specific HC emission values are not within ±10% of the uncorrected results or the applicable standard, whichever is greater. For data that does meet the drift criterion, correct those test intervals for drift according to § 1065.672 and use the drift corrected results in emissions calculations.
(5) Verify PEMS gas analyzers used to determine bin emission values as follows:
(i) Invalidate data from a whole shift-day if more than 1% of recorded 1 Hz data exceeds 100% of the selected gas analyzer range. For analyzer outputs exceeding 100% of range, calculate emission results using the reported value. You must retest an engine if the range criteria are not met.
(ii) Invalidate any data for periods in which the CO and CO 2 gas analyzers do not meet the drift criterion in § 1065.550. For HC, invalidate data if the difference between the uncorrected and the corrected brake-specific HC emission values are not within ±10% of the uncorrected results or the applicable standard, whichever is greater. For data that do meet the drift criterion, correct the data for drift according to § 1065.672 and use the drift-corrected results in emissions calculations.
(iii) For PEMS NO X analyzers used to determine bin emission values, invalidate data for the engine over the entire shift-day if any data do not meet the following drift limits instead of meeting the drift criteria specified in § 1065.550:
(A) The allowable analyzer zero-drift between successive zero verifications is ±2.5 ppm. The analyzer zero-drift limit over the shift-day is ±10 ppm.
(B) The allowable analyzer span-drift limit is ±4% of the measured span value between successive span verifications.
(6) Unless you weighed PM in-situ, such as by using an inertial PM balance, place any used PM samples into covered or sealed containers and return them to the PM-stabilization environment and weigh them as described in § 1065.595.
§ 1065.940   Emission calculations.
(a) Perform emission calculations as described in § 1065.650 to calculate brake-specific emissions for each test interval using any applicable information and instructions in the standard-setting part.
(b) You may use a fixed molar mass for the diluted exhaust mixture for field testing. Determine this fixed value by engineering analysis.
§ 1065.1001   Definitions.
The definitions in this section apply to this part. The definitions apply to all subparts unless we note otherwise. All undefined terms have the meaning the Act gives them. The definitions follow:
300 series stainless steel means any stainless steel alloy with a Unified Numbering System for Metals and Alloys number designated from S30100 to S39000. For all instances in this part where we specify 300 series stainless steel, such parts must also have a smooth inner-wall construction. We recommend an average roughness, R a , no greater than 4 µm.
Accuracy means the absolute difference between a reference quantity and the arithmetic mean of ten mean measurements of that quantity. Determine instrument accuracy, repeatability, and noise from the same data set. We specify a procedure for determining accuracy in § 1065.305.
Act means the Clean Air Act, as amended, 42 U.S.C. 7401-7671q.
Adjustable parameter means any device, system, or element of design that someone can adjust (including those which are difficult to access) and that, if adjusted, may affect emissions or engine performance during emission testing or normal in-use operation. This includes, but is not limited to, parameters related to injection timing and fueling rate. In some cases, this may exclude a parameter that is difficult to access if it cannot be adjusted to affect emissions without significantly degrading engine performance, or if it will not be adjusted in a way that affects emissions during in-use operation.
Aerodynamic diameter means the diameter of a spherical water droplet that settles at the same constant velocity as the particle being sampled.
Aftertreatment means relating to a catalytic converter, particulate filter, or any other system, component, or technology mounted downstream of the exhaust valve (or exhaust port) whose design function is to decrease emissions in the engine exhaust before it is exhausted to the environment. Exhaust-gas recirculation (EGR) and turbochargers are not aftertreatment.
Allowed procedures means procedures that we either specify in this part 1065 or in the standard-setting part or approve under § 1065.10.
Alternate procedures means procedures allowed under § 1065.10(c)(7).
Applicable standard means an emission standard to which an engine is subject; or a family emission limit to which an engine is certified under an emission credit program in the standard-setting part.
Aqueous condensation means the precipitation of water-containing constituents from a gas phase to a liquid phase. Aqueous condensation is a function of humidity, pressure, temperature, and concentrations of other constituents such as sulfuric acid. These parameters vary as a function of engine intake-air humidity, dilution-air humidity, engine air-to-fuel ratio, and fuel composition—including the amount of hydrogen and sulfur in the fuel.
Atmospheric pressure means the wet, absolute, atmospheric static pressure. Note that if you measure atmospheric pressure in a duct, you must ensure that there are negligible pressure losses between the atmosphere and your measurement location, and you must account for changes in the duct's static pressure resulting from the flow.
Auto-ranging means a gas analyzer function that automatically changes the analyzer digital resolution to a larger range of concentrations as the concentration approaches 100% of the analyzer's current range. Auto-ranging does not mean changing an analog amplifier gain within an analyzer.
Auxiliary emission-control device means any element of design that senses temperature, motive speed, engine RPM, transmission gear, or any other parameter for the purpose of activating, modulating, delaying, or deactivating the operation of any part of the emission-control system.
Average means the arithmetic mean of a sample.
Brake power has the meaning given in the standard-setting part. If it is not defined in the standard-setting part, brake power means the usable power output of the engine, not including power required to fuel, lubricate, or heat the engine, circulate coolant to the engine, or to operate aftertreatment devices. If the engine does not power these accessories during a test, subtract the work required to perform these functions from the total work used in brake-specific emission calculations. Subtract engine fan work from total work only for air-cooled engines.
C 1 -equivalent means a convention of expressing HC concentrations based on the total number of carbon atoms present, such that the C 1 -equivalent of a molar HC concentration equals the molar concentration multiplied by the mean number of carbon atoms in each HC molecule. For example, the C 1 -equivalent of 10 µmol/mol of propane (C 3 H 8 ) is 30 µmol/mol. C 1 -equivalent molar values may be denoted as “ppmC” in the standard-setting part. Molar mass may also be expressed on a C 1 basis. Note that calculating HC masses from molar concentrations and molar masses is only valid where they are each expressed on the same carbon basis.
Calibration means the process of setting a measurement system's response so that its output agrees with a range of reference signals. Contrast with “verification”.
Calibration gas means a purified gas mixture used to calibrate gas analyzers. Calibration gases must meet the specifications of § 1065.750. Note that calibration gases and span gases are qualitatively the same, but differ in terms of their primary function. Various performance verification checks for gas analyzers and sample handling components might refer to either calibration gases or span gases.
Carbon-containing fuel means an engine fuel that is characterized by compounds containing carbon. For example, gasoline, diesel, alcohol, liquefied petroleum gas, and natural gas are carbon-containing fuels.
Certification means relating to the process of obtaining a certificate of conformity for an engine family that complies with the emission standards and requirements in the standard-setting part.
Compression-ignition means relating to a type of reciprocating, internal-combustion engine that is not a spark-ignition engine.
Confidence interval means the range associated with a probability that a quantity will be considered statistically equivalent to a reference quantity.
Constant-speed engine means an engine whose certification is limited to constant-speed operation. Engines whose constant-speed governor function is removed or disabled are no longer constant-speed engines.
Constant-speed operation means engine operation with a governor that automatically controls the operator demand to maintain engine speed, even under changing load. Governors do not always maintain speed exactly constant. Typically speed can decrease (0.1 to 10) % below the speed at zero load, such that the minimum speed occurs near the engine's point of maximum power. (Note: An engine with an adjustable governor setting may be considered to operate at constant speed, subject to our approval. For such engines, the governor setting is considered an adjustable parameter.)
Coriolis meter means a flow-measurement instrument that determines the mass flow of a fluid by sensing the vibration and twist of specially designed flow tubes as the flow passes through them. The twisting characteristic is called the Coriolis effect. According to Newton's Second Law of Motion, the amount of sensor tube twist is directly proportional to the mass flow rate of the fluid flowing through the tube. See § 1065.220.
Dewpoint means a measure of humidity stated as the equilibrium temperature at which water condenses under a given pressure from moist air with a given absolute humidity. Dewpoint is specified as a temperature in °C or K, and is valid only for the pressure at which it is measured. See § 1065.645 to determine water vapor mole fractions from dewpoints using the pressure at which the dewpoint is measured.
Diesel exhaust fluid (DEF) means a liquid reducing agent (other than the engine fuel) used in conjunction with selective catalytic reduction to reduce NO X emissions. Diesel exhaust fluid is generally understood to be an aqueous solution of urea conforming to the specifications of ISO 18611 or ISO 22241.
Dilution ratio (DR) means the amount of diluted exhaust per amount of undiluted exhaust.
Discrete-mode means relating to a discrete-mode type of steady-state test, as described in the standard-setting part.
Dispersion means either:
(1) The broadening and lowering of a signal due to any fluid capacitance, fluid mixing, or electronic filtering in a sampling system. (Note: To adjust a signal so its dispersion matches that of another signal, you may adjust the system's fluid capacitance, fluid mixing, or electronic filtering.)
(2) The mixing of a fluid, especially as a result of fluid mechanical forces or chemical diffusion.
Drift means the difference between a zero or calibration signal and the respective value reported by a measurement instrument immediately after it was used in an emission test, as long as you zeroed and spanned the instrument just before the test.
Dual-fuel has the meaning given in the standard-setting part.
Duty cycle means one of the following:
(1) A series of speed and torque values (or power values) that an engine must follow during a laboratory test. Duty cycles are specified in the standard-setting part. A single duty cycle may consist of one or more test intervals. A series of speed and torque values meeting the definition of this paragraph (1) may also be considered a test cycle. For example, a duty cycle may be a ramped-modal cycle, which has one test interval; a cold-start plus hot-start transient cycle, which has two test intervals; or a discrete-mode cycle, which has one test interval for each mode.
(2) A set of weighting factors and the corresponding speed and torque values, where the weighting factors are used to combine the results of multiple test intervals into a composite result.
Electric power generation application means an application whose purpose is to generate a precise frequency of electricity, which is characterized by an engine that controls engine speed very precisely. This would generally not apply to welders or portable home generators.
Electronic control module means an engine's electronic device that uses data from engine sensors to control engine parameters.
Emission-control system means any device, system, or element of design that controls or reduces the emissions of regulated pollutants from an engine.
Emission-data engine means an engine that is tested for certification. This includes engines tested to establish deterioration factors.
Emission-related maintenance means maintenance that substantially affects emissions or is likely to substantially affect emission deterioration.
Engine family means a group of engines with similar emission characteristics throughout the useful life, as specified in the standard-setting part.
Engine governed speed means the engine operating speed when it is controlled by the installed governor.
Enhanced-idle means a mode of engine idle operation where idle speed is elevated above warm idle speed as determined by the electronic control module, for example during engine warm-up or to increase exhaust temperature.
EPA Program Officer means the Director, Compliance Division, U.S. Environmental Protection Agency, 2000 Traverwood Dr., Ann Arbor, MI 48105.
Exhaust-gas recirculation means a technology that reduces emissions by routing exhaust gases that had been exhausted from the combustion chamber(s) back into the engine to be mixed with incoming air before or during combustion. The use of valve timing to increase the amount of residual exhaust gas in the combustion chamber(s) that is mixed with incoming air before or during combustion is not considered exhaust-gas recirculation for the purposes of this part.
Fall time, t 90-10 , means the time interval of a measurement instrument's response after any step decrease to the input between the following points:
(1) The point at which the response has fallen 10% of the total amount it will fall in response to the step change.
(2) The point at which the response has fallen 90% of the total amount it will fall in response to the step change.
Flexible-fuel has the meaning given in the standard-setting part.
Flow-weighted mean means the mean of a quantity after it is weighted proportional to a corresponding flow rate. For example, if a gas concentration is measured continuously from the raw exhaust of an engine, its flow-weighted mean concentration is the sum of the products of each recorded concentration times its respective exhaust flow rate, divided by the sum of the recorded flow rates. As another example, the bag concentration from a CVS system is the same as the flow-weighted mean concentration, because the CVS system itself flow-weights the bag concentration.
Fuel type means a general category of fuels such as gasoline or LPG. There can be multiple grades within a single type of fuel, such as all-season and winter-grade gasoline.
Good engineering judgment means judgments made consistent with generally accepted scientific and engineering principles and all available relevant information. See 40 CFR 1068.5 for the administrative process we use to evaluate good engineering judgment.
HEPA filter means high-efficiency particulate air filters that are rated to achieve a minimum initial particle-removal efficiency of 99.97% using ASTM F1471 (incorporated by reference, see § 1065.1010).
High-idle speed means the engine speed at which an engine governor function controls engine speed with operator demand at maximum and with zero load applied. “Warm high-idle speed” is the high-idle speed of a warmed-up engine.
High-speed governor means any device, system, or element of design that modulates the engine output torque for the purpose of limiting the maximum engine speed.
Hydraulic diameter means the diameter of a circle whose area is equal to the area of a noncircular cross section of tubing, including its wall thickness. The wall thickness is included only for the purpose of facilitating a simplified and nonintrusive measurement.
Hydrocarbon (HC) means THC, THCE, NMHC, NMNEHC, NMOG, or NMHCE, as applicable. Hydrocarbon generally means the hydrocarbon group on which the emission standards are based for each type of fuel and engine.
Identification number means a unique specification (for example, a model number/serial number combination) that allows someone to distinguish a particular engine from other similar engines.
Idle speed means the engine speed at which an engine governor function controls engine speed with operator demand at minimum and with minimum load applied (greater than or equal to zero). For engines without a governor function that controls idle speed, idle speed means the manufacturer-declared value for lowest engine speed possible with minimum load. This definition does not apply for operation designated as “high-idle speed.” “Warm idle speed” is the idle speed of a warmed-up engine.
Intermediate speed has the meaning given in § 1065.610.
Lean-burn engine means an engine with a nominal air fuel ratio substantially leaner than stoichiometric. For example, diesel-fueled engines are typically lean-burn engines, and gasoline-fueled engines are lean-burn engines if they have an air-to-fuel mass ratio above 14.7:1.
Linearity means the degree to which measured values agree with respective reference values. Linearity is quantified using a linear regression of pairs of measured values and reference values over a range of values expected or observed during testing. Perfect linearity would result in an intercept, a 0, equal to zero, a slope, a 1, of one, a coefficient of determination, r 2 , of one, and a standard error of the estimate, SEE, of zero. The term “linearity” is not used in this part to refer to the shape of a measurement instrument's unprocessed response curve, such as a curve relating emission concentration to voltage output. A properly performing instrument with a nonlinear response curve will meet linearity specifications.
Manufacturer has the meaning given in section 216(1) of the Act. In general, this term includes any person who manufactures an engine or vehicle for sale in the United States or otherwise introduces a new nonroad engine into commerce in the United States. This includes importers who import engines or vehicles for resale.
Maximum test speed has the meaning given in § 1065.610.
Maximum test torque has the meaning given in § 1065.610.
Measurement allowance means a specified adjustment in the applicable emission standard or a measured emission value to reflect the relative quality of the measurement. See the standard-setting part to determine whether any measurement allowances apply for your testing. Measurement allowances generally apply only for field testing and are intended to account for reduced accuracy or precision that result from using field-grade measurement systems.
Mode means one of the following:
(1) A distinct combination of engine speed and load for steady-state testing.
(2) A continuous combination of speeds and loads specifying a transition during a ramped-modal test.
(3) A distinct operator demand setting, such as would occur when testing locomotives or constant-speed engines.
Neat means fuel that is free from mixture or dilution with other fuels. For example, hydrogen or natural gas fuel used without diesel pilot fuel are neat.
NIST-accepted means relating to a value that has been assigned or named by NIST.
NIST-traceable means relating to a standard value that can be related to NIST-stated references through an unbroken chain of comparisons, all having stated uncertainties, as specified in NIST Technical Note 1297 (incorporated by reference, see § 1065.1010). Allowable uncertainty limits specified for NIST-traceability refer to the propagated uncertainty specified by NIST.
Noise means the precision of 30 seconds of updated recorded values from a measurement instrument as it quantifies a zero or reference value. Determine instrument noise, repeatability, and accuracy from the same data set. We specify a procedure for determining noise in § 1065.305.
No-load means a dynamometer setting of zero torque.
Nonmethane hydrocarbon equivalent (NMHCE) means the sum of the carbon mass contributions of non-oxygenated nonmethane hydrocarbons, alcohols and aldehydes, or other organic compounds that are measured separately as contained in a gas sample, expressed as exhaust nonmethane hydrocarbon from petroleum-fueled engines. The hydrogen-to-carbon ratio of the equivalent hydrocarbon is 1.85:1.
Nonmethane hydrocarbons (NMHC) means the sum of all hydrocarbon species except methane. Refer to § 1065.660 for NMHC determination.
Nonmethane nonethane hydrocarbon (NMNEHC) means the sum of all hydrocarbon species except methane and ethane. Refer to § 1065.660 for NMNEHC determination.
Nonroad means relating to nonroad engines.
Nonroad engine has the meaning we give in 40 CFR 1068.30. In general this means all internal-combustion engines except motor vehicle engines, stationary engines, engines used solely for competition, or engines used in aircraft.
Open crankcase emissions means any flow from an engine's crankcase that is emitted directly into the environment. Crankcase emissions are not “open crankcase emissions” if the engine is designed to always route all crankcase emissions back into the engine (for example, through the intake system or an aftertreatment system) such that all the crankcase emissions, or their products, are emitted into the environment only through the engine exhaust system.
Operator demand means an engine operator's input to control engine output. The “operator” may be a person (i.e., manual), or a governor (i.e., automatic) that mechanically or electronically signals an input that demands engine output. Input may be from an accelerator pedal or signal, a throttle-control lever or signal, a fuel lever or signal, a speed lever or signal, or a governor setpoint or signal. Output means engine power, P , which is the product of engine speed, f n , and engine torque, T.
Oxides of nitrogen means NO and NO 2 as measured by the procedures specified in § 1065.270. Oxides of nitrogen are expressed quantitatively as if the NO is in the form of NO 2 , such that you use an effective molar mass for all oxides of nitrogen equivalent to that of NO 2 .
Oxygenated fuels means fuels composed of at least 25% oxygen-containing compounds, such as ethanol or methanol. Testing engines that use oxygenated fuels generally requires the use of the sampling methods in subpart I of this part. However, you should read the standard-setting part and subpart I of this part to determine appropriate sampling methods.
Partial pressure means the pressure, p , attributable to a single gas in a gas mixture. For an ideal gas, the partial pressure divided by the total pressure is equal to the constituent's molar concentration, x .
Percent (%) means a representation of exactly 0.01. Numbers expressed as percentages in this part (such as a tolerance of ±2%) have infinite precision, so 2% and 2.000000000% have the same meaning. This means that where we specify some percentage of a total value, the calculated value has the same number of significant digits as the total value. For example, 2% of a span value where the span value is 101.3302 is 2.026604.
Portable emission measurement system (PEMS) means a measurement system consisting of portable equipment that can be used to generate brake-specific emission measurements during field testing or laboratory testing.
Precision means two times the standard deviation of a set of measured values of a single zero or reference quantity. See also the related definitions of noise and repeatability in this section.
Procedures means all aspects of engine testing, including the equipment specifications, calibrations, calculations and other protocols and specifications needed to measure emissions, unless we specify otherwise.
Proving ring is a device used to measure static force based on the linear relationship between stress and strain in an elastic material. It is typically a steel alloy ring, and you measure the deflection (strain) of its diameter when a static force (stress) is applied across its diameter.
PTFE means polytetrafluoroethylene, commonly known as Teflon TM .
Purified air means air meeting the specifications for purified air in § 1065.750. Purified air may be produced by purifying ambient air. The purification may occur at the test site or at another location (such as at a gas supplier's facility). Alternatively, purified air may be synthetically generated, using good engineering judgment, from purified oxygen and nitrogen. The addition of other elements normally present in purified ambient air (such as Ar) is not required.
Ramped-modal means relating to a ramped-modal type of steady-state test, as described in the standard-setting part.
Recommend has the meaning given in § 1065.201.
Rechargeable Energy Storage System (RESS) means engine or equipment components that store recovered energy for later use to propel the vehicle or accomplish a different primary function. Examples of RESS include the battery system or a hydraulic accumulator in a hybrid vehicle.
Regression statistics means any of the regression statistics specified in § 1065.602.
Repeatability means the precision of ten mean measurements of a reference quantity. Determine instrument repeatability, accuracy, and noise from the same data set. We specify a procedure for determining repeatability in § 1065.305.
Revoke has the meaning given in 40 CFR 1068.30.
Rise time, t 10-90 , means the time interval of a measurement instrument's response after any step increase to the input between the following points:
(1) The point at which the response has risen 10% of the total amount it will rise in response to the step change.
(2) The point at which the response has risen 90% of the total amount it will rise in response to the step change.
Roughness (or average roughness, R a ) means the size of finely distributed vertical surface deviations from a smooth surface, as determined when traversing a surface. It is an integral of the absolute value of the roughness profile measured over an evaluation length.
Round means to apply the rounding convention specified in § 1065.20(e), unless otherwise specified.
Scheduled maintenance means adjusting, repairing, removing, disassembling, cleaning, or replacing components or systems periodically to keep a part or system from failing, malfunctioning, or wearing prematurely. It also may mean actions you expect are necessary to correct an overt indication of failure or malfunction for which periodic maintenance is not appropriate.
Shared atmospheric pressure meter means an atmospheric pressure meter whose output is used as the atmospheric pressure for an entire test facility that has more than one dynamometer test cell.
Shared humidity measurement means a humidity measurement that is used as the humidity for an entire test facility that has more than one dynamometer test cell.
Span means to adjust an instrument so that it gives a proper response to a calibration standard that represents between 75% and 100% of the maximum value in the instrument range or expected range of use.
Span gas means a purified gas mixture used to span gas analyzers. Span gases must meet the specifications of § 1065.750. Note that calibration gases and span gases are qualitatively the same, but differ in terms of their primary function. Various performance verification checks for gas analyzers and sample handling components might refer to either calibration gases or span gases.
Spark-ignition means relating to a gasoline-fueled engine or any other type of engine with a spark plug (or other sparking device) and with operating characteristics significantly similar to the theoretical Otto combustion cycle. Spark-ignition engines usually use a throttle to regulate intake air flow to control power during normal operation.
Special procedures means procedures allowed under § 1065.10(c)(2).
Specified procedures means procedures we specify in this part 1065 or the standard-setting part. Other procedures allowed or required by § 1065.10(c) are not specified procedures.
Standard deviation has the meaning given in § 1065.602. Note this is the standard deviation for a non-biased sample.
Standard-setting part means the part in the Code of Federal Regulations that defines emission standards for a particular engine. See § 1065.1(a).
Steady-state means relating to emission tests in which engine speed and load are held at a finite set of nominally constant values. Steady-state tests are generally either discrete-mode tests or ramped-modal tests.
Stoichiometric means relating to the particular ratio of air and fuel such that if the fuel were fully oxidized, there would be no remaining fuel or oxygen. For example, stoichiometric combustion in a gasoline-fueled engine typically occurs at an air-to-fuel mass ratio of about 14.7:1.
Storage medium means a particulate filter, sample bag, or any other storage device used for batch sampling.
t 0−50 means the time interval of a measurement system's response after any step increase to the input between the following points:
(1) The point at which the step change is initiated at the sample probe.
(2) The point at which the response has risen 50% of the total amount it will rise in response to the step change.
t 100−50 means the time interval of a measurement system's response after any step decrease to the input between the following points:
(1) The point at which the step change is initiated at the sample probe.
(2) The point at which the response has fallen 50% of the total amount it will fall in response to the step change.
Test engine means an engine in a test sample.
Test interval means a duration of time over which you determine mass of emissions. For example, the standard-setting part may specify a complete laboratory duty cycle as a cold-start test interval, plus a hot-start test interval. As another example, a standard-setting part may specify a field-test interval, such as a “not-to-exceed” (NTE) event, as a duration of time over which an engine operates within a certain range of speed and torque. In cases where multiple test intervals occur over a duty cycle, the standard-setting part may specify additional calculations that weight and combine results to arrive at composite values for comparison against the applicable standards in this chapter.
Test sample means the collection of engines selected from the population of an engine family for emission testing.
Tolerance means the interval in which at least 95% of a set of recorded values of a certain quantity must lie. Use the specified recording frequencies and time intervals to determine if a quantity is within the applicable tolerance. The concept of tolerance is intended to address random variability. You may not take advantage of the tolerance specification to incorporate a bias into a measurement.
Total hydrocarbon (THC) means the combined mass of organic compounds measured by the specified procedure for measuring total hydrocarbon, expressed as a hydrocarbon with a hydrogen-to-carbon mass ratio of 1.85:1.
Total hydrocarbon equivalent (THCE) means the sum of the carbon mass contributions of non-oxygenated hydrocarbons, alcohols and aldehydes, or other organic compounds that are measured separately as contained in a gas sample, expressed as exhaust hydrocarbon from petroleum-fueled engines. The hydrogen-to-carbon ratio of the equivalent hydrocarbon is 1.85:1.
Transformation time , t 50 , means the overall system response time to any step change in input, generally the average of the time to reach 50% response to a step increase, t 0−50 , or to a step decrease, t 100−50 .
Uncertainty means uncertainty with respect to NIST-traceability. See the definition of NIST-traceable in this section.
United States means the States, the District of Columbia, the Commonwealth of Puerto Rico, the Commonwealth of the Northern Mariana Islands, Guam, American Samoa, and the U.S. Virgin Islands.
Useful life means the period during which a new engine is required to comply with all applicable emission standards. The standard-setting part defines the specific useful-life periods for individual engines.
Variable-speed engine means an engine that is not a constant-speed engine.
Vehicle means any vehicle, vessel, or type of equipment using engines to which this part applies. For purposes of this part, the term “vehicle” may include nonmotive machines or equipment such as a pump or generator.
Verification means to evaluate whether or not a measurement system's outputs agree with a range of applied reference signals to within one or more predetermined thresholds for acceptance. Contrast with “calibration”.
We (us, our) means the Administrator of the Environmental Protection Agency and any authorized representatives.
Work has the meaning given in § 1065.110.
Zero means to adjust an instrument so it gives a zero response to a zero calibration standard, such as purified nitrogen or purified air for measuring concentrations of emission constituents.
Zero gas means a gas that yields a zero response in an analyzer. This may either be purified nitrogen, purified air, a combination of purified air and purified nitrogen. For field testing, zero gas may include ambient air.
§ 1065.1005   Symbols, abbreviations, acronyms, and units of measure.
The procedures in this part generally follow the International System of Units (SI), as detailed in NIST Special Publication 811, which we incorporate by reference in § 1065.1010. See § 1065.20 for specific provisions related to these conventions. This section summarizes the way we use symbols, units of measure, and other abbreviations.
(a) Symbols for quantities. This part uses the following symbols and units of measure for various quantities:
Table 1 of § 1065.1005—Symbols for Quantities
1 See paragraph (f)(2) of this section for the values to use for molar masses. Note that in the cases of NO X and HC, the regulations specify effective molar masses based on assumed speciation rather than actual speciation.
2 Note that mole fractions for THC, THCE, NMHC, NMHCE, and NOTHC are expressed on a C 1 -equivalent basis.
(b) Symbols for chemical species. This part uses the following symbols for chemical species and exhaust constituents:
Table 2 of § 1065.1005—Symbols for Chemical Species and Exhaust Constituents
(c) Prefixes. This part uses the following prefixes for units and unit symbols:
Table 3 of § 1065.1005—Prefixes
(d) Superscripts . This part uses the following superscripts for modifying quantity symbols:
Table 4 of § 1065.1005—Superscripts
(e) Subscripts . This part uses the following subscripts for modifying quantity symbols:
Table 5 of § 1065.1005—Subscripts
(f) Constants.
(1) This part uses the following constants for the composition of dry air:
Table 6 of § 1065.1005—Constants
(2) This part uses the following molar masses or effective molar masses of chemical species:
Table 7 of § 1065.1005—Molar Masses
1 See paragraph (f)(1) of this section for the composition of dry air.
2 The effective molar masses of THC, THCE, NMHC, NMHCE, and NMNEHC are defined on a C 1 basis and are based on an atomic hydrogen-to-carbon ratio, α, of 1.85 (with β, γ, and δ equal to zero).
3 The effective molar mass of NO X is defined by the molar mass of nitrogen dioxide, NO 2 .
(3) This part uses the following molar gas constant for ideal gases:
Table 8 of § 1065.1005—Molar Gas Constant for Ideal Gases
(4) This part uses the following ratios of specific heats for dilution air and diluted exhaust:
Table 9 of § 1065.1005—Ratios of Specific Heats for Dilution Air and Diluted Exhaust
(g) Other acronyms and abbreviations. This part uses the following additional abbreviations and acronyms:
Table 10 of § 1065.1005—Other Acronyms and Abbreviations
§ 1065.1010   Incorporation by reference.
Certain material is incorporated by reference into this part with the approval of the Director of the Federal Register under 5 U.S.C. 552(a) and 1 CFR part 51. To enforce any edition other than that specified in this section, EPA must publish a document in the Federal Register and the material must be available to the public. All approved incorporation by reference (IBR) material is available for inspection at EPA and at the National Archives and Records Administration (NARA). Contact EPA at: U.S. EPA, Air and Radiation Docket Center, WJC West Building, Room 3334, 1301 Constitution Ave. NW, Washington, DC 20004; www.epa.gov/dockets ; (202) 202-1744. For information on inspecting this material at NARA, visit www.archives.gov/federal-register/cfr/ibr-locations.html or email fr.inspection@nara.gov . The material may be obtained from the following sources:
(a) ASTM material . The following standards are available from ASTM International, 100 Barr Harbor Dr., P.O. Box C700, West Conshohocken, PA 19428-2959, (877) 909-ASTM, or http://www.astm.org:
(1) ASTM D86-12, Standard Test Method for Distillation of Petroleum Products at Atmospheric Pressure, approved December 1, 2012 (“ASTM D86”), IBR approved for §§ 1065.703(b) and 1065.710(b) and (c).
(2) ASTM D93-13, Standard Test Methods for Flash Point by Pensky-Martens Closed Cup Tester, approved July 15, 2013 (“ASTM D93”), IBR approved for § 1065.703(b).
(3) ASTM D130-12, Standard Test Method for Corrosiveness to Copper from Petroleum Products by Copper Strip Test, approved November 1, 2012 (“ASTM D130”), IBR approved for § 1065.710(b).
(4) ASTM D381-12, Standard Test Method for Gum Content in Fuels by Jet Evaporation, approved April 15, 2012 (“ASTM D381”), IBR approved for § 1065.710(b).
(5) ASTM D445-12, Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity), approved April 15, 2012 (“ASTM D445”), IBR approved for § 1065.703(b).
(6) ASTM D525-12a, Standard Test Method for Oxidation Stability of Gasoline (Induction Period Method), approved September 1, 2012 (“ASTM D525”), IBR approved for § 1065.710(b).
(7) ASTM D613-13, Standard Test Method for Cetane Number of Diesel Fuel Oil, approved December 1, 2013 (“ASTM D613”), IBR approved for § 1065.703(b).
(8) ASTM D910-13a, Standard Specification for Aviation Gasolines, approved December 1, 2013 (“ASTM D910”), IBR approved for § 1065.701(f).
(9) ASTM D975-13a, Standard Specification for Diesel Fuel Oils, approved December 1, 2013 (“ASTM D975”), IBR approved for § 1065.701(f).
(10) ASTM D1267-12, Standard Test Method for Gage Vapor Pressure of Liquefied Petroleum (LP) Gases (LP-Gas Method), approved November 1, 2012 (“ASTM D1267”), IBR approved for § 1065.720(a).
(11) ASTM D1319-13, Standard Test Method for Hydrocarbon Types in Liquid Petroleum Products by Fluorescent Indicator Adsorption, approved May 1, 2013 (“ASTM D1319”), IBR approved for § 1065.710(c).
(12) ASTM D1655-13a, Standard Specification for Aviation Turbine Fuels, approved December 1, 2013 (“ASTM D1655”), IBR approved for § 1065.701(f).
(13) ASTM D1837-11, Standard Test Method for Volatility of Liquefied Petroleum (LP) Gases, approved October 1, 2011 (“ASTM D1837”), IBR approved for § 1065.720(a).
(14) ASTM D1838-12a, Standard Test Method for Copper Strip Corrosion by Liquefied Petroleum (LP) Gases, approved December 1, 2012 (“ASTM D1838”), IBR approved for § 1065.720(a).
(15) ASTM D1945-03 (Reapproved 2010), Standard Test Method for Analysis of Natural Gas by Gas Chromatography, approved January 1, 2010 (“ASTM D1945”), IBR approved for § 1065.715(a).
(16) ASTM D2158-11, Standard Test Method for Residues in Liquefied Petroleum (LP) Gases, approved January 1, 2011 (“ASTM D2158”), IBR approved for § 1065.720(a).
(17) ASTM D2163-07, Standard Test Method for Determination of Hydrocarbons in Liquefied Petroleum (LP) Gases and Propane/Propene Mixtures by Gas Chromatography, approved December 1, 2007 (“ASTM D2163”), IBR approved for § 1065.720(a).
(18) ASTM D2598-12, Standard Practice for Calculation of Certain Physical Properties of Liquefied Petroleum (LP) Gases from Compositional Analysis, approved November 1, 2012 (“ASTM D2598”), IBR approved for § 1065.720(a).
(19) ASTM D2622-16, Standard Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry, approved January 1, 2016 (“ASTM D2622”), IBR approved for §§ 1065.703(b) and 1065.710(b) and (c).
(20) ASTM D2699-13b, Standard Test Method for Research Octane Number of Spark-Ignition Engine Fuel, approved October 1, 2013 (“ASTM D2699”), IBR approved for § 1065.710(b).
(21) ASTM D2700-13b, Standard Test Method for Motor Octane Number of Spark-Ignition Engine Fuel, approved October 1, 2013 (“ASTM D2700”), IBR approved for § 1065.710(b).
(22) ASTM D2713-13, Standard Test Method for Dryness of Propane (Valve Freeze Method), approved October 1, 2013 (“ASTM D2713”), IBR approved for § 1065.720(a).
(23) ASTM D2880-13b, Standard Specification for Gas Turbine Fuel Oils, approved November 15, 2013 (“ASTM D2880”), IBR approved for § 1065.701(f).
(24) ASTM D2986-95a, Standard Practice for Evaluation of Air Assay Media by the Monodisperse DOP (Dioctyl Phthalate) Smoke Test, approved September 10, 1995 (“ASTM D2986”), IBR approved for § 1065.170(c). ( Note: This standard was withdrawn by ASTM.)
(25) ASTM D3231-13, Standard Test Method for Phosphorus in Gasoline, approved June 15, 2013 (“ASTM D3231”), IBR approved for § 1065.710(b) and (c).
(26) ASTM D3237-12, Standard Test Method for Lead in Gasoline By Atomic Absorption Spectroscopy, approved June 1, 2012 (“ASTM D3237”), IBR approved for § 1065.710(b) and (c).
(27) ASTM D4052-11, Standard Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter, approved October 15, 2011 (“ASTM D4052”), IBR approved for § 1065.703(b).
(28) ASTM D4629-12, Standard Test Method for Trace Nitrogen in Liquid Petroleum Hydrocarbons by Syringe/Inlet Oxidative Combustion and Chemiluminescence Detection, approved April 15, 2012 (“ASTM D4629”), IBR approved for § 1065.655(e).
(29) ASTM D4814-13b, Standard Specification for Automotive Spark-Ignition Engine Fuel, approved December 1, 2013 (“ASTM D4814”), IBR approved for § 1065.701(f).
(30) ASTM D4815-13, Standard Test Method for Determination of MTBE, ETBE, TAME, DIPE, tertiary-Amyl Alcohol and C1 to C4 Alcohols in Gasoline by Gas Chromatography, approved October 1, 2013 (“ASTM D4815”), IBR approved for § 1065.710(b).
(31) ASTM D5186-03 (Reapproved 2009), Standard Test Method for Determination of the Aromatic Content and Polynuclear Aromatic Content of Diesel Fuels and Aviation Turbine Fuels By Supercritical Fluid Chromatography, approved April 15, 2009 (“ASTM D5186”), IBR approved for § 1065.703(b).
(32) ASTM D5191-13, Standard Test Method for Vapor Pressure of Petroleum Products (Mini Method), approved December 1, 2013 (“ASTM D5191”), IBR approved for § 1065.710(b) and (c).
(33) ASTM D5291-10, Standard Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Petroleum Products and Lubricants, approved May 1, 2010 (“ASTM D5291”), IBR approved for § 1065.655(e).
(34) ASTM D5453-19a, Standard Test Method for Determination of Total Sulfur in Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel Engine Fuel, and Engine Oil by Ultraviolet Fluorescence, approved July 1, 2019 (“ASTM D5453”), IBR approved for §§ 1065.703(b) and 1065.710(b).
(35) ASTM D5599-00 (Reapproved 2010), Standard Test Method for Determination of Oxygenates in Gasoline by Gas Chromatography and Oxygen Selective Flame Ionization Detection, approved October 1, 2010 (“ASTM D5599”), IBR approved for §§ 1065.655(e) and 1065.710(b).
(36) ASTM D5762-12 Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence, approved April 15, 2012 (“ASTM D5762”), IBR approved for § 1065.655(e).
(37) ASTM D5769-10, Standard Test Method for Determination of Benzene, Toluene, and Total Aromatics in Finished Gasolines by Gas Chromatography/Mass Spectrometry, approved May 1, 2010 (“ASTM D5769”), IBR approved for § 1065.710(b).
(38) ASTM D5797-13, Standard Specification for Fuel Methanol (M70- M85) for Automotive Spark-Ignition Engines, approved June 15, 2013 (“ASTM D5797”), IBR approved for § 1065.701(f).
(39) ASTM D5798-13a, Standard Specification for Ethanol Fuel Blends for Flexible Fuel Automotive Spark-Ignition Engines, approved June 15, 2013 (“ASTM D5798”), IBR approved for § 1065.701(f).
(40) ASTM D6348-12 1 , Standard Test Method for Determination of Gaseous Compounds by Extractive Direct Interface Fourier Transform Infrared (FTIR) Spectroscopy, approved February 1, 2012 (“ASTM D6348”), IBR approved for §§ 1065.257(b), 1065.266(c), 1065.275(b), and 1065.277(b).
(41) ASTM D6550-10, Standard Test Method for Determination of Olefin Content of Gasolines by Supercritical-Fluid Chromatography, approved October 1, 2010 (“ASTM D6550”), IBR approved for § 1065.710(b).
(42) ASTM D6615-11a, Standard Specification for Jet B Wide-Cut Aviation Turbine Fuel, approved October 1, 2011 (“ASTM D6615”), IBR approved for § 1065.701(f).
(43) ASTM D6667-14 (Reapproved 2019), Standard Test Method for Determination of Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet Fluorescence, approved May 1, 2019 (“ASTM D6667”), IBR approved for § 1065.720(a).
(44) ASTM D6751-12, Standard Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate Fuels, approved August 1, 2012 (“ASTM D6751”), IBR approved for § 1065.701(f).
(45) ASTM D6985-04a, Standard Specification for Middle Distillate Fuel Oil—Military Marine Applications, approved November 1, 2004 (“ASTM D6985”), IBR approved for § 1065.701(f). (Note: This standard was withdrawn by ASTM.)
(46) ASTM D7039-15a (Reapproved 2020), Standard Test Method for Sulfur in Gasoline, Diesel Fuel, Jet Fuel, Kerosine, Biodiesel, Biodiesel Blends, and Gasoline-Ethanol Blends by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry, approved May 1, 2020 (“ASTM D7039”), IBR approved for §§ 1065.703(b) and 1065.710(b).
(47) ASTM F1471-09, Standard Test Method for Air Cleaning Performance of a High- Efficiency Particulate Air Filter System, approved March 1, 2009 (“ASTM F1471”), IBR approved for § 1065.1001.
(b) California Air Resources Board material. The following documents are available from the California Air Resources Board, Haagen-Smit Laboratory, 9528 Telstar Ave., El Monte, CA 91731-2908, (800) 242-4450, or http://www.arb.ca.gov :
(1) California Non-Methane Organic Gas Test Procedures, Amended July 30, 2002, Mobile Source Division, California Air Resources Board, IBR approved for § 1065.805(f).
(2) [Reserved]
(c) Institute of Petroleum material. The following documents are available from the Energy Institute, 61 New Cavendish St., London, W1G 7AR, UK, or by calling + 44-(0)20-7467-7100, or at http://www.energyinst.org :
(1) IP-470, 2005, Determination of aluminum, silicon, vanadium, nickel, iron, calcium, zinc, and sodium in residual fuels by atomic absorption spectrometry, IBR approved for § 1065.705(b).
(2) IP-500, 2003, Determination of the phosphorus content of residual fuels by ultra-violet spectrometry, IBR approved for § 1065.705(b).
(3) IP-501, 2005, Determination of aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc and phosphorus in residual fuel oil by ashing, fusion and inductively coupled plasma emission spectrometry, IBR approved for § 1065.705(b).
(d) ISO material. The following standards are available from the International Organization for Standardization, 1, ch. de la Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, 41-22-749-01-11, or http://www.iso.org :
(1) ISO 2719:2002, Determination of flash point—Pensky-Martens closed cup method (“ISO 2719”), IBR approved for § 1065.705(c).
(2) ISO 3016:1994, Petroleum products—Determination of pour point (“ISO 3016”), IBR approved for § 1065.705(c).
(3) ISO 3104:1994/Cor 1:1997, Petroleum products—Transparent and opaque liquids—Determination of kinematic viscosity and calculation of dynamic viscosity (“ISO 3104”), IBR approved for § 1065.705(c).
(4) ISO 3675:1998, Crude petroleum and liquid petroleum products—Laboratory determination of density—Hydrometer method (“ISO 3675”), IBR approved for § 1065.705(c).
(5) ISO 3733:1999, Petroleum products and bituminous materials—Determination of water—Distillation method (“ISO 3733”), IBR approved for § 1065.705(c).
(6) ISO 6245:2001, Petroleum products—Determination of ash (“ISO 6245”), IBR approved for § 1065.705(c).
(7) ISO 8217:2012(E), Petroleum products—Fuels (class F)—Specifications of marine fuels, Fifth edition, August 15, 2012 (“ISO 8217”), IBR approved for § 1065.705(b) and (c).
(8) ISO 8754:2003, Petroleum products—Determination of sulfur content—Energy-dispersive X-ray Fluorescence spectrometry (“ISO 8754”), IBR approved for § 1065.705(c).
(9) ISO 10307-2(E):2009, Petroleum products—Total sediment in residual fuel oils—Part 2: Determination using standard procedures for ageing, Second Ed., February 1, 2009 (“ISO 10307”), as modified by ISO 10307-2:2009/Cor.1:2010(E), Technical Corrigendum 1, published May 15, 2010, IBR approved for § 1065.705(c).
(10) ISO 10370:1993/Cor 1:1996, Petroleum products—Determination of carbon residue—Micro method (“ISO 10370”), IBR approved for § 1065.705(c).
(11) ISO 10478:1994, Petroleum products—Determination of aluminium and silicon in fuel oils—Inductively coupled plasma emission and atomic absorption spectroscopy methods (“ISO 10478”), IBR approved for § 1065.705(c).
(12) ISO 12185:1996/Cor 1:2001, Crude petroleum and petroleum products—Determination of density—Oscillating U-tube method (“ISO 12185”), IBR approved for § 1065.705(c).
(13) ISO 14596:2007, Petroleum products—Determination of sulfur content—Wavelength-dispersive X-ray fluorescence spectrometry (“ISO 14596”), IBR approved for § 1065.705(c).
(14) ISO 14597:1997, Petroleum products—Determination of vanadium and nickel content—Wavelength dispersive X-ray fluorescence spectrometry (“ISO 14597”), IBR approved for § 1065.705(c).
(15) ISO 14644-1:1999, Cleanrooms and associated controlled environments (“ISO 14644”), IBR approved for § 1065.190(b).
(e) NIST material. The following documents are available from National Institute of Standards and Technology, 100 Bureau Drive, Stop 1070, Gaithersburg, MD 20899-1070, (301) 975-6478, or www.nist.gov :
(1) NIST Special Publication 811, 2008 Edition, Guide for the Use of the International System of Units (SI), March 2008, IBR approved for §§ 1065.20(a) and 1065.1005.
(2) NIST Technical Note 1297, 1994 Edition, Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement Results, IBR approved for §§ 1065.365(g), 1065.750(a), and 1065.1001.
(f) SAE International material. The following standards are available from SAE International, 400 Commonwealth Dr., Warrendale, PA 15096-0001, (724) 776-4841, or http://www.sae.org :
(1) SAE 770141, 1977, Optimization of Flame Ionization Detector for Determination of Hydrocarbon in Diluted Automotive Exhausts, Glenn D. Reschke, IBR approved for § 1065.360(c).
(2) SAE J1151, Methane Measurement Using Gas Chromatography, stabilized September 2011, IBR approved for §§ 1065.267(b) and 1065.750(a).
§ 1065.1101   Applicability.
This subpart specifies procedures that may be used to measure emission constituents that are not measured (or not separately measured) by the test procedures in the other subparts of this part. These procedures are included to facilitate consistent measurement of unregulated pollutants for purposes other than compliance with emission standards. Unless otherwise specified in the standard-setting part, use of these procedures is optional and does not replace any requirements in the rest of this part.
§ 1065.1103   General provisions for SVOC measurement.
The provisions of §§ 1065.1103 through 1065.1111 specify procedures for measuring semi-volatile organic compounds (SVOC) along with PM. These sections specify how to collect a sample of the SVOCs during exhaust emission testing, as well as how to use wet chemistry techniques to extract SVOCs from the sample media for analysis. Note that the precise method you use will depend on the category of SVOCs being measured. For example, the method used to measure polynuclear aromatic hydrocarbons (PAHs) will differ slightly from the method used to measure dioxins. Follow standard analytic chemistry methods for any aspects of the analysis that are not specified.
(a) Laboratory cleanliness is especially important throughout SVOC testing. Thoroughly clean all sampling system components and glassware before testing to avoid sample contamination. For the purposes of this subpart, the sampling system is defined as sample pathway from the sample probe inlet to the downstream most point where the sample is captured (in this case the condensate trap).
(b) We recommend that media blanks be analyzed for each batch of sample media (sorbent, filters, etc.) prepared for testing. Blank sorbent modules (i.e., field blanks) should be stored in a sealed environment and should periodically accompany the test sampling system throughout the course of a test, including sampling system and sorbent module disassembly, sample packaging, and storage. Use good engineering judgment to determine the frequency with which you should generate field blanks. The field blank sample should be close to the sampler during testing.
(c) We recommend the use of isotope dilution techniques, including the use of isotopically labeled surrogate, internal, alternate, and injection standards.
(d) If your target analytes degrade when exposed to ultraviolet radiation, such as nitropolynuclear aromatic hydrocarbons (nPAHs), perform these procedures in the dark or with ultraviolet filters installed over the lights.
(e) The following definitions and abbreviations apply for SVOC measurements:
(1) Soxhlet extraction means the extraction method invented by Franz von Soxhlet, in which the sample is placed in a thimble and rinsed repeatedly with a recycle of the extraction solvent.
(2) XAD-2 means a hydrophobic crosslinked polystyrene copolymer resin adsorbent known commercially as Amberlite® XAD®-2, or an equivalent adsorbent like XAD-4.
(3) Semi-volatile organic compound (SVOC) means an organic compound that is sufficiently volatile to exist in vapor form in engine exhaust, but that readily condenses to liquid or solid form under atmospheric conditions. Most SVOCs have at least 14 carbon atoms per molecule or they have a boiling point between (240 and 400) °C. SVOCs include dioxin, quinone, and nitro-PAH compounds. They may be a natural byproduct of combustion or they may be created post-combustion. Note that SVOCs may be included in measured values of hydrocarbons and/or PM using the procedures specified in this part.
(4) Kuderna-Danish concentrator means laboratory glassware known by this name that consists of an air-cooled condenser on top of an extraction bulb.
(5) Dean-Stark trap means laboratory glassware known by this name that uses a reflux condenser to collect water from samples extracted under reflux.
(6) PUF means polyurethane foam.
(7) Isotopically labeled means relating to a compound in which either all the hydrogen atoms are replaced with the atomic isotope hydrogen-2 (deuterium) or one of the carbon atoms at a defined position in the molecule is replaced with the atomic isotope carbon-13.
§ 1065.1105   Sampling system design.
(a) General. We recommend that you design your SVOC batch sampler to extract sample from undiluted emissions to maximize the sampled SVOC quantity. If you dilute your sample, we recommend using annular dilution. If you dilute your sample, but do not use annular dilution, you must precondition your sampling system to reach equilibrium with respect to loss and re-entrainment of SVOCs to the walls of the sampling system. To the extent practical, adjust sampling times based on the emission rate of target analytes from the engine to obtain analyte concentrations above the detection limit. In some instances you may need to run repeat test cycles without replacing the sample media or disassembling the batch sampler.
(b) Sample probe, transfer lines, and sample media holder design and construction. The sampling system should consist of a sample probe, transfer line, PM filter holder, cooling coil, sorbent module, and condensate trap. Construct sample probes, transfer lines, and sample media holders that have inside surfaces of nickel, titanium or another nonreactive material capable of withstanding raw exhaust gas temperatures. Seal all joints in the hot zone of the system with gaskets made of nonreactive material similar to that of the sampling system components. You may use teflon gaskets in the cold zone. We recommend locating all components as close to probes as practical to shorten sampling system length and minimize the surface exposed to engine exhaust.
(c) Sample system configuration. This paragraph (c) specifies the components necessary to collect SVOC samples, along with our recommended design parameters. Where you do not follow our recommendations, use good engineering judgment to design your sampling system so it does not result in loss of SVOC during sampling. The sampling system should contain the following components in series in the order listed:
(1) Use a sample probe similar to the PM sample probe specified in subpart B of this part.
(2) Use a PM filter holder similar to the holder specified in subpart B of this part, although you will likely need to use a larger size to accommodate the high sample flow rates. We recommend using a 110 mm filter for testing spark ignition engines or engines that utilize exhaust aftertreatment for PM removal and a 293 mm filter for other engines. If you are not analyzing separately for SVOCs in gas and particle phases, you do not have to control the temperature of the filter holder. Note that this differs from normal PM sampling procedures, which maintain the filter at a much lower temperature to capture a significant fraction of exhaust SVOC on the filter. In this method, SVOCs that pass through the filter will be collected on the downstream sorbent module. If you are collecting SVOCs in gas and particle phases, control your filter face temperature according to § 1065.140(e)(4).
(3) Use good engineering judgment to design a cooling coil that will drop the sample temperature to approximately 5 °C. Note that downstream of the cooling coil, the sample will be a mixture of vapor phase hydrocarbons in CO 2 , air, and a primarily aqueous liquid phase.
(4) Use a hydrophobic sorbent in a sealed sorbent module. Note that this sorbent module is intended to be the final stage for collecting the SVOC sample and should be sized accordingly. We recommend sizing the module to hold 40 g of XAD-2 along with PUF plugs at either end of the module, noting that you may vary the mass of XAD used for testing based on the anticipated SVOC emission concentration and sample flow rate.
(5) Include a condensate trap to separate the aqueous liquid phase from the gas stream. We recommend using a peristaltic pump to remove water from the condensate trap over the course of the test to prevent build-up of the condensate. Note that for some tests it may be appropriate to collect this water for analysis.
(d) Sampler flow control. For testing using the recommended filter and sorbent module sizes, we recommend targeting an average sample flow rate of 70 liters per minute to maximize SVOC collection. The sampler must be designed to maintain proportional sampling throughout the test. Verify proportional sampling after an emission test as described in § 1065.545.
(e) Water bath. Design the sample system with a water bath in which the cooling coil, sorbent module, and condensate trap will be submerged. Use a heat exchanger or ice to maintain the bath temperature at (3 to 7) °C.
§ 1065.1107   Sample media and sample system preparation; sample system assembly.
This section describes the appropriate types of sample media and the cleaning procedure required to prepare the media and wetted sample surfaces for sampling.
(a) Sample media. The sampling system uses two types of sample media in series: The first to simultaneously capture the PM and associated particle phase SVOCs, and a second to capture SVOCs that remain in the gas phase, as follows:
(1) For capturing PM, we recommend using pure quartz filters with no binder if you are not analyzing separately for SVOCs in gas and particle phases. If you are analyzing separately, you must use polytetrafluoroethylene (PTFE) filters with PTFE support. Select the filter diameter to minimize filter change intervals, accounting for the expected PM emission rate, sample flow rate. Note that when repeating test cycles to increase sample mass, you may replace the filter without replacing the sorbent or otherwise disassembling the batch sampler. In those cases, include all filters in the extraction.
(2) For capturing gaseous SVOCs, utilize XAD-2 resin with or without PUF plugs. Note that two PUF plugs are typically used to contain the XAD-2 resin in the sorbent module.
(b) Sample media and sampler preparation. Prepare pre-cleaned PM filters and pre-cleaned PUF plugs/XAD-2 as needed. Store sample media in containers protected from light and ambient air if you do not use them immediately after cleaning. Use the following preparation procedure, or an analogous procedure with different solvents and extraction times:
(1) Pre-clean the filters via Soxhlet extraction with methylene chloride for 24 hours and dry over dry nitrogen in a low-temperature vacuum oven.
(2) Pre-clean PUF and XAD-2 with a series of Soxhlet extractions: 8 hours with water, 22 hours with methanol, 22 hours with methylene chloride, and 22 hours with toluene, followed by drying with nitrogen.
(3) Clean sampler components, including the probe, filter holder, condenser, sorbent module, and condensate collection vessel by rinsing three times with methylene chloride and then three times with toluene. Prepare pre-cleaned aluminum foil for capping the probe inlet of the sampler after the sampling system has been assembled.
(c) Sorbent spiking. Use good engineering judgment to verify the extent to which your extraction methods recover SVOCs absorbed on the sample media. We recommend spiking the XAD-2 resin with a surrogate standard before testing with a carbon-13 or hydrogen-2 isotopically labeled standard for each of the class of analytes targeted for analysis. Perform this spiking as follows:
(1) Insert the lower PUF plug into the bottom of the sorbent module.
(2) Add half of one portion of XAD-2 resin to the module and spike the XAD-2 in the module with the standard.
(3) Wait 1 hour for the solvent from the standard(s) to evaporate, add the remaining 20 g of the XAD-2 resin to the module, and then insert a PUF plug in the top of the sorbent module.
(4) Cover the inlet and outlet of the sorbent module with pre-cleaned aluminum foil.
(d) Sampling system assembly. After preparing the sample media and the sampler, assemble the condensate trap, cooling coil, filter holder with filter, sample probe, and sorbent module, then lower the assembly into the reservoir. Cover the probe inlet with pre-cleaned aluminum foil.
§ 1065.1109   Post-test sampler disassembly and sample extraction.
This section describes the process for disassembling and rinsing the sampling system and extracting and cleaning up the sample.
(a) Sampling system disassembly. Disassemble the sampling system in a clean environment as follows after the test:
(1) Remove the PM filter, PUF plugs, and all the XAD-2 from the sampling system and store them at or below 5 °C until analysis.
(2) Rinse sampling system wetted surfaces upstream of the condensate trap with acetone followed by toluene (or a comparable solvent system), ensuring that all the solvent remaining in liquid phase is collected (note that a fraction of the acetone and toluene will likely be lost to evaporation during mixing). Rinse with solvent volumes that are sufficient to cover all the surfaces exposed to the sample during testing. We recommend three fresh solvent rinses with acetone and two with toluene. We recommend rinse volumes of 60 ml per rinse for all sampling system components except the condenser coil, of which you should use 200 ml per rinse. Keep the acetone rinsate separate from the toluene rinsate to the extent practicable. Rinsate fractions should be stored separately in glass bottles that have been pre-rinsed with acetone, hexane, and toluene (or purchase pre-cleaned bottles).
(3) Use good engineering judgment to determine if you should analyze the aqueous condensate phase for SVOCs. If you determine that analysis is necessary, use toluene to perform a liquid-liquid extraction of the SVOCs from the collected aqueous condensate using a separatory funnel or an equivalent method. Add the toluene from this aqueous extraction to the toluene rinsate fraction described in paragraph (a)(2) of this section.
(4) Reduce rinsate solvent volumes as needed using a Kuderna-Danish concentrator or rotary evaporator and retain these rinse solvents for reuse during sample media extraction for the same test. Be careful to avoid loss of low molecular weight analytes when concentrating with rotary evaporation.
(b) Sample extraction. Extract the SVOCs from the sorbent using Soxhlet extraction as described in this paragraph (b). Two 16 hour extractions are necessary to accommodate the Soxhlet extractions of all SVOCs from a single sample. This reduces the possibility of losing low molecular weight SVOCs and promotes water removal. We recommend performing the first extraction with acetone/hexane and the second using toluene (or an equivalent solvent system). You may alternatively use an equivalent method such as an automated solvent extractor.
(1) We recommend equipping the Soxhlet extractor with a Dean-Stark trap to facilitate removal of residual water from the sampling system rinse. The Soxhlet apparatus must be large enough to allow extraction of the PUF, XAD-2, and filter in a single batch. Include in the extractor setup a glass thimble with a coarse or extra coarse sintered glass bottom. Pre-clean the extractor using proper glass-cleaning procedures. We recommend that the Soxhlet apparatus be cleaned with a (4 to 8) hour Soxhlet extraction with methylene chloride at a cycling rate of three cycles per hour. Discard the solvent used for pre-cleaning (no analysis is necessary).
(2) Load the extractor thimble before placing it in the extractor by first rolling the PM filter around the inner circumference of the thimble, with the sampled side facing in. Push one PUF plug down into the bottom of the thimble, add approximately half of the XAD-2, and then spike the XAD-2 in the thimble with the isotopically labeled extraction standards of known mass. Target the center of the XAD-2 bed for delivering the extraction standard. We recommend using multiple isotopically labeled extraction standards that cover the range of target analytes. This generally means that you should use isotopically labeled standards at least for the lowest and highest molecular weight analytes for each category of compounds (such as PAHs and dioxins). These extraction standards monitor the efficiency of the extraction and are also used to determine analyte concentrations after analysis. Upon completion of spiking, add the remaining XAD-2 to the thimble, insert the remaining PUF plug, and place the thimble into the extractor. Note that if you are collecting and analyzing for SVOCs in gas and particle phases, perform separate extractions for the filter and XAD-2.
(3) For the initial extraction, combine the concentrated acetone rinses (from the sampling system in paragraph (a) of this section) with enough hexane to bring the solvent volume up to the target level of 700 ml. Assemble the extractor and turn on the heating controls and cooling water. Allow the sample to reflux for 16 hours with the rheostat adjusted to cycle the extraction at a rate of (3.0 ±0.5) cycles per hour. Drain the water from the Dean-Stark trap as it accumulates by opening the stopcock on the trap. Set aside the water for analysis or discard it. In most cases, any water present will be removed within approximately 2 hours after starting the extraction.
(4) After completing the initial extraction, remove the solvent and concentrate it to (4.0 ±0.5) ml using a Kuderna-Danish concentrator that includes a condenser such as a three-ball Snyder column with venting dimples and a graduated collection tube. Hold the water bath temperature at (75 to 80) °C. Using this concentrator will minimize evaporative loss of analytes with lower molecular weight.
(i) Rinse the round bottom flask of the extractor with (60 to 100) ml of hexane and add the rinsate to this concentrated extract.
(ii) Concentrate the mixture to (4 ±0.5) ml using a Kuderna-Danish concentrator or similar apparatus.
(iii) Repeat the steps in paragraphs (b)(4)(i) and (ii) of this section three times, or as necessary to remove all the residual solvent from the round bottom flask of the extractor, concentrating the final rinsate to (4 ±0.5) ml.
(5) For the second extraction, combine the toluene rinses (from the sampling system in paragraph (a) of this section) with any additional toluene needed to bring the solvent volume up to the target level of 700 ml. As noted in paragraph (a) of this section, you may need to concentrate the rinsate before adding it to the extraction apparatus if the rinsate solvent volume is too large. Allow the sample to reflux for 16 hours with the rheostat adjusted to cycle the extraction at a rate of (3.0 ±0.5) cycles per hour. Check the Dean-Stark trap for water during the first 2 hours of the extraction (though little or no water should be present during this stage).
(6) Upon completion of the second extraction, remove the solvent and concentrate it to (4 ±0.5) ml as described in paragraph (b)(4) of this section. Using hexane from paragraph (b)(4) of this section as the rinse solvent effectively performs a solvent exchange of toluene with hexane.
(7) Combine the concentrated extract from paragraph (b)(4) of this section with the concentrated extract from paragraph (b)(6) of this section. Divide the extract into a number of fractions based on the number of analyses you need to perform. Perform the separate sample clean-up described in paragraph (c) of this section as needed for each fraction.
(c) Sample clean-up. This paragraph (c) describes how to perform sample cleaning to remove from the sample extract any solids and any SVOCs that will not be analyzed. This process, known as “sample clean-up”, reduces the potential for interference or co-elution of peaks during analytical analysis. Before performing the sample clean-up, spike the extract with an alternate standard that contains a known mass of isotopically labeled compounds that are identical to the target analytes (except for the labeling). The category of the target analyte compounds (such as PAHs or dioxin) will determine the number of compounds that make up the standard. For example, PAHs require the use of four compounds in the alternate standard to cover the four basic ring structures of PAHs (2-ring, 3-ring, 4-ring, and 5-ring structures). These alternate standards are used to monitor the efficiency of the clean-up procedure. Before sample clean-up, concentrate the fractionated sample to about 2 ml with a Kuderna-Danish concentrator or rotary evaporator, and then transfer the extract to an 8 ml test tube with hexane rinse. Concentrate it to a volume of about 1 ml using a Kuderna-Danish concentrator. Use good engineering judgment to select an appropriate column chromatographic clean-up option for your target analytes. Note that these clean-up techniques generally remove compounds based on their polarity. The following procedures are examples of clean-up techniques for PAHs and nPAHs.
(1) PAH clean-up. The following method is appropriate for clean-up of extracts intended for analysis of PAHs:
(i) Pack a glass gravity column (250 mm × 10 mm recommended) by inserting a clean glass wool plug into the bottom of the column and add 10 g of activated silica gel in methylene chloride. Tap the column to settle the silica gel and then add a 1 cm layer of anhydrous sodium sulfate. Verify the volume of solvent required to completely elute all the PAHs and adjust the weight of the silica gel accordingly to account for variations among batches of silica gel that may affect the elution volume of the various PAHs.
(ii) Elute the column with 40 ml of hexane. The rate for all elutions should be about 2 ml/min. You may increase the elution rate by using dry air or nitrogen to maintain the headspace slightly above atmospheric pressure. Discard the eluate just before exposing the sodium sulfate layer to the air or nitrogen and transfer the 1 ml sample extract onto the column using two additional 2 ml rinses of hexane. Just before exposing the sodium sulfate layer to the air or nitrogen, begin elution of the column with 25 ml of hexane followed by 25 ml of 40 volume % methylene chloride in hexane. Collect the entire eluate and concentrate it to about 5 ml using the Kuderna-Danish concentrator or a rotary evaporator. Make sure not to evaporate all the solvent from the extract during the concentration process. Transfer the eluate to a small sample vial using a hexane rinse and concentrate it to 100 µl using a stream of nitrogen without violently disturbing the solvent. Store the extracts in a refrigerator at or below 4 °C, and away from light.
(2) nPAH clean up. The following procedure, adapted from “Determination and Comparison of Nitrated-Polycyclic Aromatic Hydrocarbons Measured in Air and Diesel Particulate Reference Materials” (Bamford, H.A., et al , Chemosphere, Vol. 50, Issue 5, pages 575-587), is an appropriate method to clean up extracts intended for analysis of nPAHs:
(i) Condition an aminopropyl solid phase extraction (SPE) cartridge by eluting it with 20 ml of 20 volume % methylene chloride in hexane. Transfer the extract quantitatively to the SPE cartridge with at least two methylene chloride rinses. Elute the extract through the SPE cartridge by using 40 ml of 20 volume % methylene chloride in hexane to minimize potential interference of polar constituents, and then reduce the extract to 0.5 ml in hexane and subject it to normal-phase liquid chromatography using a pre-prepared 9.6 mm × 25 cm semi-preparative Chromegabond® amino/cyano column (5 µm particle size) to isolate the nPAH fraction. The mobile phase is 20 volume % methylene chloride in hexane at a constant flow rate of 5 ml per minute. Back-flash the column with 60 ml of methylene chloride and then condition it with 200 ml of 20 volume % methylene chloride in hexane before each injection. Collect the effluent and concentrate it to about 2 ml using the Kuderna-Danish concentrator or a rotary evaporator. Transfer it to a minivial using a hexane rinse and concentrate it to 100 µl using a gentle stream of nitrogen. Store the extracts at or below 4 °C, and away from light.
(ii) [Reserved]
§ 1065.1111   Sample analysis.
This subpart does not specify chromatographic or analytical methods to analyze extracts, because the appropriateness of such methods is highly dependent on the nature of the target analytes. However, we recommend that you spike the extract with an injection standard that contains a known mass of an isotopically labeled compound that is identical to one of the target analytes (except for labeling). This injection standard allows you to monitor the efficiency of the analytical process by verifying the volume of sample injected for analysis.
§ 1065.1113   General provisions related to vanadium sublimation temperatures in SCR catalysts.
Sections 1065.1113 through 1065.1121 specify procedures for determining vanadium emissions from a catalyst based on catalyst temperature. Vanadium can be emitted from the surface of SCR catalysts at temperatures above 550 °C, dependent on the catalyst formulation. These procedures are appropriate for measuring the vanadium sublimation product from a reactor by sampling onto an equivalent mass of alumina and performing analysis by Inductively Coupled Plasma—Optical Emission Spectroscopy (ICP-OES). Follow standard analytic chemistry methods for any aspects of the analysis that are not specified.
(a) The procedure is adapted from “Behavior of Titania-supported Vanadia and Tungsta SCR Catalysts at High Temperatures in Reactant Streams: Tungsten and Vanadium Oxide and Hydroxide Vapor Pressure Reduction by Surficial Stabilization” (Chapman, D.M., Applied Catalysis A: General, 2011, 392, 143-150) with modifications to the acid digestion method from “Measuring the trace elemental composition of size-resolved airborne particles” (Herner, J.D. et al, Environmental Science and Technology, 2006, 40, 1925-1933).
(b) Laboratory cleanliness is especially important throughout vanadium testing. Thoroughly clean all sampling system components and glassware before testing to avoid sample contamination.
§ 1065.1115   Reactor design and setup.
Vanadium measurements rely on a reactor that adsorbs sublimation vapors of vanadium onto an alumina capture bed with high surface area.
(a) Configure the reactor with the alumina capture bed downstream of the catalyst in the reactor's hot zone to adsorb vanadium vapors at high temperature. You may use quartz beads upstream of the catalyst to help stabilize reactor gas temperatures. Select an alumina material and design the reactor to minimize sintering of the alumina. For a 1-inch diameter reactor, use 4 to 5 g of 1/8 inch extrudates or -14/+24 mesh (approximately 0.7 to 1.4 mm) gamma alumina (such as Alfa Aesar, aluminum oxide, gamma, catalyst support, high surface area, bimodal). Position the alumina downstream from either an equivalent amount of -14/+24 mesh catalyst sample or an approximately 1-inch diameter by 1 to 3-inch long catalyst-coated monolith sample cored from the production-intent vanadium catalyst substrate. Separate the alumina from the catalyst with a 0.2 to 0.4 g plug of quartz wool. Place a short 4 g plug of quartz wool downstream of the alumina to maintain the position of that bed. Use good engineering judgment to adjust as appropriate for reactors of different sizes.
(b) Include the quartz wool with the capture bed to measure vanadium content. We recommend analyzing the downstream quartz wool separately from the alumina to see if the alumina fails to capture some residual vanadium.
(c) Configure the reactor such that both the sample and capture beds are in the reactor's hot zone. Design the reactor to maintain similar temperatures in the capture bed and catalyst. Monitor the catalyst and alumina temperatures with Type K thermocouples inserted into a thermocouple well that is in contact with the catalyst sample bed.
(d) If there is a risk that the quartz wool and capture bed are not able to collect all the vanadium, configure the reactor with an additional capture bed and quartz wool plug just outside the hot zone and analyze the additional capture bed and quartz wool separately.
(e) An example of a catalyst-coated monolith and capture bed arrangement in the reactor tube are shown in the following figure:

(f) You may need to account for vanadium-loaded particles contaminating catalyst-coated monoliths as a result of physical abrasion. To do this, determine how much titanium is in the capture bed and compare to an alumina blank. Using these values and available information about the ratio of vanadium to titanium in the catalyst, subtract the mass of vanadium catalyst material associated with the catalyst particles from the total measured vanadium on the capture bed to determine the vanadium recovered due to sublimation.
§ 1065.1117   Reactor aging cycle for determination of vanadium sublimation temperature.
This section describes the conditions and process required to operate the reactor described in § 1065.1115 for collection of the vanadium sublimation samples for determination of vanadium sublimation temperature. The reactor aging cycle constitutes the process of testing the catalyst sample over all the test conditions described in paragraph (b) of this section.
(a) Set up the reactor to flow gases with a space velocity of at least 35,000/hr with a pressure drop across the catalyst and capture beds less than 35 kPa. Use test gases meeting the following specifications, noting that not all gases will be used at the same time:
(1) 5 vol% O 2 , balance N 2 .
(2) NO, balance N 2 . Use an NO concentration of (200 to 500) ppm.
(3) NH 3 , balance N 2 . Use an NH 3 concentration of (200 to 500) ppm.
(b) Perform testing as follows:
(1) Add a new catalyst sample and capture bed into the reactor as described in § 1065.1113. Heat the reactor to 550 °C while flowing the oxygen blend specified in paragraph (a)(1) of this section as a pretest gas mixture. Ensure that no H 2 O is added to the pretest gas mixture to reduce the risk of sintering and vanadium sublimation.
(2) Start testing at a temperature that is lower than the point at which vanadium starts to sublime. Start testing when the reactor reaches 550 °C unless testing supports a lower starting temperature. Once the reactor reaches the starting temperature and the catalyst has been equilibrated to the reactor temperature, flow NO and NH 3 test gases for 18 hours with a nominal H 2 O content of 5 volume percent. If an initial starting temperature of 550 °C results in vanadium sublimation, you may retest using a new catalyst sample and a lower initial starting temperature.
(3) After 18 hours of exposure, flow the pretest oxygen blend as specified in paragraph (b)(1) of this section and allow the reactor to cool down to room temperature.
(4) Analyze the sample as described in § 1065.1121.
(5) Repeat the testing in paragraphs (b)(1) through (4) of this section by raising the reactor temperature in increments of 50 °C up to the temperature at which vanadium sublimation begins.
(6) Once sublimation has been detected, repeat the testing in paragraphs (b)(1) through (4) of this section by decreasing the reactor temperature in increments of 25 °C until the vanadium concentration falls below the sublimation threshold.
(7) Repeat the testing in paragraphs (b)(1) through (6) of this section with a nominal H 2 O concentration of 10 volume percent or the maximum water concentration expected at the standard.
(8) You may optionally test in a manner other than testing a single catalyst formulation in series across all test temperatures. For example, you may test additional samples at the same reactor temperature before moving on to the next temperature.
(c) The effective sublimation temperature for the tested catalyst is the lowest reactor temperature determined in paragraph (b) of this section below which vanadium emissions are less than the method detection limit.
§ 1065.1119   Blank testing.
This section describes the process for analyzing blanks. Use blanks to determine the background effects and the potential for contamination from the sampling process.
(a) Take blanks from the same batch of alumina used for the capture bed.
(b) Media blanks are used to determine if there is any contamination in the sample media. Analyze at least one media blank for each reactor aging cycle or round of testing performed under § 1065.1117. If your sample media is taken from the same lot, you may analyze media blanks less frequently consistent with good engineering judgment.
(c) Field blanks are used to determine if there is any contamination from environmental exposure of the sample media. Analyze at least one field blank for each reactor aging cycle or round of testing performed under § 1065.1117. Field blanks must be contained in a sealed environment and accompany the reactor sampling system throughout the course of a test, including reactor disassembly, sample packaging, and storage. Use good engineering judgment to determine how frequently to generate field blanks. Keep the field blank sample close to the reactor during testing.
(d) Reactor blanks are used to determine if there is any contamination from the sampling system. Analyze at least one reactor blank for each reactor aging cycle or round of testing performed under § 1065.1117.
(1) Test reactor blanks with the reactor on and operated identically to that of a catalyst test in § 1065.1117 with the exception that when loading the reactor, only the alumina capture bed will be loaded (no catalyst sample is loaded for the reactor blank). We recommend acquiring reactor blanks with the reactor operating at average test temperature you used when acquiring your test samples under § 1065.1117.
(2) You must run at least three reactor blanks if the result from the initial blank analysis is above the detection limit of the method, with additional blank runs based on the uncertainty of the reactor blank measurements, consistent with good engineering judgment.
§ 1065.1121   Vanadium sample dissolution and analysis in alumina capture beds.
This section describes the process for dissolution of vanadium from the vanadium sublimation samples collect in § 1065.1117 and any blanks collected in § 1065.1119 as well as the analysis of the digestates to determine the mass of vanadium emitted and the associated sublimation temperature threshold based on the results of all the samples taken during the reactor aging cycle.
(a) Digest the samples using the following procedure, or an equivalent procedure:
(1) Place the recovered alumina, a portion of the ground quartz tube from the reactor, and the quartz wool in a Teflon pressure vessel with a mixture made from 1.5 mL of 16 N HNO 3 , 0.5 mL of 28 N HF, and 0.2 mL of 12 N HCl. Note that the amount of ground quartz tube from the reactor included in the digestion can influence the vanadium concentration of both the volatilized vanadium from the sample and the method detection limit. You must be consistent with the amount ground quartz tube included in the sample analysis for your testing. You must limit the amount of quartz tube to include only portions of the tube that would be likely to encounter volatilized vanadium.
(2) Program a microwave oven to heat the sample to 180 °C over 9 minutes, followed by a 10-minute hold at that temperature, and 1 hour of ventilation/cooling.
(3) After cooling, dilute the digests to 30 mL with high purity 18MΩ water prior to ICP-MS (or ICP-OES) analysis. Note that this digestion technique requires adequate safety measures when working with HF at high temperature and pressure. To avoid “carry-over” contamination, rigorously clean the vessels between samples as described in “Microwave digestion procedures for environmental matrixes” (Lough, G.C. et al, Analyst. 1998, 123 (7), 103R-133R).
(b) Analyze the digestates for vanadium as follows:
(1) Perform the analysis using ICP-OES (or ICP-MS) using standard plasma conditions (1350 W forward power) and a desolvating microconcentric nebulizer, which will significantly reduce oxide- and chloride-based interferences.
(2) We recommend that you digest and analyze a minimum of three solid vanadium NIST Standard Reference Materials in duplicate with every batch of 25 vanadium alumina capture bed samples that you analyze in this section, as described in “Emissions of metals associated with motor vehicle roadways” (Herner, J.D. et al, Environmental Science and Technology. 2005, 39, 826-836). This will serve as a quality assurance check to help gauge the relative uncertainties in each measurement, specifically if the measurement errors are normally distributed and independent.
(3) Use the 3-sigma approach to determine the analytical method detection limits for vanadium and the 10-sigma approach if you determine the reporting limit. This process involves analyzing at least seven replicates of a reactor blank using the analytical method described in paragraphs (a) and (b)(1) of this section, converting the responses into concentration units, and calculating the standard deviation. Determine the detection limit by multiplying the standard deviation by 3 and adding it to the average. Determine the reporting limit by multiplying the standard deviation by 10 and adding it to the average. Determine the following analytical method detection limits:
(i) Determine the ICP-MS (or ICP-OES) instrumental detection limit (ng/L) by measuring at least seven blank samples made up of the reagents from paragraph (a) of this section.
(ii) Determine the method detection limit (µg/m 3 of flow) by measuring at least seven reactor blank samples taken as described in § 1065.1119(d).
(iii) We recommend that your method detection limit determined under paragraph (b)(3)(ii) of this section is at or below 15 µg/m 3 . You must report your detection limits determined in this paragraph (b)(3) and reporting limits (if determined) with your test results.
(4) If you account for vanadium-loaded particles contaminating catalyst-coated monoliths as a result of physical abrasion as allowed in § 1065.1115(f), use the 3-sigma approach to determine the analytical method detection limits for titanium and the 10-sigma approach if you determine the reporting limit. This process involves analyzing at least seven replicates of a blank using the analytical method described in paragraphs (a) and (b)(1) of this section, converting the responses into concentration units, and calculating the standard deviation. Determine the detection limit by multiplying the standard deviation by 3 and subtracting it from the average. Determine the reporting limit by multiplying the standard deviation by 10 and subtracting it from the average.
(i) Determine the ICP-MS (or ICP-OES) instrumental detection limit (ng/L) by measuring at least seven blank samples made up of the reagents from paragraph (a) of this section.
(ii) Determine the method detection limit (µg/m 3 of flow) by measuring at least seven reactor blank samples taken as described in § 1065.1119(d).
§ 1065.1123   General provisions for determining exhaust opacity.
The provisions of § 1065.1125 describe system specifications for measuring percent opacity of exhaust for all types of engines. The provisions of § 1065.1127 describe how to use such a system to determine percent opacity of engine exhaust for applications other than locomotives. See 40 CFR 1033.525 for measurement procedures for locomotives.
§ 1065.1125   Exhaust opacity measurement system.
Smokemeters measure exhaust opacity using full-flow open-path light extinction with a built-in light beam across the exhaust stack or plume. Prepare and install a smokemeter system as follows:
(a) Except as specified in paragraph (d) of this section, use a smokemeter capable of providing continuous measurement that meets the following specifications:
(1) Use an incandescent lamp with a color temperature between (2800 and 3250) K or a different light source with a spectral peak between (550 and 570) nm.
(2) Collimate the light beam to a nominal diameter of 3 centimeters and maximum divergence angle of 6 degrees.
(3) Include a photocell or photodiode as a detector. The detector must have a maximum spectral response between (550 and 570) nm, with less than 4 percent of that maximum response below 430 nm and above 680 nm. These specifications correspond to visual perception with the human eye.
(4) Use a collimating tube with an aperture that matches the diameter of the light beam. Restrict the detector to viewing within a 16 degree included angle.
(5) Optionally use an air curtain across the light source and detector window to minimize deposition of smoke particles, as long as it does not measurably affect the opacity of the sample.
(6) The diagram in the following figure illustrates the smokemeter configuration:
(b) Smokemeters for locomotive applications must have a full-scale response time of 0.5 seconds or less. Smokemeters for locomotive applications may attenuate signal responses with frequencies higher than 10 Hz with a separate low-pass electronic filter that has the following performance characteristics:
(1) Three decibel point: 10 Hz.
(2) Insertion loss: (0.0 ±0.5) dB.
(3) Selectivity: 12 dB down at 40 Hz minimum.
(4) Attenuation: 27 dB down at 40 Hz minimum.
(c) Configure exhaust systems as follows for measuring exhaust opacity:
(1) For locomotive applications:
(i) Optionally add a stack extension to the locomotive muffler.
(ii) For in-line measurements, the smokemeter is integral to the stack extension.
(iii) For end-of-line measurements, mount the smokemeter directly at the end of the stack extension or muffler.
(iv) For all testing, minimize distance from the optical centerline to the muffler outlet; in no case may it be more than 300 cm. The maximum allowable distance of unducted space upstream of the optical centerline is 50 cm, whether the unducted portion is upstream or downstream of the stack extensions.
(2) Meet the following specifications for all other applications:
(i) For in-line measurements, install the smokemeter in an exhaust pipe segment downstream of all engine components. This will typically be part of a laboratory configuration to route the exhaust to an analyzer. The exhaust pipe diameter must be constant within 3 exhaust pipe diameters before and after the smokemeter's optical centerline. The exhaust pipe diameter may not change by more than a 12-degree half-angle within 6 exhaust pipe diameters upstream of the smokemeter's optical centerline.
(ii) For end-of-line measurements with systems that vent exhaust to the ambient, add a stack extension and position the smokemeter such that its optical centerline is (2.5 ±0.625) cm upstream of the stack extension's exit. Configure the exhaust stack and extension such that at least the last 60 cm is a straight pipe with a circular cross section with an approximate inside diameter as specified in the following table:
Table 1 to Paragraph ( c )(2)( ii ) of § 1065.1125—Approximate Exhaust Pipe Diameter Based on Engine Power
(iii) For both in-line and end-of-line measurements, install the smokemeter so its optical centerline is (3 to 10) meters further downstream than the point in the exhaust stream that is farthest downstream considering all the following components: exhaust manifolds, turbocharger outlets, exhaust aftertreatment devices, and junction points for combining exhaust flow from multiple exhaust manifolds.
(3) Orient the light beam perpendicular to the direction of exhaust flow. Install the smokemeter so it does not influence exhaust flow distribution or the shape of the exhaust plume. Set up the smokemeter's optical path length as follows:
(i) For locomotive applications, the optical path length must be at least as wide as the exhaust plume.
(ii) For all other applications, the optical path length must be the same as the diameter of the exhaust flow. For noncircular exhaust configurations, set up the smokemeter such that the light beam's path length is across the longest axis with an optical path length equal to the hydraulic diameter of the exhaust flow.
(4) The smokemeter must not interfere with the engine's ability to meet the exhaust backpressure requirements in § 1065.130(h).
(5) For engines with multiple exhaust outlets, measure opacity using one of the following methods:
(i) Join the exhaust outlets together to form a single flow path and install the smokemeter (3 to 10) m downstream of the point where the exhaust streams converge or the last exhaust aftertreatment device, whichever is farthest downstream.
(ii) Install a smokemeter in each of the exhaust flow paths. Report all measured values. All measured values must comply with standards.
(6) The smokemeter may use purge air or a different method to prevent carbon or other exhaust deposits on the light source and detector. Such a method used with end-of-line measurements may not cause the smoke plume to change by more than 0.5 cm at the smokemeter. If such a method affects the smokemeter's optical path length, follow the smokemeter manufacturer's instructions to properly account for that effect.
(d) You may use smokemeters meeting alternative specifications as follows:
(1) You may use smokemeters that use other electronic or optical techniques if they employ substantially identical measurement principles and produce substantially equivalent results.
(2) You may ask us to approve the use of a smokemeter that relies on partial flow sampling. Follow the instrument manufacturer's installation, calibration, operation, and maintenance procedures if we approve your request. These procedures must include correcting for any change in the path length of the exhaust plume relative to the diameter of the engine's exhaust outlet.