### NOTICE

This technical report does not necessarily represent final EPA decisions or positions. It is intended to present technical analysis of issues using data that are currently available. The purpose in the release of such reports is to facilitate the exchange of technical information and to inform the public of technical developments. 

### Assessment and Standards Division Office of Transportation and Air Quality U.S. Environmental Protection Agency

National Renewable Energy Laboratory U.S. Department of Energy

Coordinating Research Council 

# EPAct/V2/E

- 89: Assessing the Effect of Five Gasoline Properties on Exhaust Emissions from Light

- Duty Vehicles Certified to Tier 2 Standards

Final Report on Program Design and Data Collection

Appendix K Detailed Measurement and Analysis Methods

E PA-420-R-13-004 April 2013

### K-1 A. QA OBJECTIVES FOR TESTI NG OF LIGHT

- DUTY VEHICLES

The QA objectives for precision, accuracy, and completeness are presented in Table 1. All measurements will be representative of the fuels, vehicle engine exhaust, and conditions being measured. Completeness equals number of tests performed divided by number of tests proposed times 100.

TABLE 1. PRECISION, ACCURACY, AND COMPLETENESS OBJECTIVES FOR LIGHT

DUTY ENGINES

Measurement Experimental Precision

Parameter (Method) Reference Conditions Std. Dev. Accuracy,% Completeness,%

HC SwRI and Dilute 0.04 a ±15 b >95

(FID) SAE a,b Exhaust

CO SwRI and Dilute 0.06 b ±20 b >95

(NDIR) SAE a,b Exhaust

CO 2 SwRI and Dilute 4 b ±5 b >95

(NDIR) SAE a,b Exhaust

NO

x SwRI and Dilute 0.08 a ±10 b >95

(CL) SAE a,b Exhaust

Particulate, 47 mm SwRI and Dilute 0.05 a ±10 b >95
(Gravimetric) SAE a,b Exhaust

Fuel Economy SwRI and Dilute 1 a ±5 b >95 (Carbon Balance) SAE a,b Exhaust

Aldehydes EPA (1,2) Dilute See Appendix K >95 (DNPH/HPLC) CRC (3) Exhaust

Alcohols EPA (1,2) Dilute See Appendix K >9 5 (water impinger/GC

- FID) CRC (3) Exhaust

________________________ a Precision experienced at SwRI, but precision is vehicle dependent.
b Accuracy goals were based on SwRI experience and SAE Technical Paper 790232, "Iden tification, Quantification

and Reduction of Sources of Variability in Vehicle Emissions and Fuel Economy Measurements," N.J. Sheth and T.I. Rice, 1979.

c ±100% of defined detection limit; precision generally improves with increase d sample concentration.

### K-2 B. SAMPLING METHODS

The sampling system is comprised primarily of the exhaust sampling system to which continuous measurement devices, a dilute exhaust bag sampler, impinger and cartridge samplers,
and particle filters are attached. The sampling procedures employed for the determination of regulated and unregulated emissions for light

- duty engines are identified below. In the event of errors, mishaps, or deviations from procedure, the project leader, Kevin Whitney is to be
notified.

All procedures will be designed to maximize test

- to

- test repeatability. For example, the following steps will be taken:

• The position and angle of the vehicle cooling fan shall be consistent for each vehicle and
each test.

• The airflow around the vehicle during tests shall be kept consistent.

• To the extent possible, the CARB laboratory correlation program will be used in support of this program’s QA procedures.

• Sample side verification of exhaust analyzers will be performed monthly by sampling span gases from a sample bag.

• Sample flow proportionality will be verified after each emissions test. For PM samples, a proportionality statistic will be calculated. For other parameters, the constancy of tunnel
flows will be verified.

• Duplicate vehicle coastdown checks from 70 to 30 mph will be performed following each sulfur purge procedure.

• A check will be performed before, during, and at the en d of each test to assure than manually controlled parameters are set and adhered to during each test.

• Battery chargers will be utilized to maintain the state of battery charge of test vehicles between vehicle prep procedures and emissions tests.

• The LA92 driving cycle will be used for the vehicle prep procedures to match the driving cycle used in emissions tests.

• NOx analyzers will be equipped with NH3 traps to prevent contamination of NOx

converters.

B.1. Exhaust Gas Sampling System Description

A Horiba selectable flow CVS system will be used to sample exhaust emissions. Test technicians first connect the vehicle exhaust pipe to the CVS inlet. While the vehicle operates on the dynamometer, an adjustable

- speed turbine blower dilutes the exhaust with ambient air. This dilution prevents the exhaust moisture from condensing and provides controllable sampling
cond itions. A sample pump and a control system transfers diluted exhaust aliquots to several different Kynar bags during specific phases of each test run. Regulating needle valves maintain constant sample flow rates for the alcohol impingers and DNPH cartrid ges, and mass flow controllers maintain proper flow into the bags. Exhaust backpressure will be recorded continuously at the tailpipe during emissions testing. Table 2 summarizes the CVS system specifications.

### K-3 TABLE 2. CVS SPECIF ICATIONS

Measurement
Variable Operating Range Expected in Field Instrument Description Range Accuracy How Verified /
Determined

Pressure 950 to 1050 millibar

Horiba Variable

Flow Constant Volume Sampler 0 to 1500
millibar ± 2 % reading Sensors calibrated
and verified during installation. Temperature 20 to 45 °C 0 to 100 °C ± 2 % reading

Volumetric Flow
Rate 200 to 500 ft 3 /min 150 to 1100
ft 3 /min ± 0.5 % reading



### B.2. Dilute Exhaust Bag Sampling

The Kynar bags (sample and background) specified for HC speciation analysis will be removed from the Horiba sampling system, marked with a sample ID/custody label, and transported to the GC laboratory. Analysis of sample Bag 1 will begin immediately (within one hour) for the C 1 

### -C 4 

### analysis and within four hours for the b enzene

- toluene and C 5 

### -C 12 

### analysis. Times that analyses are started will be reported. For tests in which multiple test phases will be analyzed for HC speciation, analysis order shall be: Bag 1, Bag 3, Bag 2, Background Bags.

B.3. Carbonyl Compound Sampling

Heated (235 ±15 ̊ F ) sample lines from the dilution tunnel carry sample gas to a cart which holds the DNPH sampling cartridges. The cart includes controls for the flow rate and measures the volume sampled. Thermocouples with electronic readouts allow recording of the gas temperature sampled, so coupled with the recorded barometric pressure, the volume sampled can be corrected to standard temperature and pressure.

Immediately following the end of the sampled test phase (within 15 minutes), the DNPH

ca rtridge will be extracted with 5.0 ml acetonitrile in accordance with the manufacturer’s instructions. The extract will be promptly sealed and analyzed (within one hour), or stored at
<40 ° 

### F for no longer than three calendar days until analysis. Every eff ort will be made to analyze the sample the same day. Samples and sampling media will be stored separately from calibration
standards.

B.4. Alcohol Sampling

Heated (235 ±15 ̊ F ) sample lines from the dilution tunnel carry sample gas to a cart
which holds glass impingers filled with ultra

- pure water. The cart includes controls for the flow rate and measures the volume sampled. Thermocouples with electronic readouts allow recording of gas temperature sampled, so coupled with the recorded barometric pressure, the volume sampled can be corrected to standard temperature and pressure. The impingers are maintained in an ice bath during sampling.

Immediately following the end of the sampled test phase, the impinger contents will be carefully transferred to sea led containers and stored at <40 ° 

### F for no longer than six calendar days until analysis. Every effort will be made to analyze the samples on the same day as collection. Samples and sampling media will be stored separately from calibration standards.

### K-4 Eth anol recovery will be checked during every blank test conducted in this program. Recovery shall be ≥92 percent.

B.5. Filter Sampling and Weighing

Whatman Teflo filters with polypropylene support rings will be used for particulate matter (PM) measuremen ts. Particle filters are stored, conditioned, and weighed in a room at SwRI that strictly conforms to 40 CFR 86.1312 and Part 1065. A PM filter field blank will be tested daily. This field blank shall be a tared filter that is installed in a sample hold er, then returned to the filter room for weighing by the same procedures as actual samples.

C. SAMPLE HANDLING AND CUSTODY

Only PM filters, bag, impinger, and cartridge samples involve manual handling, because gaseous emission measurements are made and recorded by the computer

- controlled data system associated with the continuous sampling system.

C.1. Particle Filters

Particle filters are managed by a bar code tracking system. Test I.D., date, time, and technician name are tracked with this system. This procedure is compliant with 40 CFR 86.1312
and Part 1065.

C.2. Bag Samples

Because bag samples may be handled by multiple analysts, a bag sample tag is affixed to each sample or background bag. With this tag, progress and times of analysis can be recorded. A bag sample tag is shown in Figure 1.

### K-5 BAG ANALYSIS

S A M P L E

Project No. 13363.01.101 EPA Work Assignment 0-1

Test No.: Date: / /

Dyno 8 Operator:

Bag Description

LA

- 92 Unified Cycle

□ Bag 1 End of Test :____ :_____

□ Bag 2 End of Test :____ :_____

□ Bag 3 End of Test :____ :_____

Analysis Required Analysis Start (Time) Analyzed by:

□ C 1 

### -C 4 

### speciation :

□ Benz

- Tol speciation :

□ C 5 

### -C 12 

### speciation :

FIGURE 1. BAG SAMPL E TAG

### K-6 C.3. Cartridge and Impinger Samples

Sampling of carbonyl compounds is to be performed with DNPH cartridges, and alcohols, with liquid impingers, as described above. Tracking of sample times and extraction times will be made by recording times on the cartridge tag (Figure 2) and impinger data sheet (Figure 3).

ALDEHYDE DNPH CARTRIDGE

Project No. 13363.01.101 EPA Work Assignment 0-1

Test No.: Date: / /

Dyno 8 Analyst:

Bag Description

LA

- 92 Unified Cycle □ Bag 1 End of Test :____ :_____ □ Bag 2 End of Test :____ :_____ □ Bag 3 End of Test :____ :_____

Cartridge Extraction Required within 15 min Extraction (Time) Analyst
Initials:

□ Bag 1 :

□ Bag 2 :

□ Bag 3 :

□ Background :

FIGURE 2. DNPH CARTRIDGE TAG

### K-7 Project 13363.01.101 Date: / / Dyno 8 Initials:

Test Number: 

### DNPH Cartridge Alcohol Impinger
Sample Background Sample Background

Test Cycle: Temp: Temp: Temp: Temp:

Barameter, “Hg: Counts: Counts: Counts: Counts:

End Time: Sx 1° Sx 2° Sx 1° Sx 2°

Test Cycle: Temp: Temp: Temp: Temp:

Barameter, “Hg: Counts: Counts: Counts: Counts:

End Time: Sx 1° Sx 2° Sx 1° Sx 2°

Test Cycle: Temp: Temp: Temp: Temp:

Barameter, “Hg: Counts: Counts: Counts: Counts:

End Time: Sx 1° Sx 2° Sx 1° Sx 2°



### FIGURE 3. IMPINGER AND CARTRIDGE SAMPLING DATA SHEET

D. ANALYTICAL METHODS

The analytical procedures employed for the determination of regulated and unregulated emissions for light

- duty engines are given below. 

### In the event of errors, mishaps, or deviations from procedure, the project leader, Kevin Whitney is to be notified.

D.1. Filter Weighing

The chamber in which the PM filters are conditioned and weighed conforms to 40 CFR
86.1339 and Part 1065 without deviation.

D.2. Gaseous Analyzers

Horiba analytical benches equipped with either MEXA 7000

- Series analyzers are used to determine NMHC, CO, NO X 

### , and CO 2 

### concentrations in dilute exhaust. Sample pumps transfer the dilute exhaust from Kynar bags to each analyzer as commanded by the control system. Each analyzer used for these measurements is accurate to ± 2 percent. Table 3 provides a summary of the emissions analyzers to be used.

### K-8 TABLE 3 . EMISSION ANALYZER SPECIFICATIONS

Measurement
Variable Expected Operating

Range Instrument Mfg., Model / Type Instrument Range(s) Accuracy a How Verified /
Determined

THC 0

- 100 ppmC Horiba FIA

- 220

or FIA

- 726LE

/ FID 0

- 10 ppmC

0

- 50 ppmC

0

- 1000 ppmC

± 1.0 % FS

or ± 2.0 %
of the
calibration point a Gas divider with protocol calibration gases at 11 points (minimum) spaced throughout span (including zero) NO X 0

- 100 ppm Horiba CLA

- 220
or CLA

- 750LE

/ CL 0

- 30 ppm

0

- 100 ppm

0

- 300 ppm

Low CO 0

- 50 ppm Horiba AIA

- 210
or AIA

- 721LE

/ NDIR 0

- 10 ppm

0

- 50 ppm

CO 0

- 1000 ppm Horiba AIA

- 220

or AIA

- 721A

/ NDIR 0

- 1000 ppm

CO 2 0

- 1.5 % Horiba AIA

- 220

or AIA

- 722

/ NDIR 0

- 4 %

a The most stringent accuracy specification applies for each calibration point.



### E. QUALITY CONTROL

SwRI verifies performance of each analyzer through a series of zero and calibration gas challenges. Each zero and calibration gas must conform to certain specifications and/or be
NIST

- traceable. Table 4 summarizes the applicable QA/QC checks. If all cal ibration gases and QA/QC checks meet their specifications, then SwRI will infer that the emissions analyzers meet Table 1 accuracy specifications.

SwRI verifies all new Standard Reference Material (SRM) or other NIST

- traceable reference gas concentrations with an emissions analyzer that has been calibrated within the last 30 days. The operator will first zero the analyzer with a certified zero grade gas and then span it with a NIST SRM (or equivalent) three times to ensure stability and minimal analyzer d rift.

The operator will then introduce the new reference gas into the analyzer and record the concentration, followed by reintroduction of the NIST SRM to ensure that the analyzer span point does not drift more than ±0.1 percent of span point. The operat or will repeat these last two steps until three consistent values are obtained. The mean of these three determinations must be within one percent of its NIST SRM concentration. SwRI will then consider the reference gas as suitable for emissions analyzer calibrations.

### K-9 For chemical evaluations, QC measures are generally specified in the analytical method. A summary of actions taken to ensure data quality for analytical procedures is presented in
Table 5.

TABLE 4 . EMISSION ANALYZER QA/QC CHECKS

QA/QC Check When Performed / Frequency Expected or
Allowable Result Response to Check
Failure or Out of
Control Condition

NIST

- traceable calibration gas
verifications Prior to being put
into service Average of three readings must
be within ± 1 % of verified NIST
SRM concentration Identify cause of any problem and correct;
discard bottle and replace if necessary

Zero

- gas verification against NIST certified zero gases Prior to being put
into service HC < 1 ppmC CO < 1 ppm
CO 2 < 400 ppm
NO

x < 0.1 ppm
O 2 between 18 and 21% Discard bottle and replace

Gas divider linearity verification Monthly All points within ± 2 % of linear
fit

FS within ± 0.5 % of known
value Identify cause of any problem and correct; replace gas divider if

necessary

Analyzer calibrations Monthly All values within ± 2% of point

or ± 1% of FS; Zero point within ± 0.2% of FS

Identify cause of any problem and correct; recalibrate analyzer Wet CO 2 interference check Monthly CO 0 to 300 ppm, interference ≤ 3 ppm

CO > 300 ppm, interference ≤
1% FS

NO X analyzer interference check Monthly CO 2 interference ≤ 3%

NO X analyzer water quench check Once, before each phase of program Proper opreration

NO X analyzer converter efficiency
check Monthly NO

x converter efficiency > 95%



### TABLE 5 . SUMMARY OF QA/QC CHECKS FOR ANALYTICAL PROCEDURES

Procedure Type Blank Field
Blank Duplicate Analysis Continuing
Calibration
Check Holding
Time Preservation During Storage Light
Alcohols GC

- FID 1 per batch 1 per day 1 per 10 samples 1 per 10 samples 6 days Keep at
<4 ◦ 

### F Aldehydes
and
Ketones HPLC

- UV 1 per batch 1 per day 1 per 10 samples 1 per 10 samples 15 minutes to extraction; 3 days Keep at
<4 ◦ 

### F

HC Speciation GC

- FID 1 per day n/a no end of day 1 hour for C2

- C4 Analysis protect from UV light
Particulate

Matter
Mass Gravimetric Reference filter every

2 hours n/a At least three

measurements on each filter Monthly
reference

check Filters may be
out of chamber

only ≤ 1 hr Temperature and humidity
control

### K-10 F. INSTRUMENT/EQUIPMENT TESTING, INSPECTION, AND MAINTENANCE

Gaseous analyzers conform to 40 CFR 86.1311 without deviation. Internal QC checks
and corrective actions are summarized in Table 6.

TABLE 6 . INTERNAL QUALITY CONTROL CHECKS AND CORRECTIVE
ACTION

EQUIPMENT
AND/OR
MEASUREMENT OPERATIONAL CHECK CONTROL LIMIT(S) ( reference no.) CORRECTIVE
ACTION

Driver's aid Speed agreement a EPA (29) Repair and/or
recalibrate

CVS Propane recovery b ±2% (25,29) Check for leaks and by procedural

assessment

Speed, RPM a ±5% (25,29) Check speed sensor and recalibrate rpm

Engine Dynamometer Load and Speed, RPM a Federal Register (25) Check and/or repair load cell and rpm indicator; recalibrate

CO bag analyzer CaSO 4 and ascarite conditioning column Blue indicator of CaSO 4 (25,29) Change CaSO 4 and

ascarite column soon
after CaSO 4 indicator

turns color. Leak
check before continuing bag analysis.

NO x bag analyzer Percent efficiency of NO 2 to

NO converter b Percent efficiency greater

than 90% (25,29) Repair analyzer

Sampling bags Leak

- check bags before and
after each test Bag holds gauge vacuum pressure of 27.6 in. Hg Discard bag and note finding in test results. Repeat test as applicable.

HFID analyzer Leak

- check sampling system a Flowmeter float is at zero position Correct leak before sample analysis

Sample gas temperature immediately before heated
filter and before the HFID a 375±10 ° F (25,29) Locate sampling line heating problem and
correct before conducting sample analysis

Zero and span before each

range c Zero at 0.0 of full
- scale and span to set value (25,29) Determine problem and adjust zero and span accordingly

Pre

- analysis and post
analysis zero and span of each range c Zero and span drift

- limit of 2% of full
- scale chart

deflection (25,29) Repeat test

Pre

- analysis and post
analysis tunnel HC back
grounds c Continuous tunnel and bag HC backgrounds agree to
within l% of full

- scale chart

deflection (25,29) Determine cause for discrepanc y and

correct

### K-11 TABLE 6 . INTERNAL QUALITY CONTROL CHECKS AND CORRECTIVE
ACTION

EQUIPMENT
AND/OR
MEASUREMENT OPERATIONAL CHECK CONTROL LIMIT(S) ( reference no.) CORRECTIVE
ACTION

47 mm filter sampling system Leak

- check sampling system a Flowmeter float is at zero position Correct leak before particulate sampling

Sampling rate c Flowrate constant ±5% throughout test Check for leaks or
restrictions on sampling line and
filter

47 mm reference
filters Weight tolerance c ±1% of the nominal filter loading (27) Reweigh all filters being conditioned

Particle Dilution
Tunnel Particle sampling zone temperature c 125 ° F or less Increase level of sample dilution

Aldehydes and
ketones Leak

- check sampling system c Flowmeter float is at zero position Correct leak before sample collection

Sampling rate c Flowrate constant ±5% throughout test Check for leaks or
restrictions on sampling line and
filter

Dry gas meter volume d Compare to flowmeter
estimate Recalibrate or replace dry gas meter

Aldehydes and
ketones Sample identification c Date, project, cycle, and test no. if designated Correct labeling

Sample preparation c Within 15 minutes of end of sampled phase Void sample

Sample analysis c Within 3 days of end of sampled date Void sample

HC, CO, NO x , and CO bag analyzers Leak

- check analyzer sampling system a Flowmeter float at zero position Correct leak before bag analysis

Zero and span before each

range c Zero at 0.0 of full

- scale and span to set value (25,29) If not adjustable using analyzer zero and gain control within specified limits, repair analyzer

Pre

- analysis and post
analysis zero and span of each range c Zero and span drift limit of
2% of full

- scale meter reading (25,29) Repeat bag analysis



### In the event of out of specification conditions, equipment should be repaired and
recalibrated. If a significant delay will result, the project leader, Kevin Whitney is to be notified.

G. I NSTRUMENT/EQUIPMENT CALIBRATION AND FREQUENCY

Sampling and analytical methodologies and test procedures adhere to Title 40 CFR Parts 86 and 600 requirements. All equipment calibrations are conducted according to the schedules in 40 CFR § 86.116. Table 7 summarizes the relevant calibrations, Title 40 CFR citations, and their frequencies. Calibrations and QA/QC checks are discussed in more detail below.

### K-12 TABLE 7 . EQUIPMENT CALIBRATIONS SUMMARY

Equipment Description Title 40 CFR
Procedure Calibration Frequency

CO analyzer § 86.121 Monthly

CO 2 

### analyzer § 86.122 Monthly

HC analyzer § 86.124 Monthly

NO X 

### analyzer § 86.123 Monthly
Chassis dynamometer § 86.118 Daily

CVS system § 86.119 Weekly
Speciated Hydrocarbons EPA (41) 

### Each Sample Set

Alcohols EPA (39) 

### Each Sample Set

Aldehydes and Ketones EPA (1, 2, 3) 

### Each Sample Set

Analytical equipment in the chemistry laboratories is calibrated at least once daily, with a calibration verification performed at the end of the batch.

G.1. Gas Meter Calibrations



## A ll gas meters, selected from the list of routinely used instruments given in the recall database, are calibrated to conform to 40 CFR 86.1320. Any necessary correction is made by mechanically adjusting the meter and recalibrating.

G.2. Gaseous Analyzers

The gaseous analyzers to be utilized in this program are discussed in the following
sections.

G.2.1. Hydrocarbon Analyzers

The HC analyzers used in this testing program are calibrated in conformance with 40
CFR 86.1321.

G.2.2. Carbon Monoxide Analyzers

The CO analyzers used in this testing program are calibrated in conformance with 40
CFR 86.1322 and 40 CFR 89.320.

G.2.3. Oxides of Nitrogen Analyzers

The NO
x 

### analyzers used in this testing program are calibrated in conformance with 40
CFR 86.1323 and 40 CFR 89.321.

### K-13 G.2.4. Carbon Dioxide Analyzers

The carbon dioxide (CO 2 

### ) analyzers used in this testing program are calibrated in
conformance with 40 CFR 86.1324 and 40 CFR 89.322.

G.2.5. Methane Analyzers

The methane analyzers used in this testing program are calibrated in conformance with 40 CFR 86.1325, without deviation.

G.3. Analyzer Gases

The gases used for instrument calibration conform to 40 CFR 86.114 and 40 CFR 89.312
without deviation.

SwRI verifies each new working zero air (or N 2 

### ) cylinder’s impurities to ensure that it is
suitable for emissions analyzer zero checks. Comparisons between a certified Vehicle Emission Zero (VEZ) Gas (or equivalent) and the candidate zero gas will serve this purpose. SwRI will employ an emissions ca rt (or suite of instruments) that has been calibrated within the last 30 days for this procedure. The operator will zero the analyzers with certified VEZ gas and span them
with NIST

- traceable reference gases to ensure stability and minimal analyzer drift. The operator will then introduce the candidate cylinder’s zero gas to the sample train and record the HC, CO,
CO 2 

### , and NO
x 

### values. The results must fall within specified ranges for the zero gas to be deemed suitable for instrumental analyzer calibration s.

Prior to the monthly exhaust emission analyzer calibrations, SwRI verifies the calibration gas divider linearity with an HC analyzer known to have a linear response and a HC span gas. The operator will first zero and then span the instrument such that the span occupies 100 meter or chart divisions. The operator will operate the divider in each of its settings in descending order and compare the observed results with a linear scale. The difference between the
commanded and observed concentrations must be within ±2.0 percent of the commanded concentration. Also, this difference must be less than ± 0.5 percent of the span value.

NIST

- traceable calibration gases, in conjunction with a verified gas divider and zero gas, will create individual gas concentrations with which to challenge each instrumental analyzer. The gas divider will generate 11 concentrations in 10 percent increments from 0 to 100 percent of each analyzer’s span. Analyzer response at each point must be within ± 2.0 percent of the

concentr ation or ± 1.0 percent of span, whichever is more stringent. Zero gas response must be

within ± 0.2 percent of span (the CFR requires ± 0.3 percent). If any point is outside these limits, operators will generate a new calibration curve.

### K-14 REFERENCES

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- 02

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