P.1 

OAR Box 1827 

Prepped by Charmelle Mathews 

Document Number: 

139) ll-A-9 

Docket Number: 

A-90-07 

Printed 11/19/2008 12:40:48 PM Sheet 139 of 147 
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\ '-

A-90-07 

Research Protocol Method for 

Analysis of Detailed Hydrocarbons emitted from Automobiles 

by Gas Chromatography 

Prepared by 

John E. Sigsby Jr. 

U.S. Environmental Protection Agency 

Research Triangle Park, North Carolina 27711 

and 

William Crews and Paula Siudak 

Mantech Environmental Inc 

Prepared for 

U.S. Environmental Protection Agency 

Mobile Source Emission Research Branch 

Chemical Processes and Characterization Division 

Atmospheric Research and Exposure Assessment Laboratory 

Originally Prepared 

June 1989 

Revised 

June 1991 
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Disclaimer 

The Research Protocol/Method (RPM) described herein should not be 

interpreted as a generally accepted standard or equivalent method 

or procedure. This RPM was developed for use within the Mobile 

Source Emission Research Branch and may not be applicable to the 

needs of other organi2ations. 
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REVISIONS 

Revision 1 

Original write up, cleared June 30, 1989 

Revision 2 

Front end on System A changed to provide propane propylene 

split. 

Revision 3 

Perkin Elmer 8700 on line with dual FID's. 
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1.0 Scope and Application 

This recommended method is intended for the analysis of 

detailed hydrocarbons (HC) in the emissions from Mobile Sources. 

The method(s) minimum quantification and detection limit are 

determined by the total volume of sample taken. The level of 

quantification is 3 times the limit of detection. Typical values 

for the limit of detection are around 0.01 ppm with a ten cc 

sample. This method is intended to provide a general assessment 

of the nature of the emissions and not to be an absolute 

definition of them. If the emission level of a specific component 

is of overriding interest, a separate analysis for that compound 

should be made. See also Interferences, Section 4.0. 

2.0 Summary of Method 

There are two separate analytical systems in use within the 

Branch. They both use the same basic methodology but with 

different specific parameters due to the difference in the 

instrumentation utilized. One system utilizes Perkin Elmer (P&E) 

Gas Chromatographs, SYSTEM A, while the other is based on the use 

of Hewlett Packard Model 5880 Gas Chromatographs (HP),SYSTEM B. 

Both systems transfer the raw data to a PC-AT or compatible 

where the data is verified and final editing takes place. The 

data is then transferred to a central PC for final calculations 

and merging into the laboratory data base for final reporting. 

Samples up to about 150 ppm carbon are analyzed on these 

systems. Samples containing higher concentrations are diluted 

into this range. 

Each system takes a known and precisely measured volume of 

sample and measures a wide variety of hydrocarbons using flame 

ionization detection. Separate samples are taken for methane. The 

two through three carbon hydrocarbons can either be analyzed by a 

seperate sample or with the two through eleven carbon 

hydrocarbons. 

Each system records the output of the flame ionization 

detector (FID) through an integrally configured integration and 

recording system that records the data along with appropriate 

retention times which allows for future re-editing of the data as 

well as delivering "identified" chromatographic peaks. The signal 

is also recorded on a strip chart recorder as it is being 

created. 

4.0 Interferences 

Any compound that co-elutes with an identified hydrocarbon 
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may be termed an interferant. These may be hydrocarbons, in which 

case the response factor (in ppm Carbon/area) will be similar to 

that of the compound identified, or it may be of a different 

organic class with a correspondingly different FID response. In 

the latter case the quantification will be adversely effected and 

invalidated to the extent of the response differences. In the 

case of a co-eluting hydrocarbon, the quantitative mass 

calculation will not be grossly affected on a carbon basis but 

any subsequent interpretation of the results may be in error due 

to the misidentification, particularly if the two hydrocarbons 

are of different classes, for example paraffins and olefins. 

5.0 Personnel Requirements 

The researcher utilizing this procedure is expected to be 

familiar with gas chromatography, its practice, and its 

application to hydrocarbon analysis. In addition, the operator is 

expected to be familiar with good analytical practice. The 

operator will be expected to optimize the gas chromatograph and 

operate it. The instrument manual may be an aide in this 

activity. The procedures utilized are the result of many years of 

research and involve considerable modification of the purchased 

instrumentation. Normal operating procedures include: start up, 

both daily and after shut down; sensitivity determination; 

maintenance schedules; sample preparation; and the regular 

reporting of analytical results, both routine and those that are 

at variance with expectation. 

6.0 Facilities Requirements 

No special laboratory facilities are required. 

7.0 Safety Requirements 

Calibration standards, samples, and most laboratory reagents 

used in this method pose no unusual hazard to the researcher, if 

normal laboratory safety practices are followed. Eye and hand 

protection is required when using cryogens. Compressed gases must 

be stored and handled properly. Electrical connections can pose a 

hazard if improperly made or left exposed. 

The American Chemical Society ( ACS ) guidelines regarding 

the handling of chemicals used in these methods should be 

followed. 

7.3 Heated Surfaces 

The GC injection ports, column, column oven, and detectors 

may be maintained at temperatures high enough to cause burns. The 

researcher should exercise caution and avoid contact with these 
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surfaces. 

7.5 Compressed Gases 

See pages F14 through F18 of the EPA/RTP Safety manual 

(reference 2) for safety precautions. 

7.5.2 Cryogenic Liquids, (Liquid Nitrogen) 

See pages F18 through F20 of the EPA/RTP Safety Manual 

(reference 2) for precautions. 

WARNING - Cryogenic fluid . May cause severe frostbite. Wear 

hand and eye protection. Use with adequate room ventilation. Keep 

contact with air to the minimum to avoid build up of liquid 

oxygen. 

8.0. Apparatus and Equipment 

This section defines the specific instrumental requirements 

of this method. 

8.1 Gas Chromatograph 

The gas chromatographs used in this method are equipped for 

sub-ambient temperature programing, have a flame ionization 

detector (FID) and an electronic integrator. 

The instruments used are: 

System Al: Perkin Elmer Sigma 2000 and integrator 

System A2: Perkin Elmer 8700 and integrator 

System B: Hewlett Packard 5880A Gas chromatograph. 

Each system is described separately, where appropriate. 

8.1.1 Gas Chromatograph Column 

Up to three different columns are used in this analysis. 

Column I: Higher molecular weight hydrocarbons through Cll. 

Type: Fused Silica Capillary column 

Diameter: 0.32 

Length: 60 meters X 2 = 120 meters 
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Liquid Phase: DB-1, Methyl Silicone bonded liquid phase 

Liquid Phase Thickness: 1.0 um 

Column II: Methane - System A & B 

Type: Packed solid adsorbent 

Diameter: 1/8 th inch OD Stainless Steel 

Length: 6 feet 

Packing Material: 60 - 80 mesh, 13X Molecular sieve 

Column III: Two and Three Carbon Hydrocarbons 

Type: Packed solid adsorbent 

Diameter: 1/8 inch OD Stainless Steel 

t 

Length: 6 feet 

Packing Material: 40 -60 mesh, Type 58 Silica Gel 

8.1.2B Inlet System A2 & B 

The inlet system is illustrated in Figures 1B1 and 1B2. 

8.1.2.1 Connection of inlet system to column 

The capillary column is connected directly to the sampling 

valve using a Swagelok capillary column connector and graphite 

ferrules. The packed columns are connected using standard 1/8-

in to 1/16-in Swagelok reducing unions and 316 stainless steel 

ferrules. 

8.1.3 Sample Loop 

The sample loop is constructed of clean, chromatographic 

grade 1/8-in OD stainless steel tubing. A 4-ft in length, which 

is coiled to fit inside the sampler housing or gas chromatograph. 

The loop is flushed with methylene chloride and dried with zero 

grade air prior to use. 

8.1.3.1 Sample Trap 

The sample trap is constructed of clean, chromatographic grade 
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l/9-in OD stainless steel tubing. A 6-inch in length is firmly 

packed with 10.2 cm of glass wool. A temperature controller 

maintains concentration and desorption temperatures. The 

controller is set to -170 degrees C (temperature maintained by 

using liquid nitrogen) for trapping two through eleven carbon 

hydrocarbons and ramped to +200 degrees C for desorption. The 

trap is wrapped with insulation tape to prevent cold and hot 

spots. 

8.5 Tubing and Connectors 

All tubing is chromatographic grade stainless steel. All 

connections are made with stainless steal compression tube 

fittings. (Swagelok or equivalent). 

8.6- Regulators for Compressed Gases 

Carrier gas, hydrogen, and air delivery pressures are 

controlled by two stage regulators mounted at the tank. 

Caution: Due to the possibility of contamination by organic 

materials, only regulators with stainless steel 

diaphragms should be used. 

9.0 Reagents/Materials 

All gases used to operate the GC system should be the 

highest grade reasonable. Detailed specifications may vary 

between manufacturers but should be restricive enough so as not 

to cause any decrease in instrument performance. Propane 

calibration gases are obtained from NIST (NBS) and are SRM's. 

Other calibration materials are fabricated by using the highest 

obtainable grade of hydrocarbon and diluting in known volumes of 

zero grade or better air. 

9.1 Gases and Cryogens 

The following are recommended for use with this method. 

9.1.1 Helium Carrier Gas 

High Purity, minimum purity of 99.995 percent helium, Bureau 

of Mines 

9.1.2 Detector Air 

Zero Grade, with total hydrocarbon less than 1 ppm carbon, 

containing 20 +/- 0.5 % oxygen 

9.1.3 Detector Hydrogen 
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Pre-purified grade, 99.99 percent hydrogen or better 

9.1.5 Liquid Nitrogen ( for GC oven cooling) 

Commercial grade is acceptable 

9.1.8 Propane in Air, Benzene in Air, two through twelve carbon 

hydrocarbon mixture in Air ( for calibration). Either or all may 

be available 

NIST (NBS) SRM 1665, 3 ppm compound in air (nominal) 

NIST SRM 1666, 10 ppm compound in air 

NATIONAL SPECILITY GAS (NIST TRACEABLE) 25 ppmC (C2 - Cll, 

see also section 11.3.2) 

SCOTT SRM CAL 6495, 0.254 ppm in air 

9.1.9 Instrument Air Vacuum 

The six port Seiscor gas sampling valves require clean, 

filtered air at 350 kpa (35 psig) and a clean vacuum of 

approximately 20 in Hg for proper operation. 

11.3 Gas Chromatograph Calibration 

Calibration of these instruments in the parts per million 

carbon range (ppm C) is performed using the following procedure. 

11.3.1 Instrument Optimization 

A propane in air sample should first be analyzed and 

adjustments made to the carrier gas linear velocity such that the 

propane peak elutes at approximately 14.5 minutes following 

injection. The hydrocarbon compounds should elute in the order of 

retention times as shown in Table 1 when using the capillary 

column and other columns as specified in this document. The 

elution times should be determined by preparing and analyzing 

known samples of each compound and/or known mixtures of the 

compounds expected, such as the gasoline used in the experiment 

or of known calibration mixtures. The more complex the mixture 

the greater is the surety that the retention order has been 

maintained. The precise retention times depend upon column 

length, carrier flow rate, effective column temperature, etc. 

The flame-ionization detector hydrogen and air flow rates 

are controlled by critical orifices installed by the 

manufacturer. Proper head pressures are specified for optimum 
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signal to noise ratio. System Al: Pressures for the Perkin Elmer 

2000 are set with the air pressure at 40 psig and the hydrogen at 

20 psig on detector and helium carrier at 65 psig. System A2: 

Pressures for the Perkin Elmer 8700 are set with the air pressure 

at 22 psig and hydrogen pressure at 22'psig at the detector, and 

the helium carrier at 60 and 67 psig. System B: Pressures for 

the HP 5880 are specified as Air at 40 psig, Hydrogen at 40 psig, 

and helium at 68 psig. The carrier gas flow on each system is 

adjusted to provide optimum separation. 

11.3.2 Calibration 

The response of the FID is assumed to be linear with respect 

to the number of carbon atoms present in the detected compound. 

Thus, it is convenient to measure compound peak concentration in 

terms of parts per million carbon (ppm C) where: 

Concentration ppm C = (number of carbon atoms in the compound) x 

(concentration ppm Molar) 

For a fixed sample volume, the concentration is proportional 

to the area under the chromatographic peak. The area under the 

peak is converted to ppm C concentrations in the computer by the 

following calculation: 

Cone, ppm C = (k)(Area) 

Area is given in integrator counts and* k is an 

experimentally determined calibration constant (ppm C/count). 

Multiple values of k are used depending on compound retention 

time and class, a fifth order polynomial fit is used to apply the 

response factors for the two through eleven carbon hydrocarbons. 

A calibration mixture of about 14 compounds is used for 

instrument calibration and daily span checks. The cylinders are 

from National Welders Specialty Gases and are certified by them. 

A typical Certificate is shown as Figure 2. A typical mixture 

might include; propane, isobutane, n-butane, isopentane, 2-

methylpentane, benzene, cyclohexane, n-heptane, toluene, noctane, para-&-meta xylene, , ortho-xylene, n-nonane, and ndecane. A separate cylinder containing methane is used for that 

analysis. A minimum of six injections are performed on a 

quarterly basis and the instrument response recorded. A control 

chart is generated from this data and kept on the instrument PC. 

Print outs may be kept in loose leaf notebooks for reference. If 

the sum of the area counts or any of the individual area counts 

falls outside the 95% confidence interval of the mean (+/- 1.96 

standard deviations from the mean), the operators will perform 

standard troubleshooting procedures to determine the cause. The 

entire calibration will then be repeated and new values entered 
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into the control chart. On a daily basis, the dilute calibration 

mix is injected into the instrument and the response noted. If 

the daily span checks indicate that any of the individual 

responses or the sum of the area counts fall outside the 95% 

confidence interval of the mean of the daily calibrations (+/-

1.96 standard deviations from the mean of the daily 

calibrations), a second injection is performed. If the second 

injection also falls outside the 95% confidence interval of the 

mean of the daily calibrations, standard troubleshooting 

procedures are performed to determine the cause and another 

injection is performed. A typical Control Chart is shown in 

Figure 3. System A and System B uses the latest fifty runs to 

determine the average used in the control chart and this average 

is updated daily. The control charts are visually inspected 

daily (on the PC) with the results stored on the PC associated 

with the data reduction for each unit. Selected typical results 

are output quarterly for inclusion in the quarterly reports for 

the projects covered. 

11.3.3 Calibration Quality Control 

Problems leading to a failure of the system to meet the 

quality assurance requirements shown in the above control charts 

roust be corrected before proceeding with the analysis. Large 

variations may be due to equipment failure. 

It is assumed that the response of the FID is linear with 

carbon number and class (i.e. r > 0.95). This assumption has 

been previously verified for several hydrocarbons. The intercept 

should not be significantly different for zero at the 0.05 

confidence level. A positive intercept may imply contamination. 

The slope of the calibration curve shall be within 5 percent of 

the previously determined value. 

11.3.3.1 Establishment of Initial Warning and Control Limits 

Initial Warning and Control limits are determined as 1.96 

and Three standard deviations of the previously determined 

averages. (Section 11.3.2) 

11.4 Standardization 

Information to be supplied at a later date. Both detailed 

hydrocarbon laboratories are undergoing modifications in order to 

standardize the GC and data processing systems. 

12.0 Analysis Procedures 

The analysis procedure is the same for each gas 

chromatograph but the preparation stages differ slightly. 
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12.1 Preparation stage steps: 

12.1.1.A Perkin Elmer Sigma 2000, System Al, Evaporative 

Emissions, C4 through Cll 

A. Adjustment of instrument gas flow rates (except carrier 

gas) which should be corrected or adjusted before hand. 

1. Set the detector air pressure to 140 KPa (20 psig). 

2. Set the detector hydrogen pressure to 140 kPa (20 

psig). 

B. Adjustment of Carrier Gas Flow Rate 

Verify that the carrier gas pressure is at the optimum 

pressure for the separation required. 

C. Set up detector 

Hold the detector igniter at the chimney of FID number 

2 and slowly increase the detector air pressure to 280 

kPa (40 psig). A popping sound should be heard, 

indicating the detector lit. This can be verified by 

holding a mirror or piece of glass up to the chimney 

and looking for condensation. 

D. Column and Valve Temperatures 

Detector • 275°C. 

Initial Oven Temperature = -100°C. 

There is an initial hold of 6.5 minutes. 

Oven Temperature Programming Rate 1 = 20°C/min. 

Oven Temperature 1 = -45°C. 

Hold for 4 minutes. 

Oven Temperature Programming Rate 2 = 2°C/min. 

Oven Temperature 2 = -15°C. 

Oven Temperature Programming Rate 4 = 6°C/min. 

Final Oven Temperature = 175°C. 
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Six Port Valve Temperature = 90°C. 

12.1.I.B Front End Analysis 

Isothermal at ambient temperature 

Analytical carrier flow 35 ml/min 

Backflush flow 35 ml/min 

Detector temperature 275 °AC. 

12.1.2.A System A2, Perkin Elmer 8700, C2 through Cll 

A. Adjustment of instrument gas flow rates (except carrier 

gas) which should be corrected or adjusted before hand. 

1. Set the detector air pressure to 20 psig. 

2. Set the detector hydrogen pressure to 20 psig. 

B. Adjustment of Carrier Gas Flow Rate 

Verify that the carrier gas pressure is at 80 psig at 

the helium cylinder. Adjust the carrier gas pressure 

regulator on the 8700 to the pressure indicated in the 

method and displayed on the screen. Refer to Section 

1.11.1 for fine tuning of the carrier gas flow rate. 

C. Set up detector 

Open the hydrogen toggle valve on the back of the 8700 

to allow the hydrogen to purge the lines. After 

approximately two minutes, close the hydrogen toggle 

valve and hold the FID igniter against the chimney of 

the FID. Open the hydrogen toggle valve and the 

igniter should glow brightly and a slight popping sound 

may be heard, indicating ignition. This can be 

verified by holding a mirror or piece of glass up to 

the chimney and looking for condensation. 

D. Column and Valve Temperature 

The oven temperature adjustment, R47, on the analog 

board was adjusted 10 - 11 turns CCW to obtain a 

temperature colder than that allowed by the 

methods software. The actual oven temperature is 

15°C colder than the screen indicates when the 

method is set to -80°C and 25°C cooler when the 
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method is set for 200°C. This adjustment allows 

the initial oven temperature to attain -95°C while 

the method is set for -80°C. The following 

temperature listing will be those set in the 

method and not the actual oven temperatures. The 

programming rates are unaffected. 

Detector = 275°C. 

Initial Oven Temperature = -80°C. 

Oven Temperature Programming Rate 1 •= 20°C/min. 

Oven Temperature l = -40°C. 

Oven Temperature Programming Rate 2 = 2°C/min. 

Oven Temperature 2 = -15°C. 

Oven Temperature Programming Rate 3 = 6°C/min. 

Oven Temperature 3 = i20°C. 

Oven Temperature Programming Rate 4 = 8°C/min. 

Final Oven Temperature = 220°C. 

Six Port Valve Temperature = 90°C. 

12.1.I.B Hewlett Packard 5880A. 

A. Adjustment of instrument gas flow rates (except carrier 

gas) which should be corrected or adjusted before hand. 

1. Set the detector air pressure to 275 KPa (40 psig). 

2. Set the detector hydrogen pressure to 275 kPa (40 

psig). 

B. Adjustment of Carrier Gas Flow Rate 

Verify that the carrier gas pressure is at the optimum 

pressure for the separation required. 

C. Set up detector 

Hold the A Channel detector igniter switch to manual. 

A popping sound should be heard, indicating the 

detector lit. This can be verified by holding a mirror 
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or piece of glass up to the chimney and looking for 

condensation. 

D. Column and Valve Temperatures 

Detector = 275°C. 

Initial Oven Temperature = -60°C. 

There is an initial hold of 9 minutes. 

Oven Temperature Programming Rate 1 = 20°C/min. 

Oven Temperature 1 = -25°C. 

Oven Temperature Programming Rate 2 = 3°C/min. 

Oven Temperature 2 = 25°C. 

Oven Temperature Programming Rate 4 = 8°C/min. 

Final Oven Temperature = 190°C. 

There is an final hold of 10 minutes. 

Six Port Valve Temperature = 90°C. 

12.2.A Analysis Stage Steps 

Filling the sample loop and injecting the sample are carried 

out as follows: 

Turn on the sample pump for one minute which insures that at 

least 10 sample volumes have flowed through the loop. After one 

minute of sample loop fill time, close valve V2 which picks up 

the 5-cc sample and diverts it to V3 for methane analysis. After 

methane elutes V2 is returned to open position and VI and V3 are 

closed which back flushes the molecular sieve porapak system and 

brings the Silica Gel column on line for the C2-C3 analysis. A 

second sample is pulled and injected following the same procedure 

used for methane. After acetylene elutes (15 minutes), VI, V2, 

and V3 are returned to their normally open positions which now 

backflushes the silica gel column. Note that propane and 

propylene are also analyzed during this analysis. The raw data is 

calculated and entered in the IBM PC/AT when editing. 

13.0 Calculations 

Using the calibration constant (k) determined in section 

11.3.2, calculate the concentration of each compound (peak) as 
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follows: 

Concentration, ppm C = (k)(Area) 

where the area is integrator counts. Most integrators may be 

programmed to perform this calculation and present the results 

directly in units of concentration. 

The appropriate formula to calculate the limits of 

prediction are given in section 11.3.3.1. 

14.0 Data Reporting 

The concentration of each hydrocarbon found should be 

reported to the computer section in the format proscribed. The 

integrator output and strip chart record for all samples, 

calibrations, and daily standards are identified uniquely and 

saved. Electronic storage is made of each of these runs for 

archiving and latter editing and transfer to the main computer 

group. Each sample is logged in a,sample log as run. The log book 

has the following format: 

Date, AME run number, File name, Remarks (description of 

run, instrument # on which it was run, dilution of liquid 

samples, total hydrocarbon concentration, and any other 

information pertinent to the current project.). 

The file name is 8 characters in length and uses the 

following convention: 

X 99999 X X 

Program ID AME RUN # Run Type 

A - Z 99999 A - Z 

CASE PROGRAM OF (1ST Letter) 

Sample Position 

A - Z 

•f 

•g 

•h 

"j 

' OR 

1

 OR 

• OR 

' OR 

• OR 

• OR 

• OR 

' OR 

A

1

: 

B ' : 

C : 

F

1

 : 

G': 

H«: 

J

1

: 

'0' : 

G_CPR0G 

G_CPR0G 

G_CPROG 

G_CPROG 

G_CPR0G 

G_CPR0G 

G_CPR0G 

G CPROG 

FFV 

CNG 

ALTFUEL 

SHEDRL 

FFV 

CNG 

ALTFUEL 

SHEDRL 

CASE CYCLE OF (2ND Letter) 
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•a' OR 'A': G_CCYC = FTP 

•b' OR 'B•: G_CCYC = HWFET 

•d• OR •D•: G_CCYC = NYCC 

•f• OR •F•: G_CCYC = CUE 

•h' OR 'H': G_CCYC = LIQFC 

IF G_CPROG = SHEDRL THEN 

•n' OR 'N«: G_CCYC = EVAP 

ELSE : G_CCYC = N/A 

•o' OR *0': G_CCYC » MFTP 

CASE BAGPOS OF (3RD Letter) 

'a' OR 'A': BAGPOS • BAG I, HWFET, NYCC, CUE, HOTSOAK START 

•b' OR 'B': BAGPOS = BAGII, HOTSOAK FINAL 

•c* OR 'C1: BAGPOS - BAGIII, DIURNAL START 

•d1 OR 'D': BAGPOS - BKG, DIURNAL FINAL 

NOTE: The details of the above table are modified and/or expanded 

to include new projects as they occur. 

This number, the date, and the AME run number are recorded with all 

electronically stored data for each chromatographic run to provide 

unique identification. The accuracy of data transfer is checked by the 

data processing section by checking the sum of the transmitted data 

values against the sum of these values which is calculated at the point 

of editing and transmitted at the end of the data file. If there is a 

discrepancy the cause is ascertained and the file resubmitted, there are 

several other checks that are preformed prior to data entry into 

"Archived Mobile Source Emissions" (AME) such as reasonableness of the 

run number, individual compounds numbers, etc. Again if a discrepancy at 

any point is seen it is corrected. 

15.0 Corrective Action 

Corrective action will be taken whenever abnormalities are observed 

or daily checks fall outside control points. Specific checks include: 

Control charts 

response factors 

Relative retention times 

Variation seen in editing process of reference peaks 

Physical malfunctions 

The nature and type of corrective action required in any situation 

is determined and documented by the operator. This requires 
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chromatographic experience and is part of the basic qualifications 

required. 

16.0 Method Precision 

Precision of repetitive analysis of daily standards of the methods 

are being updated. They will be included when completed. Typical RSD of 

the calibration mix is less than six percent. 

Precision is maintained and demonstrated in the control charts. 

Precision of other measured compounds should be similar to that of 

compounds which are close in retention time. This statement applies only 

to hydrocarbons. Oxygenated materials behave differently and can effect 

the precision of those compounds near by and will have a separate but 

undetermined precision of their own. 

18.0 Quality Control 

This section specifies the regular QC program and discusses 

responsibilities for evaluation of the QC data. Calibration QC was 

discussed in section 11.3. These procedures require real-time review of 

analytical performance by the analyst, and QC review directly after 

input into the main data base. 

18.1 QC Checks and Frequency 

* On a quarterly basis the calibration mix is analyzed consecutively 

six times. For these six analyses the mean and standard deviation of 

the area counts are calculated for each of the compounds. The average 

areas are then summed, the summations then form the basis for the 

instrument response factors (k). The response factors are updated for 

any trends that appear in instrument response or if the instrument 

reaches an out of control state. 

A dilute calibration mix is ran daily to assure instrument 

stability. Corrective action is taken if unacceptable trends are noted 

or if the instrument reaches an out of control state. Daily checks are 

compared to the control chart to ensure that the instrument is operating 

with in the control limits on any given day. If the daily span check is 

out of control then a second span check is preformed. Corrective action 

is taken if the second check is also out of control. The first out of 

control check will be treated as an anomaly if the second check is 

within the control limits. 

On a quarterly basis samples are exchanged between instrument 

systems. These are to be either "real" samples collected during an 

ongoing program or "simulated" samples prepared by the vaporization of a 

full range gasoline. Samples may be prepared by either or both groups 

and then run on all systems. Results from each analysis will be co-pared 

on a compound by compound basis as well as by carbon number and class 

totals and overall total. This comparison is examined by the QC 
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coordinator or his designee to assure that the instruments being used 

agree on the compound identification and quantification. Limits are 

currently being investigated. 

18.1.3 Control Charts 

See also Section 11.3.2 

Calibration control charts will be maintained on the response 

factors observed when running the daily calibration mix. At least fifty 

runs will be used as the data background to provide averages and 

variance statistics. If, due to system changes fifty points are not 

available the largest number possible will be used. These average and 

variance statistics are to be updated as previously described. When 

values are found in the warning area (greater than +/- 2 sigma) the 

project officer and the QC officer will be notified. If the exceedance 

continues or if the value exceeds the action limit (3 sigma) immediate 

steps to ascertain the cause will be instituted. Appropriate corrective 

action for the situation will be determined by the analyst in 

cooperation with the QC Officer and the project Officer. All exceedances 

and corrective actions will be recorded in the appropriate laboratory 

notebook. The control chart will be distributed quarterly as part of the 

normal reporting procedure. Copies will be given to the QC officer as 

well as included in the quarterly report to the project officer. Trends 

will also be monitored and reported when significant. 

It is recognized that major instrument repair may cause a step 

change in average values. If such a change occurs and the 

instrumentation is otherwise operating properly the change will be 

accommodated. It will be assumed that the previous statistics are still 

sound although the mean has been displaced. This accommodation will 

continue until either fifty days calibrations have been completed at 

which point the new data statistic will replace the previously used 

ones. If at any time, the new statistics significantly exceed the old an 

explanation will be immediately be sought and appropriate corrective 

action agreed upon in conjunction with the QC Officer. 

18.2 Performance Evaluations 

Participation in performance evaluation studies is recommended and 

encouraged for this method. The samples used for these audits should be 

within the normal concentration range and be of the same species type as 

normally seen. The true values of these audits should remain unknown to 

the analyst until after the study is complete to prevent operator bias. 

All such studies shall be reported to the QC officer as well as the 

appropriate project officer and in the quarterly reports. 

18.3 Systems Audits 

This section contains the recommended procedure for performing a 
P.21 

AREAL-CPCD-MSERB RPM-001 

Revision No. 3 

Date: June 28, 1991, Page: 20 

system audit for this method. The need and scheduling of systems audits 

will be determined by the project officer in conjunction with the qc 

officer. The basic scope of the system audit will be: 

1. To verify the adherence to this research 

protocol/method; and 

2. To verify the data flow and archiving process used for 

the computerized data base. 

Organizations performing systems audits should review the following 

and the audit questionnaire (Appendix A). It is recommended that the 

independent audit plan be compared to this document and differences 

noted. In all cases, methods for assessing the data quality for this 

method must be approved by the organization being audited prior to the 

initiation of the audit. 

18.3.1 Audit Plan 

1. Meet with organizational personnel, identify key personnel, 

identify the purpose of the audit, and review the audit plan and 

questionnaire. 

2. Collect all QC documentation (i.e., QC Charts,forms, 

notebooks,etc. ) and data base print outs. 

3. Perform audit of sample analysis. 

4. Perform audit of sample data processing activities. 

5. Perform audit of data validation. 

6. Preform audit of data base. 

7. Complete audit questionnaire. 

8. Hold audit review meeting and critique audit findings. 

Make corrections to audit findings or questionnaire if 

required. 

It is suggested that data quality might be assigned one of three 

levels according to the following guidelines: 

1. Unknown Quality - a vital piece of QC data is missing or 

can not be verified. 

2. Questionable Quality - generally all data and documents 

are in good order, but a secondary item needed to completely 

characterize the data is missing, e.g., a control chart to 

demonstrate that the method was in control over a given time 
P.22 

AREAL-CPCD-MSERB RPM-001 

Revision No. 3 

Date: June 28, 1991, Page: 21 

interval. 

3. Known Quality - all documentation is in order, with 

data traceable from the final report to the date and time of the 

analysis. 

18.3.2 Documents 

The following documents will be reviewed at the time of the audit: 

1. Laboratory notebooks or forms used with the method. 

2. QC charts 

3. All Instrumental calibration documentation 

4. Instruction manuals and related SOP's or RPM's. 

5. Documents related to quality of the materials used. 

6. All documentation for GC computer, data validation, 

data transfer, and data archiving and reporting. 
P.23 

AREAL-CPCD-MSERB RPM-001 

Revision No. 3 

Date: June 28, 1991, Page: 22 

APPENDIX A 

DETAILED HYDROCARBONS 

BY 

GAS CHROMATOGRAPHY 

AUDIT QUESTIONNAIRE 
P.24 

AREAL-CPCD-MSERB RPM-001 

Revision No. 3 

Date: June 28, 1991, Page: 23 

1) Does the technician have a current copy of the 

RPM available at or near his station 

2) Are all reference compounds of maximum purity 

available, ACS Reagent grade or similar 

3) Are calibration results within; 

a) 5 % of the mean 

b) r2 >/= 0.95 

4) Have any outlying standards been rejected 

If so has the rejection been satisfactorily 

explained, documented and reviewed 

5) Has the calibration mix been run for precision 

at the beginning of each week in which testing 

occurred 

6) Were these runs for precision properly included 

in the instrument data base 

7) Have the statistical control charts been updated 

at the prescribed intervals 

8) Have the daily standards been run each day that 

testing occurred 

9) Have problems apparent from daily standards 

been resolved before testing commenced 

10) Have all appropriate statistics been kept current_ 

11) Have all trends been noted and reported 

12) Has appropriate action been taken to resolve 

problems noted from trends and statistics 

13) Have control charts been reported at specified 

intervals to project officer and to QA Officer 

14) Have exchange samples been run in timely fashion 

15) Have results from exchange samples been reported, 

YES NO 
P.25 

AREAL-CPCD-MSERB RPM-001 

Revision No. 3 

Date: June 28, 1991, Page: 24 

recorded in notebooks properly 

16) Have all problems uncovered by exchange samples 

or audit samples been adequately resolved, 

explained, corrected and reported to all concerned_ 

17) Have NIST (NBS) samples been run at appropriate 

intervals 

18) Are all results from these samples properly 

recorded and within specifications 

19) Is preventative maintenance preformed as scheduled_ 

20) Are files in the PC properly maintained 

21) Are laboratory and instrument notebooks properly 

maintained and all necessary.information recorded 

22) Are corrective actions taken when needed and 

properly recorded and reported 

23) Are data transfers properly recorded and checked 

24) Are QC reports filed in a timely manner 

25) Have any of the following audits been preformed 

on the laboratory 

a) System Audit 

b) Performance audit 
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P.28 

National Specialty $ases 

630 UNITED DRIVE 

DURHAM , NC27713 

(919)544-3772 

TOi National Wei den 

Raleigh, N.C. 

DATE REPORTEDi 3-27-90 

REFERENCEl 88 7887 

••* & 

MATERIAL SUBMITTEDi Cyl#CC&3746 Certified +/- 57. 

INFORMATION REQUESTEDi Ratio analysis 

METHOD OF ANALYSIS! Gas chromatograph 

RESULT OF INVESTIGATION! Traceable Certificate number 13230 

Traceable to NBS through NBS report number 731/242697 

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Nitrogen 

AUTHORIZED SIGNATURE! 

"THIS REPORT STATES ACCURATELY THE RESULTS OF THE 

INVESTIGATION MADE UPON THE' MATERIALS SUBMITTED TO THE 

ANALYTICAL LABORATORY. EVERY EFFORT HAS BEEN MADE TO 

DETERMINE OBJECTIVELY, THE INFORMATION REQUESTEDi HOWEVER, 

IN CONNECTION WITH ITS RENDERING OF THIS REPORT, NATIONAL 

SPECIALTY GASES SHALL HAVE NO LIABILITY IN EXCESS OF ITS 

ESTABLISHED CHARGE FOR THE SERVICE. ANY USE OF THIS REPORT 

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NAME 

METHANE 

ETHYLENE 

ETHANE 

ACETYLENE 

PROPANE 

PROPYLENE 

PROPAOIENE 

METHYLACETYLENE 

ISO-BUTANE 

• • • UNKNOWN •• • 

1-BUTENE 

ISO-BUTYLENE 

1,3-BUTADlENE 

N-BUTANE 

• * • UNKNOWN •* * 

TRANS-2-6UTENE 

1-BUTEN-3-YN 

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CIS-2-BUTEKE 

C4H4 

1 ,3 BUTAOYNE 

3-HtTHYL-1-BLITcNc 

ISO-PENTANE 

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C5K8 

CSH6 

2-HETHYL-1-BUTENE 

N-PENTANE 

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2.286 

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2.000 

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1.333 

1.333 

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1.714 

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••• UNKNOWN •*• 

••• UNKNOWN ••• 

HTBE 

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3-METHYLPENTANE 

2-METHYL-1-PENTENE 

1-HEXENE 

••• UNKNOWN ••• 

••• UNKNOWN ••• 

N-HEXANE 

C6H12 

C6H12 

3METHYL C1S-2-PENTENE 

2METHU-2PEMTENE 

3 OR 4 METHYL CYCLOPENTENE 

CIS OR TRANS 20R 3 HEXENE 

C6H10 

C7H16 

3 METHYL-TRANS-2 PENTENE 

METHYLCYCLOPENTANE 

METHYL-C1S-2-PENTENE 

METHYL-TRANS-2-PENTENE 

2,4-OIHETHYLPENTANE 

2,2,3 TRIHETHYL6UTANE 

C6H8 

••• UNKNOWN ••• 

C7H12 

C6H10 

BENZENE 

C7H14 

3,3 DIMETHYLPENTANE 

C7H14 

CYCLOHEXANE 

C7H14 

C7H14 

C7H14. 

C6H10 

4 METHYL TRANS-2-HEXENE 

2-METHYLHEXANE 

2,3-DIMETHYLPENTANE 

1,1 D1METHYLCYCL0PENTANE 

CYCLOHEXENE 

3-METHYLHEXANE 

C7H14 

1C1S 3DIMETMYLCYCLG?EhTENc 

TRANS-1,331METHYLCYCLCPEN1ENE 

URANS-2,DIMETHYLCYC:.C?EN7EsE 

C7H14 

ISO-OCTANE 

2 METHYL-2 HEXENE 

VETHYLCYCLC.-.EXENE 

N'-HEPTAKE 

3 METHYL CIS-2 HEXENE 

C7H14 

TRANS-2-r.EPTENE 

3 ETHYL-CIS 2 PENTENE 

C7H14 

2.3 CIHEIKYL-2-PENTEN E 

07nl2 

07H14 

2,2.4 TRi-ETHYL-1-PENiENE 

03nl4 

1 ; 

C1-.12 

Ci-12 

CSnltO 

Ci-143 

Ci-12 

Cii12 

C6H12 

Ci-112 

Ci.iU 

Ci«2., 

C6K12 

C6H12 

C6H12 

C6H10 

C6H12 

CtvilO 

C7H16 

C6H12 

Ci.<12 

C6H12 

Cii12 

C7H16 

C7*16 

Cip3 

CiHS 

C7H12 

CinlO 

Cip6 

C7p!4 

C7h16 

C7H14 

06H12 

Z7-. 14 

07v 14 

07*14 

Ci-10 

07rl4 

C7ril6 

07-116 

07-.14 

*" L . • *1 

0 7.-16 

•0 7-14, 

0 . .i 14 

0 7-14 

07-14 

""-14 

- ' . • o 

0 7-1-

0 " -'. 2 

:"- t 

: " - • -

:*-' -

-" - * -

'.'-'-

""-'- > 

'"•-' " 

: " - • -

'.±-'. 
P.32 

**"* * ' * 

\ 

Table 1 

116 

117 

113 

119 

120 

121 

122 

123 

124 

125 

126 

127 

128 

129 

130 

131 

132 

133 

134 

135 

136 

137 

123 

13? 

140 

141 

142 

143 

144 

145 

146 

147 

143 

149 

153 

1

c 1 

152 

153 

* C • 

*> C C 

1J4 

•"","*' 

155 

159 

'60 

161 

1C2 

1:3 

^i*. 

165 

.... 

'67 

* / o 

. Z * 

• ~ -

1 71 

* - ^ 

• ~3 

- -

• 7-

•"i 

110.2 

93 

114.232 

114.232 

112 

114.232 

114.232 

112.216 

114.232 

114.232 

92.141 

112.216 

114.232 

114.232 

96.161 

114.232 

114.232 

112.216 

112.216 

128.259 

112.216 

112.216 

112.216 

112.216 

112.216 

123 

112.216 

112.216 

112.216 

112.216 

112.216 

112.216 

114.232 

114.232 

112.216 

112.216 

112.216 

112.216 

112.216 

112.216 

112.216 

1*3 

123.23? 

123.259 

123.25? 

112.216 

123.25? 

112.216 

110.2 

123.259 

122.25? 

123.259 

.*A *(3 

126.243 

126.2-3 

106.163 

106.163 

123.23? 

• _ Z . .4 - "* 

•23.23? 

'22...'..? 

•23.23? 

8 

7 

8 

8 

8 

8 

8 

8 

8 

8 

7 

8 

8 

8 

7 

8 

8 

8 

8 

9 

8 

8 

8 

8 

8 

9 

8 

8 

8 

8 

8 

8 

8 

8 

8 

8 

8 

8 

8 

8 

8 

Q 

9 

9 

9 

8 

9 

8 

8 

9 

9 

9 

2 

v 

r 

s 

3 

9 

. 

9 

9 

23 2 

14 1 

13 1 

13 1 

14 1 

13 1 

0 5 

23 2 

13 1 

13 1 

31 3 

21 2 

13 1 

13 1 

23 2 

13 1 

13 1 

13 1 

14 1 

13 1 

14 1 

14 1 

14 1 

14 1 

14 1 

13 1 

14 1 

14 1 

14 1 

14 1 

14 

14 

13 

0 ! 

14 

21 ; 

0 ' 

22 ; 

14 

14 

0 

23 

13 

0 

13 

21 

13 

21 

23 

13 

13 

0 

31 

14 

14 

32 

32 

13 

' J .-i 

'. 3 

• 7 

14 

14 

18 

13 

16 

18 

14 

16 

18 

18 

8 

16 

18 

18 

12 

18 

18 

18 

16 

20 

16 

16 

16 

16 

16 

20 

16 

16 

16 

16 

16 

16 

18 

> 18 

16 

2 16 

i 16 

2 16 

1 18 

1 ' 16 

5 16 

2 14 

1 20 

5 20 

1 20 

2 16 

1 20 

2 16 

2 14 

1 20 

1 23 

5 20 

3 10 

IS 

1 13 

7 «n 

.. i J 

- j 

:. - 1 

'. 

16.2164 

16.4513 

14.4212. 

16.E093 

16.4313 

16.£398 

16.£398 

16.5131 

16.8098 

16.8098 

15.4960 

16.5131 

16.8098 

16.8098 

19.2112 

16.8098 

16.8098 

16.8098 

16.5131 

16.7768 

16.5131 

16.5131 

16.5131 

16.5131 

16.5131 

16.7429 

16.5131 

16.5131 

16.5131 

16.5131 

16.5131 

16.5131 

16.8398 

16.8398 

16.5131 

16.5131 

16.5131 

16.5131 

16.5131 

16.5131 

16.5131 

16.1870 

16.7768 

16.7763 

16.7763 

16.5131 

16.7763 

Is.5131 

16.2164 

16.7765 

16.7-63 

16.7713 

•C i-T. 

16.3131 

* *. C " 7 • 

15.J.231 

I5.i231 

Ii. 77 ; 3 

- . ;.- ' .. ~- . 3 

"-.. 7~.S 

1.750 

2.000 

2.2S0 

2.250 

2.030 

2.250 

1.750 

2.000 

2.250 

2.250 

1.143 

2.000 

2.250 

2.250 

1.714 

2.250 

2.250 

2.250 

2.000 

• 2.222 

2.000 

2.000 

2. COO 

2. COO 

2.000 

2.222 

2.COO 

2.000 

2.000 

2.000 

2.000 

2.000 

2.250 

2.250 

2.000 

2.C30 

2.COO 

2. COO 

2.250 

2.COO 

2.000 

1.750 

2.222 

2.222 

2.222 

2.000 

2.222 

2.003 

1.750 

2.222 

2.222 

2.222 

1.233 

2.003 

-» - - i 

1.253 

1.223 

2 ""^ 

-.*-.. 

- ---> 

- - 1 

-. 

CSH14 

ETHYLCYCLCPENTANE 

2,5 DIMETHYL HEXANE 

2,4 DIMETHYL HEXANE 

TR1HETHYL CYCLOPENTANE 

3,3 DIMETHYL HEXANE 

••• UNKNOWN ••• 

TR1HETHYLCYCL0PENTENE 

2,3,4-TRIMETHYLPENTANE 

2,3,3-TRIMETHYLPENTANE 

TOLUENE 

METHYL HEPTENE 

2,3 OIMETHYLHEXANE 

C8H18 

METHYLCTCLOHEXENE 

2-METHYLHEPTANE 

4-METHYLHEPTANE 

3,4 OIMETHYLHEXANE 

C8H16 

3 METHYL HEPTANE 

C£H16 

CSH16 

CSH16 

CSH16 

CSH16 

2,2,5 TRIMETHYLHEXANE 

CSH16 

C3K16 

C8H16 

C8H16 

CEH16 

C8H16 

N-OCTANE 

* " UNKNOWN ••" 

CSH16 

2-CCTENE 

••• UNKNOWN • " 

CSH16 

CSH16 

CSH16 

••• UNKN3WN «*• 

CSH14 

2,3 CR 2,3,5 TRIMETHYLhtXANc 

•** UNKNC.N •** 

C9H20 

CSH16 

C9H20 

03H16 

CSH14 

09H20 

09H20 

•THYLeENO'Ni 

"SIH.ETHUCY::. OHEXANE 

01*13 

u -mENE 

"•-XUENE 

0?H23 

.-9n20 

•** 'JNKNO.N •** 

:;H2 3 

0 9I? 3 

C3-H4 

C7H14 

CSnIS 

CSrflS 

C£rU6 

CS.TIS 

C3H14 

C3H16 

C3.-.1S 

C3-I13 

CT**:-

C£H16 

C8H18 

C8H18 

C7H12 

CEH1S 

C£H18 

C£n16 

CSH16 

C9n20 

C3H16 

C3.H16 

C£.-:16 

C3H16 

CSN16 

C9H20 

CSi-16 

C3-:i6 

CSH1S 

CS.-16 

C3.-1S 

CS-il6 

CS-13 

c

e - " Q 

C3-1S 

C3-1S 

~c^. * 

CS-i16 

C3-16 

C£n16 

C

:£-.1i 

0 c -1 -

C9.-23 

C9-20 

09-20 

02-i i 

09-20 

02-'s 

^

 C - ' -

Z

z

-ll 

Z~' 11 

Z - * 11 

11-' -' 

t ' - ' -

-

: -' z 

li ~' 1 

*; - ' J 

1 * - .* -

-•"•.. 

1 '• 11 
-

Table 1 

173 

17? 

183 

181 

182 

163 

164 

1E5 

166 

1£7 

163 

189 

190 

.V • - - - 191 

-sl-r'-W v..- ' - — 192 

193 

194 

195 

196 

197 

193 

199 

203 

201 

202 

203 

204 

205 

206 

227 

203 

20? 

• . 210 

211 

212 

213 

214 

215 

215 

217 

213 

21? 

223 

221 

222 

223 

224 

225 

226 

227 

223 

229 

230 

231 

232 

233 

234 

111 

237 

*** o 

- • 

126.243 

106.166 

126.243 

126.243 

142.236 

126.243 

126.243 

126.243 

126.243 

128.259 

126.243 

126.243 

126.243 

126.243 

126.243 

120.195 

142.286 

142.286 

142.2S6 

142.266 

142.236 

142.286 

140 

142.236 

142.236 

142.236 

123.195 

140.250 

120.195 

120.195 

142.266 

120.195 

142.266 

142.236 

142.266 

120.195 

142.236 

142.266 

142.236 

142.236 

120.195 

142.236 

142.236 

142.286 

142.266 

134.222 

156.313 

123.195 

134.222 

134.222 

156.313 

116.16 

156.313 

156.313 

156.313 

156.313 

134.222 

156.313 

134.222 

134.222 

134.222 

13,.222 

9 

8 

9 

9 

10 

9 

9 

9 

9 

9 

9 

9 

9 

9 

9 

9 

10 

10 

10 

10 

10 

10 

10 

10 

10 

10 

9 

10 

9 

9 

10 

9 

10 

10 

10 

9 

10 

10 

10 

10 

9 

10 

10 

10 

10 

10 

11 

9 

10 

10 

11 

9 

11 

11 

11 

11 

10 

11 

10 

10 

10 

10 

13 

32 

14 

14 

13 

14 

14 

14 

14 

11 

21 

21 

21 

21 

21 

31 

13 

13 

13 

13 

13 

13 

13 

13 

13 

13 

31 

14 

32 

32 

13 

32 

13 

13 

13 

32 

13 

13 

13 

13 

32 

13 

13 

13 

11 

31 

13 

32 

32 

32 

13 

36 

13 

13 

13 

13 

32 

13 

32 

32 

32 

32 

1 

3 

2 

2 

2 

2 

2 

3 

1 

1 

1 

1 

1 

1 

1 

1 

1 

1 

3 

1 

3 

3 

1 

3 

1 

1 

1 

3 

1 

1 

1 

1 

3 

1 

1 

1 

1 

3 

1 

3 

3 

3 

1 

3 

1 

1 

1 

1 

3 

1 

3 

3 

3 

3 

18 

10 

18 

18 

22 

18 

18 

18 

18 

20 

18 

18 

18 

18 

18 

12 

22 

22 

22 

22 

22 

22 

20 

22 

22 

22 

12 

20 

12 

12 

22 

12 

22 

22 

22 

12 

22 

22 

22 

22 

12 

22 

22 

22 

22 

14 

24 

12 

14 

14 

24 

8 

24 

24 

24 

14 

24 

14 

14 

14 

16.5131 

15.6231 

16.5151.. 

16.7763 

16.7504 

18.6116 

16.5131 

16.5131 

16.5131 

16.7768 

16.5131 

16.5131 

16.5131 

16.5131 

16.5131 

15.7220 

16.7504 

16.7504 

16.7504 

16.7504 

16.7504 

16.7504 

16.4813 

16.7504 

16.7504 

16.7504 

15.7220 

14.1498 

15.7220 

15.7220 

16.7504 

15.7220 

16.7504 

16.7504 

16.7504 

14.1498 

16.7504 

16.7504 

16.7504 

16.7504 

15.7220 

16.7504 

16.7504 

16.7504 

16.7504 

15.8011 

16.7239 

15.7220 

15.£011 

15.£311 

16.7239 

15.1942 

16.723? 

16.723? 

16.722? 

16.7239 

15.£311 

16.723? 

15.3311 

15.3011 

15.3011 

15.3011 

2. COO 

1.250 

2.000 

2.000 

2.200 

2.000 

2.000 

2.000 

2.000 

2.222 

2.000 

2.000 

2.000 

2.000 

2.000 

1.333 

2.200 

2.200 

2.200 

2.200 

2.200 

2.200 

2.000 

2.200 

2.200 

, 2.200 

1.333 

2.000 

1.333 

1.333 

2.200 

1.333 

2.200 

2.200 

2.200 

1.333 

2.200 

2.200 

2.200 

2.200 

1.333 

2.200 

2.200 

2.200 

2.200 

1.400 

2.182 

1.333 

1.400 

1.400 

2.132 

0.ES9 

2.132 

2.132 

2.1E2 

2.182 

1.400 

2.182 

1.430 

1.400 

1.400 

1.430 

•* 

C9H20 

O-XYLENE 

C9H18 

C9H18 

C10H22 

C9H18 

C9H18 7 

C9H18 ? 

C9H18 7 

N-NONANE 

C9H18 7 

C9H18 7 

C9H18 

C9H18 

C9H18 

ISOPROPYLBENZENE 

C10H22 7 

C10H22 7 

C10H22 ? 

C10H22 7 

C10H22 7 

C10H22 ? 

C10H20 

C10H22 7 

C10H22 7 

C10H22 7 

N-PROPYLBENZENE 

C10H20 

1METHYL-3ETHYLBENZENE 

1METHYL-4ETHYLBENZENE 

C10H22 

1,3,5 TRIMETHYLBENZENE 

C10H22 

C10H22 

C1CH22 

1-MET-2-ETHYLSENZENE 

C10H22 

C10H22 

C10H22 

C13H22 

1,2,4 TRIMETHYLBENZENE 

C1CH22 

C10H22 

C10H22 

N-DECANE 

SEC-6UTYLBENZENE 

C11H24 

1,2,3 TRIMETHYLBENZENE 

C10H14 

C10H14 

C11H24 

1N0ENE 

C11H24 

C11H24 

C11H24 ? 

C11H24 

C10H14 

011H24 » C10H14 

C10H14 

C10HU 

C1CH14 » C11H24 

CICN K 

C9W20 

C8H10 

C9rt1S 

C9H13 

C1CH22 

C9«18 

C9H18 

C9H18 

C9H18 

C9n20 

C9«fte-> 

C9H18 

C9H18 

C9H18 

C9H18 

C9H12 

C10H22 

C10H22 

C10H22 

C10H22 

C10H22 

C1CH22 

C10K20 

C10H22 

C1C.H22 

C10H22 

C9H12 

C10K20 

C9H12 

C9H12 

C1CK22 

C9H12 

C1Ch22 

C1CH22 

C10h22 

C9H12 

C1Ch22 

C1C-i22 

C13H22 

C10H22 

C9H12 

CIO.22 

C10n22 

C1CH22 

C10H22 

C10H14 

C11r24 

C9H12 

C10h14 

ClOnl . 

cr.nt . 

C9-3 

C 1 '; f 2 -

CH-2 -

CllnOClli" -

C10-1-. 

0H-3 -

: i o 11 -

01^-1 -

- 1 r -1 -

C 10 - 1 . 

' 

P.33 
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UUiMtNiAUIUiUiinuiuiui ^ 

j^oJ^teoooooooroJ ^ 

OOCTOOOOOOOOOOO O 

OJ #' *• |-W-*-»-*WW\fl l 

rj (n O) Cn fvj S S S 

• CJ • • • • CJ OOO ' 

r o * -» ro ro ro • w N M w M M M ro M M w • • • rviNUiNrviWWUUuuuiMriurviMuui J 

rooJ*Nij;j-j-o*J-#-*^J-Jro<jf~4-j^rjWoJiw^ro^ro*>^ ^ — ^ — -^^oro^roro---«- » 

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or\jr\jr\ioo-»o**-»-*-«-*-*-*-*>oo-*oo->-»- * 

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oocjr>ooooooooooooorot-JUJoror\juiro/rororor\jrot>^r\iroc>L*J M 

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»N|Onm(DN()lp>{0(D(Bn^CoapinNSN(Br9NCI||tNNNSNNS^(DSn>(D^N) S I-^co6^c>tV^5 ;

c>c>c>c>ot>r>c>c>t>- ^ — 4)n«uiv^inovAvninutui^u^^uiMOOO^^oi^ui(>noitaOBnCDU^D]^^iDD)O i 

..j r_ t > e , t . O O *.0«.JOOOOOOOOOOO-»r\J O — -* -»r\J-*- - -*- * ^-^^--^NfvJN^^rO-***WMrvlr\lrVrN'N- ' -* rvj -* -• N W W 

rxj-ftODr^i^J^^J^i^J^J^^f^roJ^J-^j^rj-*-

S^ouiuiui&uiuiinuiuioovflvn^oc^^^ooiDOMttntttaocooooaoo u USOUUlNflN^^VlvflVOOUf^MOSSSOOMOUNN^Nrv'NNOOrgOONN N 

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ar r -r r T *: T T X r. -r. T. ac a: J-: Z Z zzzz^c^x*c(^(^C^O>(^(^(^(^^^JOC^C^NC^(^(^^^ffl^O>^^^^^^^M^^^^^^ ^ 

/*J» . r. J». n * *•• n *. ^^K^^^HUKW^ A » x O 7i:ri:i:i:7:i:7:7:r**rzj:7 . zzzz z r- ic •>* -** -*i •*» >-* * -a-si-o-oj-a-j*- ^ 

9 V. zrz£Krx3 ? J? ? £ .* *.!i t ar?. " a: ?. 9 9. 8 8 8x a 2c 2 ac ? x g 9. 2 ni g -

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ooo^oooo-o o i**rot>oc>rvit>oo* >' « ^ 4-~J>'C>4>'4>J>'J>'4'-** - 4- ro 4s* *~ **• ** «~ «- **-

CA> 
Table 1 

P.35 

332 

303 

334 

305 

306 

337 

303 

309 

310 

311 

312 

313 

314 

315 

316 

317 

313 

319 

323 

321 

322 

323 

324 

325 

326 

327 

"! ".9 

142 

142 

142 

32. 

46. 

0 1 

0 1 

.19 1 

.19 1 

.19 1 

164 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

0 1 

C 1 

0425 

C696 

1 0 5 

1 0 5 

0 33 3 

0 0 5 

0 33 3 

3 11 1 

3 0 5 

3 0 ! 

3 0 '. 

3 0 ! 

3 0 ! 

3 0 ! 

3 0 ! 

3 0 ! 

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3 0 

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1 1 

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0 

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I 10 

0 

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28 

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S 0 

5 0 

i 0 

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5 4 

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16. 

0 

16. 

16. 

0 

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37 

27 

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6624 

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METHYL NAPHTHALENE 

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