CONFIDENTIAL/PROPRIETARY

KAYSER TECHNOLOGY, INC.

SUPPLEMENTAL INSTRUCTIONS
FOR THE AGILENT 3000 RGA

I. DOCUMENTATION

II. SYSTEM HIGHLIGHTS

III. CALIBRATION

IV. METHOD DEVELOPMENT FOR ACTUAL GASES

V. OPERATION OF GC WITH ACE UNIT

VI. COMMENTS ON ACE AND GC SIGNALS

VII. STARTUP AND SHUTDOWN BASICS

 KAYSER TECHNOLOGY, INC.

SUPPLEMENTAL INSTRUCTIONS
FOR THE AGILENT 3000 RGA

I. DOCUMENTATION

The following are provided by Agilent Technologies:

1. Agilent 3000 Micro Gas Chromatograph - User Information CD

Contains the "User Information" manual as a PDF file. A copy of the PDF file is
on the computer as C:\KTI AGILENT 3000\G2801-90118e.pdf.

2. Agilent Cerity Networked Data System for Chemical QA/QC CD (A.04.07

Build 7400, JULY 2006)
KTI installed the Cerity software to C:\Program Files\Agilent\Cerity QA-QC. The
software provides information to the user through extensive use of "help" pop-up
menus.

3. Installing the Gas-Liquid Separator and Pressure Reducer

SPECIAL NOTE: Software icons pinned to the PC START MENU are Cerity, DBMaint,
and ConnectAdmin. These programs, complimented by Internet Explorer and Excel, are
the software tools needed to operate the Agilent 3000 RGA.

II. SYSTEM HIGHLIGHTS

1. Gas Supply

Refer to Installation section of the User Information manual (pages 13-17)

Argon with purity of at least 99.999% and 80 psig (550 kPag) for Column A.
Helium with purity of at least 99.999% and 80 psig (550 kPag) for Column B, C, and D.
KTI added 2 Micron filters to the gas supply inlets.

Always supply the GC with gas before applying POWER to the unit. Use the
following procedure:

1. Connect the gases noted above.

2. Crack open the fittings between the 2 Micron Filters and the GC on the Argon
and Helium gas supply lines.
3. Open the Argon supply and purge the line. Tighten the fitting between the filter
and the GC.
4. Open the Helium supply and purge the line. Tighten the fitting between the filter
and the GC.

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2. Hard Electrical Connections

Refer to Installation section of the User Information manual (pages 13-18)

Power to the GC is through power converter that provides 24VDC to the GC. Connect
this power cord at the rear of the GC.

For stand-alone operations, the PC and GC communicate through a LAN "crossover

ethertwist cable". Both 3-meter and 6-meter cables are provided. Connect one of these
cables.

Connect a remote cable from the ACE interface box to the remote connection at the rear
of the GC.

Turn on the GC. The instrument will beep once at power on, then beep twice after it has
successfully passed its internal tests.

3. Special Software Setup Parameters

For stand-alone operations, the IP address of the PC has been set as TCP/IP at IP
Address 10.1.1.100. The GC is set as 10.1.1.101. The Subnet Mask for both
components is 255.255.255.0.

For Windows XP see p. 19 for instructions on the above.

4. PC to GC Communication

1. Click on Internet Explorer. The default home page is set to http://10.1.1.101/.

This connects you directly to the 3000 Micro GC page.

KTI has preset the Gas Type according to the configuration needed for the GC
(Argon as Carrier to Module A and Helium to the remaining Modules). This is
done from the web-page for the GC. The password for changing the Gas Type is
gasconfig.

Under Utilities, you can obtain the complete hardware description of the GC
under Configuration: Full System. A printout of this information is attached to this
manual.

5. Enable Cerity NDS Communication to the GC through ConnectAdmin

The Agilent 3000 RGA has been added to the instrument list through the Add button
under ConnectAdmin program. The instrument is named as "ACE RGA" and is

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connected (enabled) and disconnected by ConnectAdmin. Cerity NDS can control

the instrument when it is connected.

6. Initial Use of Cerity NDS and the GC

Open Cerity NDS from the Desktop. Immediately go to Instrument/Status to view the
current state of the GC.

If the unit was shutdown properly (described later), then each column should be at
30C with 0.0 kPa (psig) column head pressures and the detectors should be OFF.

KTI has installed methods to operate the GC. Methods are sent to the GC from
Instrument\Status\Download. For a normal Startup of the GC follow the procedure
below.

1. Download the method named SHUTDOWN2 (wait one minute), download

SHUTDOWN1 (wait a minute), download SHUTDOWN0 (and wait at least 15
minutes if gases were recently connected in order to purge air from the columns).

Download the method named COOLDOWN to place 206.9 kPa (30.0 psig) column
head pressure on the four modules, activate temperatures and turn the detectors
ON. This will flow carrier through the columns. The expected flow rates from the
Analytical and Reference ports at the rear of the GC should be 1.0 ml/min and 0.6
ml/min, respectively. These flows should be checked according to page 106 of the
User Information manual.

2. If the unit has been shutdown for a significant period of time, download the method
named BAKEOUT which will purge the columns at operating maximum temperatures
with the detectors ON. This program may require up to 12 hours to thoroughly clean
out the GC.

3. Operating methods include all of the critical setpoints required to analyze the ACE
cracked gas. KTI has included methods which accurately analyze product gases
from the ACE unit. Download ACE_ACT1S method to the GC. Wait for the GC to
stabilize (become READY) for preparation of running a calibration standard.

To print a hard copy of the instrument setpoints perform the following:

1. Method\Aquisition\Setpoints\ then press Print.
2. Select Instrument Setpoints form the pop-up menu and press Print.

NOTE: The instrument setpoints are the parameters that physically control the actions of
the GC during the analysis of an actual sample. Once a good set of parameters is
determined for the type of gas being analyzed, the remainder of the GC operations
pertain to software and analysis of the chromatogram.

The other parts of the method can also be printed to fully document the method.

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7. Cerity Database and Methods

Cerity operates with a database named "TheDB.mdb" which resides in the following
directory: C:\Program Files\Agilent\Cerity QA-QC\Default Data Directory\.

Management of TheDB.mdb is performed using the DBMaint (database maintenance)

which can only be opened and used when Cerity NDS is closed. TheDB.mdb can
become very large, so from time-to-time it is important to archive some of the records
using the DBMaint. In addition, the DBMaint can be used to export data files.

8. File Management

The Method controls:

(1) The destination folder for chromatographic results and provides a Prefix name which
may be "auto incremented".
(2) Report specifications and Export Specifications.

When a sample is logged in (under Sample) you can also provide a Sample Name. This
name will appear on the report documents, but not in any of the file names associated
with the run. The Method controls the file names and locations.

The Method\Output page allows you to select Output Type from the Output List
window. ESTD Percent Report is selected and the Report Specifications with respect
to Destinations and Layout Options are provided on the Method\Output page.

III. CALIBRATION

1. Run Actual Calibration Samples Using a Method With Proven Setpoints

Under Sample provide name/method/instrument. Also select units and whether or

not you will use an external start. Select Automatically add sample to Instrument
worklist and then press Log Sample button. If Wait for Instrument Start is selected,
then an external or remote start of the GC is required. If the sample is merely logged,
then the Instrument\Worklist\START button needs to be pressed to start the
sample (unless you have selected Automatic Worklist Start under
Instrument\Worklist).

Under Method\Analysis\Integration\Initial Settings, KTI edited the settings to

match recommended values provided in the User Information manual (Column A,
p.79; Column B, p.81; Column C, p.77; Column D, p.63).

Make a few runs. Example (09/04/07): Sample Names CAL9 to CAL14 delivered to
CAL QA auto-incremented using ACE_STD1 method. NOTE: After BAKEOUT it took
the GC about 6 hours to stabilize or equilibrate with the KTI carrier on Signal 3.

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2. Use "Method" Section to Develop the Chromatography Analysis

a. To make a "new" calibration method, delete peaks (all) under the section
Method\Analysis\Calibration\Identification.

b. Press Method\Save or Method\Save As to define the preliminary method.

(Example: ACE_STD1. The same method name can be used but it is time-
stamped to delineate it from prior methods with the same name.)

c. Go to Method\Analysis\Integration\ and open the Base Chromatogram that will

be the basis for calibration. (Example: CAL12.) Also, under Timed Events, set the
Integration OFF and ON pertinent to the Signal from each detector. Do not
include any other Timed Events.

d. Go to Method\Analysis\Calibration\Calibration and press the "Fill" button in

the left corner of the table. Enter "true" Compound Names and Amounts. Also,
under Method\Analysis\Calibration\Options select mole% and area as basis
units. Delete any unknown "trace" peaks.

e. Save Method (KTI uses ACE_STD1 again as method is in process of being built-
up).

3. Use "Reprocess" to Reanalyze the Chromatograms for the Standard Gas

a. Under Reprocess it is necessary to load the current method. There is a "folder-type"

icon on the Reprocess screen that allows you to select the appropriate method.
Before you select the appropriate method, first select the sample data you want to
reprocess. (If you select the method first and then the sample data, then the software
will trip back to the original method used to obtain that sample data. So, be careful.)

b. After selecting the sample data and then the method you can select Edit: Output.
(Example: For prefix name I used CALR instead of CAL. The "R" stands for
reprocessed.) Then, reprocess calibration samples using "group reprocess" arrow.
It is more convenient to reprocess one sample at a time and then proceed to the
Excel button and transfer the data to Excel. Then, save the data as an Excel
worksheet.

c. The Agilent 3000 is a precise analyzer. For the six repeated samples the relative
error of the analysis of a given compound in only about 1%. (Refer to C:\KTI
AGILENT 3000\CAL QA XLS\Calibration Statistics.xls.)

4. Optional: Developing a Simplified Method for the Standard Gas

Sometimes it is preferable to group specific peaks in the analysis and produce a

simplified method. This can be done, but should be performed in a manner where the
grouping is added in consistent manner and the average response factor of the group
is correct. A procedure for grouping the C5 olefins on Signal 3 is as follows.

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a. Under Method\Analysis\Calibration\Calibration select the Add Peak button.

Under the added peak place the Signal as 3, the name as C5 Olefins. Then, sum the
amounts and the areas of the peaks that are being grouped and add that to the
calibration table.

b. Delete the peaks being replaced by the C5 Olefins group.

c. Under Method\Analysis\Integration\Timed Events place the Area SUM ON and

Area Sum OFF commands at the appropriate times. Place the average retention
time in the calibration table under Method\Analysis\Calibration\Calibration.

d. Save the simplified method as ACE_STD1S.

e. Go to Reprocess and select the Base Chromatogram file. Associate the file with the
method ACE_STD1S and reprocess. Take the area count for the grouped C5 Olefin
peaks and go to Method\Analysis\Calibration\Calibration and add that area into
the calibration table for the grouped peak. Save the method again as ACE_STD1S.
(If you return to Reprocess and analyze again, you will find the Total Amount
Analyzed equal to 100.00%.)

IV. METHOD DEVELOPMENT FOR ACTUAL GASES

1. Use "Method" Section to Build-Up the Standard Gas Method for Actual Gas
Analyses

a. Column C

Note: If you are using a simplified method that groups the C5 Olefins, then go to the
next section b. Column D.

On Column C, the actual cracked gas will include a few C5 species that are not
present in most RGA calibration gas standards. KTI has added software to integrate
the most significant peaks that occur after 2-methyl-2-butene. The compound cis-2-
pentene is present in most standards and may or may not be analyzed by the GC
(depending on the amount). The peaks after 2-methyl-2-butene are grouped and
named as 2-methylpentane with a response factor equal to 2-methyl-2-butene.

The mechanics of adding this information to the method are as follows.

(1) Under Method\Analysis\Integration\ add Timed Events for Area Sum ON and
Area Sum OFF. The retention time for the sum is the average of the times for the
two events.
(2) Under Method\Analysis\Calibration\Calibration add the peak 2-methyl
pentane to signal 3 with an amount and area equal to 2-methyl-2-butene.

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b. Column D

On Column D, the actual cracked gas will include a large amount of material
representing numerous compounds not present in most RGA calibration gas
standards. These peaks are not well resolved by Column D, but the amount and
molecular weight may be estimated well from the chromatogram. KTI has added
software to integrate these unknown peaks as three groups: "C6+ 1", "C6+ 2", and
C6+ 3. All of the components on this column are given the response factor (RF) of
n-hexane as determined by the analysis of the standard gas.

The mechanics of adding this information to the method are as follows.

(1) Under Method\Analysis\Integration\ add Timed Events for Area Sum ON and
Area Sum OFF covering three time spans. The retention time for each area sum
is the average of the times for the respective ON and OFF events.
(2) Under Method\Analysis\Calibration\Calibration, add the three peak names
above to signal 4 with an amount and area equal to n-hexane. After adding the
RT, amount, and area, then delete n-hexane from the table (that was present for
the calibration gas analysis) and apply the three names above.

Save the built-up method as ACE_ACT1S. This method can be used to reprocess the
calibration standard and the results should be very close to 100%. Slight differences will
occur because of the altered integration events and retention times installed into the
"actual gas" method.

The ACE_ACT1S method can be used to analyze ACE cracked gases. The ultimate
output from the analyses will be used in the Material Balance Program.

V. OPERATION OF GC WITH THE ACE UNIT

The ACE-Model R+ will trigger the GC automatically when gas samples are ready to be
analyzed. The operator needs to setup the GC to receive these samples and save the
results as follows.

1. Under Method, if you alter the Output location for the data, it is necessary to re-save
the method. KTI recommends sending actual analysis files to a folder specific to the
project being studied. This is performed in Method\Output.

2. To setup for actual operation, go to Sample\Edit and provide sample

names\method\instrument. Also, select Wait for Instrument Start under Sample
Information.

3. After samples are logged in, go to Instrument\Worklist and check that samples are
logged-in and will run automatically. The GC will not run until it receives an external
signal from the ACE unit.

4. When the runs are completed, review each chromatogram carefully to make sure
peaks are analyzed properly. Use the Reprocess menu to make adjustments if

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necessary (example: retention times). If you edit the Method, make sure to save the
altered Method for future use.

Use Reprocess to deliver data to Excel. It is not necessary to print hard copies of any
of the chromatograms.

VI. COMMENTS ON ACE AND GC SIGNALS

The ACE unit triggers the Agilent 3000 RGA to run when the gas sample is available and
the GC is READY.

The GC is "READY" for externally triggered runs only when samples have been entered
to the worklist through Sample\Edit\Log Sample. So, if there are no samples in the
worklist, then the ACE unit will indicate the GC is BUSY. Also, during actual GC
operations on a sample the status will be BUSY.

VII. STARTUP AND SHUTDOWN BASICS

STARTUP

The procedure below is for a new installation. Normally, after initial installation, you
would begin at step no. 6.

1. Gas Supply - Connect Argon and Helium at 80 psig (550 kPag).

2. Hard Electrical Connections - Connect Power, crossover ethertwist, and Remote
cables.
3. Turn GC ON at front of the GC. Wait for two beeps after the initial beep.
4. Special Software Setup Parameters - Setup the PC as stand-alone with IP
addresses noted in Section II.
5. PC to GC Communication. Open Internet Explorer to check GC Status.
6. Enable Cerity NDS Communication to the GC using ConnectAdmin.
7. Initial Use of Cerity NDS and the GC - Open Cerity and go to Instrument\Status
to view the current operation. Download the appropriate method from the
Instrument tab.
8. Go to Instrument\Status and make sure the method is performing within the GC.

SHUTDOWN - TEMPORARY

The procedure below assumes you want to take the GC offline for a temporary
period of time.

1. From Instrument\Status download the method named COOLDOWN. This

method turns all heaters to a setpoint of 30C, leaves the detectors ON, but
retains column head pressure at 30 psig (206.9 kPag).

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2. After the unit has cooled down, download the method SHUTDOWN0 to turn OFF
the detectors, then SHUTDOWN1 which will reduce column head pressures to
15 psig (~100 kPag).
3. Leave the GC Power ON.
4. Go ConnectAdmin and Disconnect the ACE RGA.
5. If you return to Cerity NDS, you will find message "ACE RGA is Offline".

SHUTDOWN - LONG TERM

The procedure below assumes you want to take the GC offline for an extended
period of time.

1. From Instrument\Status download the method named COOLDOWN. This

method turns all heaters to a setpoint of 30C, but retains column head pressure
at 30 psig (206.9 kPag) with the detectors ON.
2. After the unit has cooled down, download the method SHUTDOWN0 and then
SHUTDOWN1 which will reduce column head pressures to 15.0 psig (~100
kPag).
3. Download SHUTDOWN2 which will reduce column head pressures to zero.
4. Go to ConnectAdmin and Disconnect the ACE RGA.
5. Turn the GC Power OFF. If you are moving the instrument, disconnect the gas
lines and plug the gas supply inlets.
6. If you return to Cerity NDS, you will find message "ACE RGA is Offline".

END

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