Professional Documents
Culture Documents
in AVTUR
www.paclp.com
PAC ROTTERDAM
Kiotoweg 555
3047 BG ROTTERDAM
The Netherlands
Dear customer,
At PAC we develop, produce, and support high end chromatography products under the
brand AC Analytical Controls and are characterized by significant added value for your
industry. It is our goal to create instruments that meet your analytical expectations today
and in the future.
Our Quality Management system (audited against ISO 9001 standards) supports our
product development, production and service-processes to ensure that our products and
services are constantly in line with your requirements.
Before your analytical system leaves our facilities it is fully calibrated and tested to
(requested) specifications. Included you will find the final technical documentation for
your FAME in AVTUR Analyzer with the following sections:
• Analysis description
• Startup procedures
• Actual settings
• Sample preparation and sample handling
• Method description
• Qualification Results
PAC also offers you a full range of support tools to ensure the analytical integrity and
performance of your application, such as consumables and spare parts, calibration and
reference samples, classroom and on-site training, service contracts, modem support and
the AC Response Center (free helpdesk).
If you have any questions regarding our support tools or if you need assistance, please do
not hesitate to contact our Response Center:
E-mail: service.netherlands@paclp.com
Phone: +31-10-2456 248
Fax: +31-10-2456 241
Website: www.paclp.com
Rick Felix
Value Stream Manager GC
www.paclp.com
AC FAME in AVTUR
on Agilent 7890
PAC Rotterdam
AC Analytical Controls BV
P.O Box 10054, 3004 AB Rotterdam
Kiotoweg 555, 3047BG Rotterdam, the Netherlands
Phone: +31-10-462 4811
Fax: +31-10-462 6330
E-mail: acbv@paclp.com
PAC Singapore
AC Analytical Controls Asia Pacific Ltd
61, Science Park Road #03-09/10 The Galen, Singapore Science Park III
Singapore 117525
Phone: +65 6412 0890
Fax: +65 6412 0899
E-mail: ac-asia@paclp.com
THIS DOCUMENT CONTAINS CONFIDENTIAL AND PROPRIETARY INFORMATION THAT IS THE SOLE PROPERTY OF PETROLEUM ANALYZER COMPANY, L.P. ("PAC") AND NO
OWNERSHIP OR LICENSE RIGHTS ARE GRANTED BY DELIVERY OF THIS DOCUMENT TO THE RECIPIENT. THIS DOCUMENT AND ALL INFORMATION DISCLOSED HEREIN (A)
SHALL NOT BE USED TO MANUFACTURE, CONSTRUCT OR FABRICATE THE GOODS DISCLOSED HEREIN OR ANY DERIVATIVE WORKS OF THE SAME; (B) SHALL NOT BE
EXPLOITED OR SOLD BY ANY MEANS; (C) SHALL NOT BE COPIED OR OTHERWISE REPRODUCED IN WHOLE OR IN PART; (D) SHALL NOT BE REVEALED OR DISCLOSED TO
ANYONE EXCEPT THOSE PERSONS EMPLOYED OR ENGAGED BY THE RECIPIENT AND HAVING A LEGITIMATE "NEED TO KNOW" THE INFORMATION CONTAINED IN THIS
DOCUMENT, OR IN ANY MANNER MADE PUBLIC WITHOUT THE EXPRESS WRITTEN PERMISSION OF PAC; (E) SHALL BE HELD BY THE RECIPIENT OF THIS DOCUMENT IN
STRICT CONFIDENCE AS A FIDUCIARY; AND (F) SHALL BE PROTECTED AND KEPT SEPARATE FROM THE DOCUMENTS AND MATERIALS OF THE RECIPIENT OF THIS
DOCUMENT. THIS DOCUMENT AND ALL INFORMATION CONTAINED HEREIN SHALL REMAIN THE PROPERTY OF PAC AND SHALL BE RETURNED UPON DEMAND. ALL
PROPRIETARY INFORMATION IS PROVIDED "AS IS" WITHOUT WARRANTY OF ANY KIND, WHETHER EXPRESS OR IMPLIED, INCLUDING WITHOUT LIMITATION ANY
WARRANTIES REGARDING THE TIMELINESS, ACCURACY OR COMPLETENESS OF THE PROPRIETARY INFORMATION.
Information
The information contained within these materials is subject to change without notice. PAC makes no warranties or guarantees, either expressed or implied in
these materials, including the warranty of merchantability or fitness for a particular purpose. At any time, PAC may modify these materials, its instruments or its
programs without notice and subsequent versions of these materials may contain different information. These materials could contain technical inaccuracies
and/or typographical errors. PAC does not assume responsibility for the accuracy of any translation of these materials.
Table of Contents
1 Instrument Description ............................................... 5
1.1 General ....................................................................................... 5
1.2 Analysis description ........................................................................ 6
1.3 Flow Diagram ................................................................................ 6
2 Specifications .......................................................... 7
2.1 Leak testing ............................................................................... 7
2.2 Hardware control test .................................................................. 7
2.3 Analytical control test .................................................................. 7
3 Startup Procedure ................................................... 10
4 Actual Settings of the Analyzer ................................... 11
4.1 Pressures and Flows ................................................................... 11
4.2 PID Settings GC ......................................................................... 11
5 Hardware Description .............................................. 12
5.1 Components............................................................................. 12
5.3 Columns.................................................................................. 13
6 Sample preparation and sample handling ...................... 14
6.1 Validation check .......................................................................... 14
7 ChemStation method description ................................ 15
7.1 CUTTING TIME IP599 C16 C18.m....................................................... 15
7.2 IP599 C16 C18.m ......................................................................... 20
7.3 CUTTING TIME C14.m .................................................................... 26
7.4 APPENDIX IP599 C14.m .................................................................. 31
8 Qualification results ................................................ 36
8.1 Cutting Time Determination C16-C18 ............................................. 36
8.2 RF check 1st dimension column ..................................................... 37
8.3 Cutting Time Determination C14 ................................................... 39
8.4 Calibration .............................................................................. 40
8.5 Validation ............................................................................... 48
9 Spares and Consumables ........................................... 52
9.1 CCG4800.100 Spare kit ............................................................... 52
9.2 CCG4800.200 Consumable kit ....................................................... 52
1 Instrument Description
1.1 General
The introduction of biodiesel into many countries has created a new threat to jet fuel
quality. It is now common for national governments to mandate the use of renewable
components in automotive fuels. One of the most common options is to blend Fatty Acid
Methyl Ester (FAME) into diesel to produce what is often called ‘biodiesel’. Biodiesel is
designated B5 when it contains 5% FAME. Pure FAME is often designated as B100.
The introduction of FAME into diesel fuel created some issues with an impact on jet fuel:
1) FAME is surface active and tends to stick to metal or glass surfaces. Where supply
chains handle both jet fuel and biodiesel this trait creates a risk of cross contamination
2) FAME is a non-hydrocarbon fuel component. The jet fuel specification states explicitly
that only hydrocarbon components or approved additives are allowed.
The international jet fuel specifications (e.g. DEF STAN 91-91) limit FAME content to less
than 5 mg/kg (ppm w/w). Levels above 5 mg/kg render the fuel off-specification.
This is a serious issue because there have been instances in which jet fuel containing
more than 5 ppm FAME has inadvertently been supplied to the airport.
A reliable and rugged means of measuring FAME content in jet fuels is required to ensure
compliance to the 5 mg/kg specification. Multi-dimensional GC using Deans switching and
refocusing technology supplies such a means.
The FAME components determined, using this multi-dimensional GC heart-cut method,
are listed in table below. These components have been specifically chosen as they
typically make up greater than 95% of the composition of the major biofuel vegetable oil
feeds currently used in biodiesel blends with conventional mineral diesel.
The IP599 method covers only C16:0, C18:0, C18:1, C18:2 and C18:3. C14:0 is included in
the appendix of the IP method.
FAME Molecular formula Symbol used
Methyl hexadecanoate (methyl palmitate) C17H34O2 C16:0
Methyl octadecanoate (methyl stearate) C19H38O2 C18:0
Methyl octadecenoate (methyl oleate) C19H36O2 C18:1
Methyl octadecadienoate (linoleate) C19H34O2 C18:2
Methyl octadecatrienoate (linolenate) C19H32O2 C18:3
Methyl heptadecanoate (methyl margarate) C19H38O2 C17:0
Methyl myrisate C15H2902 C14:0
PCM C-1
(H2)
2 Air
V1 3
1
Front
1 V2 Column 2 detector
2
FID
Refocus trap
S/SL Column 1
Back Inlet (H2)
Back
detector
monitor
FID
2 Specifications
2.3.4 LOQ
The limit of quantification for the individual FAME components is set at 1.5 mg/kg and
was determined by injecting standard 00.02.614 and performing calculation as follows:
2 nd Dimension
Component Noise (pA) Area (pA*s) Conc. (mg/kg) Peak width (min) LOQ (mg/kg)
C16:0 0.029 12.73 5.10 0.051 0.3
C18:0 0.029 15.51 4.90 0.077 0.4
C18:1 0.024 12.30 4.91 0.084 0.5
C18:2 0.032 9.10 4.97 0.093 1.0
C18:3 0.020 8.52 5.30 0.104 0.8
C14:0 0.028 26.48 5.12 0.084 0.3
C17:0 0.052 12.57 4.96 0.105 1.3
The peak symmetry was checked by running sample 00.02.615 with C16-C18 full
method.m
3 Startup Procedure
1. Check if all boxes are delivered and unpack the boxes (see installation checklist for
more details).
2. Put the Analyzer on the bench and connect the gases to the connections on the back
side of the GC as the figure below.
3. The capillary columns are already connected during factory testing. Please check if
all the connections are still ok.
4. Setup the PC on the bench.
a) If a PC wasn’t ordered with the analyzer, install and configure the ChemStation
software on the customer PC.
b) Copy the Methods from the AC Methods and Data USB key to the ChemStation
Methods directory.
5. Connect the GC to the computer using the LAN cable.
6. Connect the power cord to the GC and switch on the GC.
7. Adjust the proper pressures, flows and temperatures using the actual settings of the
analyzer, see chapter “Actual settings of the analyzer” and “ChemStation method
description”.
8. Enter the correct IP-addresses for the PC, GC and ChemStation.
9. Start the ChemStation program on the computer.
10. Load the desired method.
11. Make sure the solvent-position and waste position in the sample-tray are occupied.
The solvent vial needs to be filled with cyclohexane.
12. The GC is now ready for analysis.
2 3
Component Gas
1 Connections Front detector; Back detector; Back Inlet; Hydrogen
EPC Restriction
2 Connection Front detector; Back detector Air
3 Connection Front detector; Back detector Nitrogen
5 Hardware Description
5.1 Components
5.3 Columns
2 3
1
4 5
• Take the sample out of cold storage and put it at room temperature.
• Allow the sample to reach ambient temperature and shake well.
• Fill out the sample in a 1.5ml GC vial and cap the vial.
• Put the vial in the auto sampler turret or the tray.
• Start up the ChemStation program.
• Create a sequence with the sequence menu.
• Append a line and enter vial number; sample name; sample type and injections per
vial.
• Save the sequence and start the sequence with Run Control\ Run sequence.
NOTE - All Cutting time methods are tuned with the high range sample to make sure nothing is
cut off from the components of interest.
When either 00.02.616 or 00.02.617 falls outside its reproducibility boundaries the system
may either need to be calibrated again or it needs to be serviced.
If after calibration the found response factors for the different peaks are running too far
apart (by more than 25%), this is probably caused by one of the following reasons:
• The glass liner in the inlet is getting too active and needs replacement
• The 2nd dimension column is getting too active and needs replacement
Method Information
Data Acquisition: on
=====================================================================
Agilent 7890B
=====================================================================
GC
GC Summary
Run Time 23.4 min
Post Run Time 0 min
Oven
Equilibration Time 3 min
Max Temperature 275 °C
Maximum Temperature Override Disabled
Slow Fan Disabled
Temperature
Setpoint On
(Initial) 230 °C
Hold Time 15 min
Post Run 100 °C
Program
#1 Rate 25 °C/min
#1 Value 275 °C
#1 Hold Time 6.6 min
ALS
Back Injector
Syringe Size 5 μL
Injection Volume 2.5 μL
Solvent A Washes (PreInj) 0
Solvent A Washes (PostInj) 4
Solvent A Volume 4 μL
Solvent B Washes (PreInj) 0
Solvent B Washes (PostInj) 0
Solvent B Volume 4 μL
Sample Washes 4
Sample Wash Volume 4 μL
Sample Pumps 6
Dwell Time (PreInj) 0 min
Dwell Time (PostInj) 0 min
Solvent Wash Draw Speed 150 μL/min
Solvent Wash Dispense Speed 1500 μL/min
Sample Wash Draw Speed 150 μL/min
Sample Wash Dispense Speed 1500 μL/min
Injection Dispense Speed 3000 μL/min
Viscosity Delay 0 sec
Sample Depth Disabled
Injection Type Standard
L1 Airgap 0.1 μL
Solvent Wash Mode A, B
Sample Overlap
Mode Sample overlap is not enabled
Back SS Inlet H2
Mode Split
Heater On 300 °C
Pressure On 410 kPa
Total Flow On 48.958 mL/min
Septum Purge Flow On 5 mL/min
Gas Saver On 20 After 2 min mL/min
Split Ratio 20 :1
Split Flow 41.865 mL/min
Liner A Liner has not been selected.
Column
Column Outlet Pressure 0 kPa
Column #1
Column Information PAC 10.73.154
1st Dimension Column FAME in A
Temperature Range -60 °C—275 °C (275 °C)
Dimensions 30 m x 250 μm x 1 μm
In Back SS Inlet H2
Out PCM C
(Initial) 230 °C
Pressure 410 kPa
Flow 2.0933 mL/min
Average Velocity 25.372 cm/sec
Holdup Time 1.9707 min
Control Mode Ramped Pressure
Pressure
Setpoint On
(Initial) 410 kPa
Hold Time 20 min
Post Run 410 kPa
Program
#1 Rate 100 kPa/min
#1 Value 50 kPa
#1 Hold Time 0 min
Column #2
Column Information PAC 10.73.138
2nd Dimension Column FAME in A
Temperature Range -60 °C—275 °C (275 °C)
Dimensions 60 m x 250 μm x 0.2 μm
In PCM C H2
Out Front Detector FID
(Initial) 230 °C
Pressure 360 kPa
Flow 4.4728 mL/min
Average Velocity 81.483 cm/sec
Holdup Time 1.2273 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 360 kPa
Column #3
Column Information PAC 10.52.029
Monitor Column FAME in AVTUR
Temperature Range -60 °C—275 °C (275 °C)
Dimensions 1.8 m x 100 μm x 0 μm
Column lock Unlocked
In PCM C H2
Out Back Detector FID
(Initial) 230 °C
Pressure 360 kPa
Flow 3.8413 mL/min
Average Velocity 435.97 cm/sec
Holdup Time 0.0068812 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 360 kPa
Valve 1
Switching Valve Off
Valve 2
Switching Valve Off
PCM C
PCM C H2
PCM C H2 Supplies Column 2
Aux PCM C N2
***Excluded from Affecting GC's Readiness
State***
Pressure
Setpoint Off
(Initial) 0 kPa
Post Run 0 kPa
Signals
Signal #1: Front Signal
Description Front Signal
Details Front Signal (FID)
Save On
Data Rate 20 Hz
Zero Signal Zero @ 0 min
Signal #3:
Description None
Signal #4:
Description None
========================================================================
Integration Events
========================================================================
------------------------------------------------------------------------
Non signal specific Integration Events
------------------------------------------------------------------------
Event Value
|--------------------------------------------------------|-------------|
Tangent Skim Mode Standard
Tail Peak Skim Height Ratio 0.000
Front Peak Skim Height Ratio 0.000
Skim Valley Ratio 20.000
Baseline Correction Classical
Peak to Valley Ratio 500.000
------------------------------------------------------------------------
Default Integration Event Table "Event"
------------------------------------------------------------------------
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_FID"
------------------------------------------------------------------------
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_FID2B"
------------------------------------------------------------------------
Method Information
Data Acquisition: on
=====================================================================
Agilent 7890B
=====================================================================
GC
GC Summary
Run Time 50 min
Post Run Time 0 min
Oven
Equilibration Time 3 min
Max Temperature 275 °C
Maximum Temperature Override Disabled
Slow Fan Disabled
Temperature
Setpoint On
(Initial) 230 °C
Hold Time 15 min
Post Run 230 °C
Program
#1 Rate 25 °C/min
#1 Value 140 °C
#1 Hold Time 1.4 min
#2 Rate 1 °C/min
#2 Value 160 °C
#2 Hold Time 0 min
#3 Rate 25 °C/min
#3 Value 275 °C
#3 Hold Time 5.4 min
ALS
Back Injector
Syringe Size 5 μL
Injection Volume 2.5 μL
Solvent A Washes (PreInj) 0
Solvent A Washes (PostInj) 4
Solvent A Volume 4 μL
Solvent B Washes (PreInj) 0
Solvent B Washes (PostInj) 0
Solvent B Volume 4 μL
Sample Washes 4
Sample Wash Volume 4 μL
Sample Pumps 6
Dwell Time (PreInj) 0 min
Dwell Time (PostInj) 0 min
Solvent Wash Draw Speed 150 μL/min
Solvent Wash Dispense Speed 1500 μL/min
Sample Wash Draw Speed 150 μL/min
Sample Wash Dispense Speed 1500 μL/min
Injection Dispense Speed 3000 μL/min
Viscosity Delay 0 sec
Sample Depth Disabled
Injection Type Standard
L1 Airgap 0.1 μL
Solvent Wash Mode A, B
Sample Overlap
Mode Sample overlap is not enabled
Back SS Inlet H2
Mode Split
Heater On 300 °C
Pressure On 410 kPa
Total Flow On 48.958 mL/min
Septum Purge Flow On 5 mL/min
Gas Saver On 20 After 2 min mL/min
Split Ratio 20 :1
Split Flow 41.865 mL/min
Liner A Liner has not been selected.
Column
Column Outlet Pressure 0 kPa
Column #1
Column #2
Column Information PAC 10.73.138
2nd Dimension Column FAME in A
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 60 m x 250 μm x 0.2 μm
Column lock Unlocked
In PCM C H2
Out Back Detector FID
(Initial) 230 °C
Pressure 360 kPa
Flow 4.4728 mL/min
Average Velocity 81.483 cm/sec
Holdup Time 1.2273 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 350 kPa
Column #3
Column Information PAC 10.52.029
Monitor Column FAME in AVTUR
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 1.8 m x 100 μm x 0 μm
Column lock Unlocked
In PCM C H2
Out Front Detector FID
(Initial) 230 °C
Pressure 360 kPa
Flow 3.8413 mL/min
Average Velocity 435.97 cm/sec
Holdup Time 0.0068812 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 350 kPa
Makeup N2
Heater On 300 °C
H2 Flow On 30 mL/min
Air Flow On 400 mL/min
Makeup Flow On 40 mL/min
Carrier Gas Flow Correction Constant Makeup and Fuel Flow
Flame On
Valve 1
Switching Valve Off
Valve 2
Switching Valve Off
PCM C
PCM C H2
PCM C H2 Supplies Column 2
Aux PCM C N2
***Excluded from Affecting GC's Readiness
State***
Pressure
Setpoint Off
(Initial) 0 kPa
Post Run 0 kPa
Signals
Signal #1: Front Signal
Description Front Signal
Details Front Signal (FID)
Save On
Data Rate 20 Hz
Signal #3:
Description None
Signal #4:
Description None
========================================================================
Integration Events
========================================================================
------------------------------------------------------------------------
Non signal specific Integration Events
------------------------------------------------------------------------
Event Value
|--------------------------------------------------------|-------------|
Tangent Skim Mode Standard
Tail Peak Skim Height Ratio 0.000
Front Peak Skim Height Ratio 0.000
Skim Valley Ratio 20.000
Baseline Correction Classical
Peak to Valley Ratio 500.000
------------------------------------------------------------------------
Default Integration Event Table "Event"
------------------------------------------------------------------------
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_FID"
------------------------------------------------------------------------
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_FID2B"
------------------------------------------------------------------------
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_FID1A"
------------------------------------------------------------------------
Method Information
Data Acquisition: on
=====================================================================
Agilent 7890B
=====================================================================
GC
GC Summary
Run Time 40 min
Post Run Time 0 min
Oven
Equilibration Time 3 min
Max Temperature 275 °C
Maximum Temperature Override Disabled
Slow Fan Disabled
Temperature
Setpoint On
(Initial) 165 °C
Hold Time 30 min
Post Run 100 °C
Program
#1 Rate 25 °C/min
#1 Value 275 °C
#1 Hold Time 5.6 min
ALS
Back Injector
Syringe Size 5 μL
Injection Volume 2.5 μL
Solvent A Washes (PreInj) 0
Solvent A Washes (PostInj) 4
Solvent A Volume 4 μL
Solvent B Washes (PreInj) 0
Solvent B Washes (PostInj) 0
Solvent B Volume 4 μL
Sample Washes 4
Sample Wash Volume 4 μL
Sample Pumps 6
Dwell Time (PreInj) 0 min
Dwell Time (PostInj) 0 min
Solvent Wash Draw Speed 150 μL/min
Solvent Wash Dispense Speed 3000 μL/min
Sample Wash Draw Speed 150 μL/min
Sample Wash Dispense Speed 3000 μL/min
Injection Dispense Speed 3000 μL/min
Viscosity Delay 0 sec
Sample Depth Disabled
Injection Type Standard
L1 Airgap 0.1 μL
Solvent Wash Mode A, B
Sample Overlap
Mode Sample overlap is not enabled
Back SS Inlet H2
Mode Split
Heater On 300 °C
Pressure On 410 kPa
Total Flow On 34.058 mL/min
Septum Purge Flow On 5 mL/min
Gas Saver On 20 After 2 min mL/min
Split Ratio 10 :1
Split Flow 26.416 mL/min
Liner A Liner has not been selected.
Column
Column Outlet Pressure 0 kPa
Column #1
Column Information PAC 10.73.154
1st Dimension Column FAME in A
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 30 m x 250 μm x 1 μm
Column lock Unlocked
In Back SS Inlet H2
Out PCM C
(Initial) 165 °C
Pressure 410 kPa
Flow 2.6416 mL/min
Average Velocity 27.882 cm/sec
Holdup Time 1.7933 min
Control Mode Ramped Pressure
Pressure
Setpoint On
(Initial) 410 kPa
Hold Time 30 min
Post Run 410 kPa
Program
#1 Rate 50 kPa/min
#1 Value 50 kPa
#1 Hold Time 0 min
Column #2
Column Information PAC 10.73.138
2nd Dimension Column FAME in A
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 60 m x 250 μm x 0.2 μm
Column lock Unlocked
In PCM C H2
Out Front Detector FID
(Initial) 165 °C
Pressure 360 kPa
Flow 5.6445 mL/min
Average Velocity 89.544 cm/sec
Holdup Time 1.1168 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 360 kPa
Column #3
Column Information PAC 10.52.029
Monitor Column FAME in AVTUR
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 1.8 m x 100 μm x 0 μm
Column lock Unlocked
In PCM C H2
Out Back Detector FID
(Initial) 165 °C
Pressure 360 kPa
Flow 4.8476 mL/min
Average Velocity 479.1 cm/sec
Holdup Time 0.0062618 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 360 kPa
Flame On
Valve 1
Switching Valve Off
Valve 2
Switching Valve Off
PCM C
PCM C H2
PCM C H2 Supplies Column 2
Aux PCM C N2
***Excluded from Affecting GC's Readiness
State***
Pressure
Setpoint Off
(Initial) 68.948 kPa
Post Run 0 kPa
Signals
Signal #1: Front Signal
Description Front Signal
Details Front Signal (FID)
Save On
Data Rate 20 Hz
Signal #3:
Description None
Signal #4:
Description None
========================================================================
Integration Events
========================================================================
------------------------------------------------------------------------
Non signal specific Integration Events
------------------------------------------------------------------------
Event Value
|--------------------------------------------------------|-------------|
Tangent Skim Mode Standard
Tail Peak Skim Height Ratio 0.000
Front Peak Skim Height Ratio 0.000
Skim Valley Ratio 20.000
Baseline Correction Classical
Peak to Valley Ratio 500.000
------------------------------------------------------------------------
Default Integration Event Table "Event"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 1.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 1.000 Initial
Initial Height Reject 1.700 Initial
Initial Shoulders OFF Initial
Initial Area Percent Reject 0.000 Initial
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_FID"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 50.000 Initial
Initial Peak Width 0.400 Initial
Initial Area Reject 0.000 Initial
Initial Height Reject 0.000 Initial
Initial Shoulders OFF Initial
Initial Area Percent Reject 0.000 Initial
Integration OFF 0.010
Integration ON 10.000
Integration OFF 30.000
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_FID1A"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 50.000 Initial
Initial Peak Width 0.020 Initial
Initial Area Reject 0.000 Initial
Initial Height Reject 0.000 Initial
Initial Shoulders OFF Initial
Initial Area Percent Reject 0.000 Initial
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_FID2B"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 10.000 Initial
Initial Peak Width 0.400 Initial
Initial Area Reject 0.000 Initial
Initial Height Reject 0.000 Initial
Initial Shoulders OFF Initial
Initial Area Percent Reject 0.000 Initial
Integration OFF 0.010
Integration ON 20.000
Integration OFF 30.000
Method Information
Data Acquisition: on
=====================================================================
Agilent 7890B
=====================================================================
GC
GC Summary
Run Time 54 min
Post Run Time 0 min
Oven
Equilibration Time 3 min
Max Temperature 275 °C
Maximum Temperature Override Disabled
Slow Fan Disabled
Temperature
Setpoint On
(Initial) 165 °C
Hold Time 30 min
Post Run 100 °C
Program
#1 Rate 25 °C/min
#1 Value 120 °C
#1 Hold Time 12.2 min
#2 Rate 25 °C/min
#2 Value 275 °C
#2 Hold Time 3.8 min
ALS
Back Injector
Syringe Size 5 μL
Injection Volume 2.5 μL
Solvent A Washes (PreInj) 0
Solvent A Washes (PostInj) 4
Solvent A Volume 4 μL
Solvent B Washes (PreInj) 0
Solvent B Washes (PostInj) 0
Solvent B Volume 4 μL
Sample Washes 4
Sample Wash Volume 4 μL
Sample Pumps 6
Dwell Time (PreInj) 0 min
Dwell Time (PostInj) 0 min
Solvent Wash Draw Speed 150 μL/min
Solvent Wash Dispense Speed 1500 μL/min
Sample Wash Draw Speed 150 μL/min
Sample Wash Dispense Speed 1500 μL/min
Injection Dispense Speed 3000 μL/min
Viscosity Delay 0 sec
Sample Depth Disabled
Injection Type Standard
L1 Airgap 0.1 μL
Solvent Wash Mode A, B
Sample Overlap
Mode Sample overlap is not enabled
Back SS Inlet H2
Mode Split
Heater On 300 °C
Pressure On 410 kPa
Total Flow On 34.058 mL/min
Septum Purge Flow On 5 mL/min
Gas Saver On 20 After 2 min mL/min
Split Ratio 10 :1
Split Flow 26.416 mL/min
Liner A Liner has not been selected.
Column
Column Outlet Pressure 0 kPa
Column #1
Column Information PAC 10.73.154
1st Dimension Column FAME in A
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 30 m x 250 μm x 1 μm
Column lock Unlocked
In Back SS Inlet H2
Out PCM C
(Initial) 165 °C
Pressure 410 kPa
Flow 2.6416 mL/min
Average Velocity 27.882 cm/sec
Holdup Time 1.7933 min
Control Mode Ramped Pressure
Pressure
Setpoint On
(Initial) 410 kPa
Hold Time 30 min
Post Run 410 kPa
Program
#1 Rate 50 kPa/min
#1 Value 50 kPa
#1 Hold Time 0 min
Column #2
Column Information PAC 10.73.138
2nd Dimension Column FAME in A
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 60 m x 250 μm x 0.2 μm
Column lock Unlocked
In PCM C H2
Out Front Detector FID
(Initial) 165 °C
Pressure 360 kPa
Flow 5.6445 mL/min
Average Velocity 89.544 cm/sec
Holdup Time 1.1168 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 360 kPa
Column #3
Column Information PAC 10.52.029
Monitor Column FAME in AVTUR
Temperature Range 0 °C—275 °C (275 °C)
Dimensions 1.8 m x 100 μm x 0 μm
Column lock Unlocked
In PCM C H2
Out Back Detector FID
(Initial) 165 °C
Pressure 360 kPa
Flow 4.8476 mL/min
Average Velocity 479.1 cm/sec
Holdup Time 0.0062618 min
Control Mode Constant Pressure
Pressure
Setpoint On
(Initial) 360 kPa
Post Run 360 kPa
Valve 1
Switching Valve Off
Valve 2
Switching Valve Off
PCM C
PCM C H2
PCM C H2 Supplies Column 2
Aux PCM C N2
***Excluded from Affecting GC's Readiness
State***
Pressure
Setpoint Off
(Initial) 0 kPa
Post Run 0 kPa
Signals
Signal #1: Front Signal
Description Front Signal
Details Front Signal (FID)
Save On
Data Rate 20 Hz
Signal #3:
Description None
Signal #4:
Description None
------------------------------------------------------------------------
Detector Default Integration Event Table "Event_FID"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 50.000 Initial
Initial Peak Width 0.400 Initial
Initial Area Reject 0.000 Initial
Initial Height Reject 0.000 Initial
Initial Shoulders OFF Initial
Initial Area Percent Reject 0.000 Initial
Integration OFF 0.010
Integration ON 10.000
Integration OFF 30.000
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_FID2B"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 5.000 Initial
Initial Peak Width 0.040 Initial
Initial Area Reject 0.000 Initial
Initial Height Reject 0.000 Initial
Initial Shoulders OFF Initial
Initial Area Percent Reject 0.000 Initial
Integration OFF 0.010
Integration ON 18.000
Integration OFF 18.700
------------------------------------------------------------------------
Signal Specific Integration Event Table "Event_FID1A"
------------------------------------------------------------------------
Event Value Time
|------------------------------------------------|-------------|-------|
Initial Slope Sensitivity 50.000 Initial
Initial Peak Width 0.020 Initial
Initial Area Reject 0.000 Initial
Initial Height Reject 0.000 Initial
Initial Shoulders OFF Initial
Initial Area Percent Reject 0.000 Initial
Integration OFF 0.010
Fixed Peak Width 0.040 35.000
Slope Sensitivity 2.000 35.000
Integration ON 38.713
Integration OFF 42.000
8 Qualification results
8.1 Cutting Time Determination C16-C18
Running sample 00.02.615, using the method C16-C18 Cutting Times, will yield a
chromatogram from which the correct cutting times to be used for C16 and C18
measurement can be determined. These cutting times need to be entered into method
C16-C18 Full Method.
FID1 A, Front Signal (D191209\S191209A 2019-12-09 16-28-48\B-001-201-00.02.615 C14 cutting time.D)
pA
70
60
50
40
30
20
10
-10
0 2.5 5 7.5 10 12.5 15 17.5 min
FID2 B, Back Signal (D191209\S191209A 2019-12-09 16-28-48\B-001-201-00.02.615 C14 cutting time.D)
pA
/3
70 1/2
18:
C
60 0
16:
C
50 0
17:
C
40 0
18:
C
30
20
10
-10
0 2.5 5 7.5 10 12.5 15 17.5 min
NOTE: When the cutting times are entered into the method, make sure that the refocus
cooling trap is activated 2 minutes before starting the 1st heart-cut (C16:0). This way the
refocus trap is cold enough (below 25 Celsius) at the moment that the 1st FAME component
C16:0 reaches it.
70
60
50
40
30
20
10
-10
0 2.5 5 7.5 10 12.5 15 17.5 min
FID2 B, Back Signal (D191209\S191209A 2019-12-09 16-28-48\B-001-201-00.02.615 C14 cutting time.D)
pA
/3
70 1/2
18:
C
60 0
16:
C
50 0
17:
C
40 0
18:
C
30
20
10
-10
0 2.5 5 7.5 10 12.5 15 17.5 min
If the found response factors for the different peaks are running too far apart (by roughly
more than 25%), this can be an indication that the glass liner in the inlet is getting too
active and needs replacement.
=====================================================================
Acq. Operator : SYSTEM Seq. Line : 1
Sample Operator : SYSTEM
Acq. Instrument : Trace Fame Avtur Location : 201 (B)
Injection Date : 12/9/2019 4:30:20 PM Inj : 1
Inj Volume : 2.5 µl
Acq. Method : C:\Chem32\2\Data\D191209\S191209A 2019-12-09 16-28-48\IP599 C16 C18
Cutting
Time.M
Last changed : 11/1/2019 9:00:06 AM by SYSTEM
Analysis Method : C:\Chem32\2\Data\D191209\S191209A 2019-12-09 16-28-48\IP599 C16 C18
Cutting
Time.M (Sequence Method)
Last changed : 12/10/2019 3:28:11 PM by SYSTEM
(modified after loading)
=====================================================================
External Standard Report
=====================================================================
Sorted By : Signal
Calib. Data Modified : 12/10/2019 3:28:11 PM
Multiplier : 1.0000
Dilution : 1.0000
Use Multiplier & Dilution Factor with ISTDs
=====================================================================
*** End of Report ***
90
80
70
60
50
40
30
20
10
0
0 5 10 15 20 25 30 35 min
FID2 B, Back Signal (D191209\S191209A 2019-12-09 16-28-48\B-002-201-00.02.615 C14 cutting time.D)
pA
90
80
70
60
50
0
4:
40
C1
30
20
10
0
0 5 10 15 20 25 30 35 min
NOTE: When the cutting times are entered into the method, make sure that the refocus
cooling trap is activated 2 minutes before starting the 1st heart-cut (C14:0). This way the
refocus trap is cold enough (below 25 Celsius) at the moment that the 1st FAME component
C14:0 reaches it.
8.4 Calibration
8.4.1 C16-C18 (00.02.614)
Chromatogram
FID1 A, Front Signal (D191029D\S191206A 2019-12-06 17-04-20\B-021-201-00.02.614.D)
pA
12
11
10
9
C16:0
8
C18:0
7 C18:1
C18:2
6
C18:3
5
C18:1
26 28 30 32 34 36 38 min
FID2 B, Back Signal (D191029D\S191206A 2019-12-06 17-04-20\B-021-201-00.02.614.D)
pA
12
11
10
26 28 30 32 34 36 38 min
ChemStation report
Data File C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\B-021-201-00.02.614.D
Sample Name: 00.02.614
Trace Fame Avtur 12/10/2019 3:33:45 PM SYSTEM
=====================================================================
Acq. Operator : SYSTEM Seq. Line : 21
Sample Operator : SYSTEM
Acq. Instrument : Trace Fame Avtur Location : 201 (B)
Injection Date : 12/7/2019 11:10:21 AM Inj : 1
Inj Volume : 2.5 µl
Acq. Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M
Last changed : 12/2/2019 3:43:39 PM by SYSTEM
Analysis Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M (
Sequence Method)
Last changed : 12/10/2019 3:33:43 PM by SYSTEM
(modified after loading)
=====================================================================
External Standard Report
=====================================================================
Sorted By : Signal
Calib. Data Modified : 12/10/2019 1:23:34 PM
Multiplier : 1.0000
Dilution : 1.0000
Use Multiplier & Dilution Factor with ISTDs
1 Warnings or Errors :
=====================================================================
*** End of Report ***
=====================================================================
Acq. Operator : SYSTEM Seq. Line : 21
Sample Operator : SYSTEM
Acq. Instrument : Trace Fame Avtur Location : 201 (B)
Injection Date : 12/7/2019 11:10:21 AM Inj : 1
Inj Volume : 2.5 µl
Sequence File : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\S191206A.S
Acq. Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M
Last changed : 12/2/2019 3:43:39 PM by SYSTEM
Analysis Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M (
Sequence Method)
Last changed : 12/9/2019 2:08:27 PM by SYSTEM
=====================================================================
Column(s)
=====================================================================
Noise determination:
Noise determination:
=====================================================================
*** End of Report ***
25
20
0
15
14:
C
-
54
.2
10
41
8
.54
5
39
0
39 39.5 40 40.5 41 41.5 42 42.5 min
FID2 B, Back Signal (D191029D\S191206A 2019-12-06 17-04-20\B-033-201-00.02.614 C14.D)
pA
25
20
15
10
0
39 39.5 40 40.5 41 41.5 42 42.5 min
ChemStation report
Data File C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\B-033-201-00.02.614 C14.D
Sample Name: 00.02.614 C14
Trace Fame Avtur 12/10/2019 3:40:50 PM SYSTEM
=====================================================================
Acq. Operator : SYSTEM Seq. Line : 33
Sample Operator : SYSTEM
Acq. Instrument : Trace Fame Avtur Location : 201 (B)
Injection Date : 12/7/2019 10:11:19 PM Inj : 1
Inj Volume : 2.5 µl
Acq. Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C14.M
Last changed : 12/2/2019 3:46:08 PM by SYSTEM
Analysis Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C14.M
(Sequence
Method)
Last changed : 12/10/2019 3:40:26 PM by SYSTEM
(modified after loading)
=====================================================================
External Standard Report
=====================================================================
Sorted By : Signal
Calib. Data Modified : Monday, December 9, 2019 11:13:12 AM
Multiplier : 1.0000
Dilution : 1.0000
Use Multiplier & Dilution Factor with ISTDs
=====================================================================
*** End of Report ***
=====================================================================
Acq. Operator : SYSTEM Seq. Line : 33
Sample Operator : SYSTEM
Acq. Instrument : Trace Fame Avtur Location : 201 (B)
Injection Date : 12/7/2019 10:11:19 PM Inj : 1
Inj Volume : 2.5 µl
Acq. Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C14.M
Last changed : 12/2/2019 3:46:08 PM by SYSTEM
Analysis Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C14.M
(Sequence
Method)
Last changed : 12/9/2019 2:57:45 PM by SYSTEM
(modified after loading)
=====================================================================
Column(s)
=====================================================================
Noise determination:
Noise determination:
=====================================================================
*** End of Report ***
8.5 Validation
8.5.1 C16-C18 (00.02.616)
Chromatogram
FID1 A, Front Signal (D191029D\S191206A 2019-12-06 17-04-20\B-045-203-00.02.616.D)
pA
12
11
10
6
C18:1
C18:2
C16:0
C18:0
C18:3
4
26 28 30 32 34 36 38 min
FID2 B, Back Signal (D191029D\S191206A 2019-12-06 17-04-20\B-045-203-00.02.616.D)
pA
12
11
10
26 28 30 32 34 36 38 min
ChemStation report
Data File C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\B-045-203-00.02.616.D
Sample Name: 00.02.616
Trace Fame Avtur 12/10/2019 3:42:41 PM SYSTEM
=====================================================================
Acq. Operator : SYSTEM Seq. Line : 45
Sample Operator : SYSTEM
Acq. Instrument : Trace Fame Avtur Location : 203 (B)
Injection Date : 12/8/2019 9:55:02 AM Inj : 1
Inj Volume : 2.5 µl
Acq. Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M
Last changed : 12/2/2019 3:43:39 PM by SYSTEM
Analysis Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M (
Sequence Method)
Last changed : 12/10/2019 3:42:21 PM by SYSTEM
(modified after loading)
=====================================================================
External Standard Report
=====================================================================
Sorted By : Signal
Calib. Data Modified : 12/10/2019 1:23:34 PM
Multiplier : 1.0000
Dilution : 1.0000
Use Multiplier & Dilution Factor with ISTDs
1 Warnings or Errors :
=====================================================================
*** End of Report ***
C18:1
35
30
25
20
15
C18:2
C16:0
10
C18:3
C18:0
C18:1
C18:1
0
26 28 30 32 34 36 38 min
FID2 B, Back Signal (D191029D\S191206A 2019-12-06 17-04-20\B-053-204-00.02.617.D)
pA
35
30
25
20
15
10
0
26 28 30 32 34 36 38 min
ChemStation report
Data File C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\B-053-204-00.02.617.D
Sample Name: 00.02.617
Trace Fame Avtur 12/10/2019 3:45:26 PM SYSTEM
=====================================================================
Acq. Operator : SYSTEM Seq. Line : 53
Sample Operator : SYSTEM
Acq. Instrument : Trace Fame Avtur Location : 204 (B)
Injection Date : 12/8/2019 5:23:03 PM Inj : 1
Inj Volume : 2.5 µl
Acq. Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M
Last changed : 12/2/2019 3:43:39 PM by SYSTEM
Analysis Method : C:\Chem32\2\Data\D191029D\S191206A 2019-12-06 17-04-20\IP599 C16 C18.M (
Sequence Method)
Last changed : 12/10/2019 3:45:21 PM by SYSTEM
(modified after loading)
=====================================================================
External Standard Report
=====================================================================
Sorted By : Signal
Calib. Data Modified : 12/10/2019 1:23:34 PM
Multiplier : 1.0000
Dilution : 1.0000
Use Multiplier & Dilution Factor with ISTDs
=====================================================================
*** End of Report ***
Information
The information contained within these materials is subject to change without notice. PAC makes no warranties or
guarantees, either expressed or implied in these materials, including the warranty of merchantability or fitness for a
particular purpose. At any time, PAC may modify these materials, its instruments or its programs without notice and
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