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[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 1
Falcon Analytical makers of the . . .
Ultrafast GC Performance in the Real World: Multi Lab Studies for
Repeatability & Reproducibility
John Crandall, President- Falcon Analytical
Steve Bostic, Marketing Consultant- Falcon Analytical
Ned Roques, Chief Chromatography Engineer – Falcon Analytical
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 2
Repeatability, Reproducibility, Precision, Accuracy… what about Stability?
•What do they really mean?
•At the end of the day… all are meant to
•Characterize analytical system performance
•Define a mode for comparison• Single instrument, single sample, many replicates
• Single instrument, many samples, many replicates
• Many instruments, single sample, many replicates
• Many instruments, many samples, many replicates
•HOW can we compare system to system performance?
Industry Group Round Robin Testing
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 3
For Absolute Certainty
• Comparisons are irrelevant without single system stability
• In gas chromatography RETENTION TIME repeatability
• And long term stability are absolute MUST HAVEs
• Area stability must also be achieved however• Calibrations can be automated
• Human intervention can be minimized
• But without retention time stability… it becomes very difficult to automate calibrations
•What retention time stability is achievable in the real world?
100 run overlay
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 4
What about Stability?Q 1 Visit: part of last run showing 60 to 140 seconds – Retention time alignment by Infometrix LineUp implemented – dimer, trimer & tetramers of olefinics
101 seconds
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 5
What about Stability?Q 1 & 2 Visits Overlaid: part of last run showing 60 to 140 seconds
101 seconds
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 6
What about Stability?Q 1, 2 & 3 Visits Overlaid: part of last run showing 60 to 140 seconds
101 seconds
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 7
What about Stability?Q 1, 2, 3 & 4 Visits Overlaid: part of last run showing 60 to 140 seconds
Of course operating processes show compositional variance. However, theretention times don’t!
4th chromatogram is after > 175,000 runs with ZERO downtime, no sample valve rotor nor column change nor detector maintenance…
ZIP
One year RT drift using
Infometrix LineUP… ZERO
Peak to peak RAW (without LineUP) drift 0.6 seconds for a WHOLE YEAR!!!
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 8
Nice Repeatability… Nice Stability…but what about Reproducibility?
• 12 Unique Samples• One well known reference gas oil
• 11 process fuel blend components or fuel products
• Each Lab Received 24 Samples• Duplicates of each sample type
• Scrambled in order with a simple number identification
• All 7 results performed by• Calidus ultrafast gas chromatograph
• Palarus Liquid Syringe Injection autosampler
• Chromperfect & Envantage Software
ASTM D7798 ILS 1014 PRECISION STUDY
Material ID Description Manufacturer
1,18 Ultra Low Sulfur Diesel Flint Hills Ultra Low Sulfur Diesel
2,16 Aviation Turbine Jet A Flint Hills Aviation Turbine Jet A
3, 11 Kensol 55-H American Refining Kensol 55-H
4,23 FCCU Light Cycle OilMarathon Petroleum FCCU Light Cycle Oil
5, 21 ASTM Reference Gas Oil SQS ASTM Reference Gas Oil
6,8 Light Cycle Oil Flint Hills Light Cycle Oil
7,20 High Sulfur Diesel Flint Hills High Sulfur Diesel
9,24 Kerosene Marathon Petroleum Kerosene
10,22 100N Marathon Petroleum Marathon 100N-Waxy Distillate
12,15 Kensol 61-H American Refining Kensol 61-H
13,17 #2 Low Sulfur Diesel American Refining #2 Low Sulfur
14,19 Kendrex 060 American Refining Kendrex 060
ILS Duration12/2013-8/2014
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 9
All 7 Lab Results Overlaid
0
100
200
300
400
500
Samples 1 & 18 Ultra Low Sulfur Diesel
Series1 Series2 Series3 Series4
Series5 Series6 Series7 Series8
Series9 Series10 Series11 Series12
Series13 Series14
0
50
100
150
200
250
300
350
Samples 2 & 16 Aviation Turbine Jet A
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 10
All 7 Lab Results Overlaid
0
100
200
300
400
500
Samples 3 & 11 Kensol 55-H
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
0
100
200
300
400
500
Samples 4 & 23 FCCU Light Cycle Oil
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 11
All 7 Lab Results Overlaid
0
200
400
600Samples 5 & 21 ASTM Reference Gas
Oil
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
0
100
200
300
400
500Samples 6 & 8 Light Cycle Oil
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 12
All 7 Lab Results Overlaid
0
100
200
300
400
500
Samples 7 & 20 High Sulfur Diesel
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
0
100
200
300
400
Samples 9 & 24 Kerosene
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 13
All 7 Lab Results Overlaid
0
200
400
600
Samples 10 & 22 100N Marathon Petroleum
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
0
100
200
300
400
Samples 12 &15 Kensol 61-H
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 14
All 7 Lab Results Overlaid
0
100
200
300
400
500
Samples 13 & 17 #2 Low Sulfur Diesel
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
0
100
200
300
400
500
Samples 14 & 19 Kendrex 060
Series1 Series2 Series3 Series4 Series5
Series6 Series7 Series8 Series9 Series10
Series11 Series12 Series13 Series14
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 15
ASTM ILS 1014 Statistical Analysis Summary Reportnow published on the ASTM website7 Labs, 7 Systems, 7 X 12 X 2 Samples
• The rigorous method for comparison of results, the ASTM ILS process demonstrates that using• Single instrument, single sample,
many replicates
• Single instrument, many samples, many replicates
• Many instruments, single sample, many replicates
• Many instruments, many samples, many replicates
• It is not just possible but demonstrated…
ASTM D7798 ILS 1014 PRECISION STUDY
Material ID Description Manufacturer
1,18 Ultra Low Sulfur Diesel Flint Hills Ultra Low Sulfur Diesel
2,16 Aviation Turbine Jet A Flint Hills Aviation Turbine Jet A
3, 11 Kensol 55-H American Refining Kensol 55-H
4,23 FCCU Light Cycle Oil Marathon Petroleum FCCU Light Cycle Oil
5, 21 ASTM Reference Gas Oil SQS ASTM Reference Gas Oil
6,8 Light Cycle Oil Flint Hills Light Cycle Oil
7,20 High Sulfur Diesel Flint Hills High Sulfur Diesel
9,24 Kerosene Marathon Petroleum Kerosene
10,22 100N Marathon Petroleum Marathon 100N-Waxy Distillate
12,15 Kensol 61-H American Refining Kensol 61-H
13,17 #2 Low Sulfur Diesel American Refining #2 Low Sulfur
14,19 Kendrex 060 American Refining Kendrex 060
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 16
Ultrafast Gas Chromatography Systems can be made statistically “identical”
Modules Make Instruments
Instruments Make AnalyzersAnalyzers Make System Solutions… One Solution
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 17
Network
Micro-PROCESS
Photometer
Micro LABMass
Spectometer
Micro LABOptical
Spectrometer
Micro LABPhotometer
Micro-PROCESS
GC
Micro-PROCESS
MassSpectrometer
Micro LABGC
At-LinePackaging
Pro
cess
Co
ntr
ol N
etw
ork
Lab
Inst
rum
en
t N
etw
ork
TransportablePackaging
Network
Micro-PROCESSOpticalSpectrometer
ERP
Copyright Falcon Analytical 2015
Old School
New Thinking…CONVERGENCE!
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 18
All Leads to…
Data
Equivalency
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 19
Industrial Implications (leaving you with food for thought)
Analytical Results Enable• Lab to Process equivalency
• Using same instrument, same method eliminates the variables with the exception of sampling
• Possibilities for online product certificates of analysis
• Plant to plant equivalency• Improves corporate product
consistency, quality and tighter process control
• Inter plant process trouble shooting• Work can now be focused on process
variances by elimination of analytical variances
System Modularity Enables
• Significant maintenance reductions• Substitute whole instruments as a
module, eliminating field repairs and costs
• Repairs/refurbishment in the lab or return to factory… like a premium car
• Packaging appropriate for the installation site• Purpose built for the application
• Deploy only what is needed for the job
• Potential for shelterless installations
• Lower costs• Capital costs
• Operational costs
• Long term maintenance costs
[email protected] Tel: (304) 647-5860Copyright Falcon Analytical 1/29/2015
433 AEI Drive – Lewisburg, WV 24901 20
Falcon Analytical makers of the . . .
Thanks for your attention.
Questions?