Fast GC Performance in the Real World: Multi Lab Studies for …s3-us-west-1.amazonaws.com/falconanalytical-net/uploads/... · 2016-07-18 · Title: Fast GC Performance in the Real

[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

mailto:[email protected]



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




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




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




What about Stability?Q 1 & 2 Visits Overlaid: part of last run showing 60 to 140 seconds

101 seconds




What about Stability?Q 1, 2 & 3 Visits Overlaid: part of last run showing 60 to 140 seconds

101 seconds




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!!!




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




All 7 Lab Results Overlaid

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Samples 1 & 18 Ultra Low Sulfur Diesel

Series1 Series2 Series3 Series4



Series13 Series14

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Samples 2 & 16 Aviation Turbine Jet A

Series1 Series2 Series3 Series4 Series5







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Samples 3 & 11 Kensol 55-H




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Samples 4 & 23 FCCU Light Cycle Oil








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600Samples 5 & 21 ASTM Reference Gas

Oil




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500Samples 6 & 8 Light Cycle Oil








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Samples 7 & 20 High Sulfur Diesel




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Samples 9 & 24 Kerosene








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Samples 10 & 22 100N Marathon Petroleum




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Samples 12 &15 Kensol 61-H








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Samples 13 & 17 #2 Low Sulfur Diesel




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Samples 14 & 19 Kendrex 060







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




Ultrafast Gas Chromatography Systems can be made statistically “identical”

Modules Make Instruments

Instruments Make AnalyzersAnalyzers Make System Solutions… One Solution




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!




All Leads to…

Data

Equivalency




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




Falcon Analytical makers of the . . .

Thanks for your attention.

Questions?


Documents

Fast GC Performance in the Real World: Multi Lab Studies for …s3-us-west-1.amazonaws.com/falconanalytical-net/uploads/... · 2016-07-18 · Title: Fast GC Performance in the Real