Ultrafast GC Performance in the Real World: Multi Lab Studies for Repeatability & Reproducibility

Transcription

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 1

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 2

3 For Absolute Certainty 1 run overlay 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? 3

4 What about Stability? Q 1 Visit: part of last run showing 6 to 14 seconds Retention time alignment by Infometrix LineUp implemented dimer, trimer & tetramers of olefinics 11 seconds 4

5 What about Stability? Q 1 & 2 Visits Overlaid: part of last run showing 6 to 14 seconds 11 seconds 5

6 What about Stability? Q 1, 2 & 3 Visits Overlaid: part of last run showing 6 to 14 seconds 11 seconds 6

7 What about Stability? Q 1, 2, 3 & 4 Visits Overlaid: part of last run showing 6 to 14 seconds Of course operating processes show compositional variance. However, the retention times don t! One year RT drift using Infometrix LineUP ZERO Peak to peak RAW (without LineUP) drift.6 seconds for a WHOLE YEAR!!! 4 th chromatogram is after > 175, runs with ZERO downtime, no sample valve rotor nor column change nor detector maintenance ZIP 7

8 Nice Repeatability Nice Stability but what about Reproducibility? ILS Duration 12/213-8/ 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 114 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 7,2 High Sulfur Diesel Flint Hills High Sulfur Diesel 9,24 Kerosene Marathon Petroleum Kerosene 1,22 1N Marathon Petroleum Marathon 1N-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 6 American Refining Kendrex 6 8

9 All 7 Lab Results Overlaid Samples 1 & 18 Ultra Low Sulfur Diesel Samples 2 & 16 Aviation Turbine Jet A Series1 Series2 Series3 Series4 Series5 Series6 Series7 Series8 Series9 Series1 Series11 Series12 Series13 Series14 Series6 Series7 Series8 Series9 Series1 9

10 All 7 Lab Results Overlaid Samples 3 & 11 Kensol 55-H Samples 4 & 23 FCCU Light Cycle Oil Series6 Series7 Series8 Series9 Series1 Series6 Series7 Series8 Series9 Series1 1

11 All 7 Lab Results Overlaid Samples 5 & 21 ASTM Reference Gas Oil 5 Samples 6 & 8 Light Cycle Oil Series6 Series7 Series8 Series9 Series1 Series6 Series7 Series8 Series9 Series1 11

12 All 7 Lab Results Overlaid Samples 7 & 2 High Sulfur Diesel Samples 9 & 24 Kerosene Series6 Series7 Series8 Series9 Series1 Series6 Series7 Series8 Series9 Series1 12

13 All 7 Lab Results Overlaid Samples 1 & 22 1N Marathon Petroleum Samples 12 &15 Kensol 61-H Series6 Series7 Series8 Series9 Series1 Series6 Series7 Series8 Series9 Series1 13

14 All 7 Lab Results Overlaid Samples 13 & 17 #2 Low Sulfur Diesel Samples 14 & 19 Kendrex 6 Series6 Series7 Series8 Series9 Series1 Series6 Series7 Series8 Series9 Series1 14

15 ASTM ILS 114 Statistical Analysis Summary Report now published on the ASTM website 7 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 114 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 7,2 High Sulfur Diesel Flint Hills High Sulfur Diesel 9,24 Kerosene Marathon Petroleum Kerosene 1,22 1N Marathon Petroleum Marathon 1N-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 6 American Refining Kendrex 6 15

16 Ultrafast Gas Chromatography Systems can be made statistically identical Modules Make Instruments Instruments Make Analyzers Analyzers Make System Solutions One Solution 16

17 Process Control Network Lab Instrument Network New Thinking CONVERGENCE! Old School Micro LAB GC Micro LAB Photometer Micro LAB Optical Spectrometer Micro LAB Mass Spectometer Transportable Packaging ERP Network Network Micro- PROCESS GC Micro- PROCESS Photometer Micro- PROCESS Optical Spectrometer Micro- PROCESS Mass Spectrometer At-Line Packaging Copyright Falcon Analytical

18 All Leads to Data Equivalency 18

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 19

20 Falcon Analytical makers of the... Thanks for your attention. Questions? 2