New Definition of Process Gas Chromatography

1. Expanding the Possibilities Micro-Technology in Process Gas Chromatography Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept New Definition of Process Gas Chromatography Torsten Maurer, Friedhelm Müller Karlsruhe, Germany

2. Classical Demandsfor a Process Chromatograph • Completely automated analysis cycle • Extreme long term stability of the analytical solution • Usable in hazardous areas • Ruggedness against environmental conditions • Networking capabilities • Integration into different Process Control Systems Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

3. New Demands More reliable information • Enhanced confidence level • Self-diagnosis • Built-in plausibility checkof the results • Validation strategies • Less expensive information • Minimized consumption of resources • Low consumption of gases and energy • No need for special trained staff • Low maintenance efforts • Remote maintenance • Module exchange instead of service Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept • More and faster information • Short cycle times • Requested by faster process modelling software • Or safety requirements (air monitoring) • Application of mathematical models for fast, ”fuzzy” information

4.  = 0.55 mmColumndiameter Theoretical plates / m HETP  = 0.45 mm  = 0.35 mm  = 0.25 mm  = 0.15 mm Gas flow m/s Fundamental components - Columns • Advantages of narrow-bore capillary columns: • tremendous separation power • inertness • wide variety of different columns from many sources • ability to be accomodated in small space Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept • Minor influence on resolution at increasing flow velocity !

5. Fundamental components - Live-InjectionPre injection Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept Sample slice from injection valve

6. Fundamental components - Live-InjectionInjection Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept Sample slice from injection valve Sample sliceto column

7. Fundamental components - Live-InjectionLoading loop Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept Advantages: • Narrow start peak width • Sample equilibrated to carrier gas pressure level (sample pressure independent) • Injection volume adjustable by time • Injection quality does no longer depend on valve quality • Tolerance against quality and even leakage of the sample valve

8. Fundamental components - Live-Injection Ideal geometry of the micromachined devicewill help to avoid split discrimination Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

9. - +Dp + Fundamental components - Live-Switching Straight Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

10. + -Dp - Fundamental components - Live-Switching Cut Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

11. + -Dp + Fundamental components - Live-Switching Backflush Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

12. Fundamental components - Micro EPC Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept Reproducibility of two pressure set points Pressure interval: 0,5 mbar Noise: < 0,2 mbar

13. 150 µm Fundamental components - Micro TCD Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

14. Micro machined analytical GC Systemcombining all functions Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

15. Micro machined analytical GC SystemAnalytical Module Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

16. Micro machined analytical GC SystemModule assembled to basic unit Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept

17. Laboratory GC Conventional Process GC Process-GC with Parallel Chromatography Approach Multi- and In-line detection Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detectio GC concept

18. Multi- and In-line detection Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detectio GC concept

19. Injection peak Area Width C5 / Det.4 Shape C5 / Det.2 C5 / Det.3 Multi- and In-line detection Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detectio GC concept C2 N2 C1 CO2 C3 C4 C6

20. Multiple detectors and in-line detectionAnalytical benefits • Conventional use at the end of the last analytical column • Monitor detector use. Already separated components can be backflushed or cutted-out. Allows faster definition of column switching times. • In-line detector use.Allows combination of very different separation principleswithin one analytical system, but no column switchingrequired to direct already separated components to acentral detector. Therefore reduced system complexity and reduced cycle times • Allows standard 100% normalisation in combination withcolumn switching • Allows partial substitution of temperature programming Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detectio GC concept

21. Multiple detectors and in-line detectionMaintenance benefits • Each singular column performance plus sample introduction performance can be monitored instead of system performance allows preventive maintenance • Permanent surveillance of the amount of injected sample • Better adjustment of column switching- all outlets completely controlled- remote adjustment (in combination with EPC)- even auto-adjustment possible • Internal leak test • Detector–to–detector signal comparison, plausibility check • ”Fast or precise” approach Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detectio GC concept

22. 200 s 20 s Adaptive calculationof peak areas Feedback • very precise • longer cycle time • lower accuracy • fast information Multi- and In-line detection Accuracy vs. fast results Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detectio GC concept

23. Conclusion • Miniaturizing in Process GC does not only mean smaller instruments. But opens new possibilities to improve the automated chromatographic analysis to a top level, not achieved up to now. • Multiple in-line-detection increases the quality and validity of results and decreases the time consumption dramatically ...... and together with • Valveless Live-techniques for injection and multi dimensional chromatography the need of maintenance and highly qualified personnel as a limiting factor is reduced. • All together provides new possibilities in remote operation and makes it possible to use a Process GC System as one distributed ”virtual” instrument with multi analytic functions. Classical Demands New Demands Columns Injection Column Switching Pressure Control Detection System Multi&in-line detection GC concept Torsten Maurer, Friedhelm Müller Karlsruhe, Germany