To NeSSi or Not to NeSSi: A Fast and Micro GC Experience Review

Transcription

1 Falcon Analytical makers of the... To NeSSi or Not to NeSSi: A Fast and Micro GC Experience Review IFPAC Annual Meeting January 26, 2016 Grand H NeSSi Arlington, VA (Washington DC), U.S.A 433 AEI Drive Lewisburg, WV

2 Abstract By now there is substantial experience using NeSSi systems with fast and micro gas chromatography. All are successful but some are more successful than others. On the surface, the modular fluid delivery sample systems are a perfect fit for fast and micro gas chromatography. However, just because one can use NeSSi doesn t necessarily mean one should use NeSSi in every case. Technical issues such as temperature, pressure and especially flow rate and even aesthetic issues must be considered carefully before plowing ahead. This presentation will review the current status of 3 installations and discuss the lessons learned. 433 AEI Drive Lewisburg, WV

3 What Is A Fast & Micro Gas Chromatograph? a GC having internal dimensions measured in microns not millimeters, retention times in seconds, not minutes and none of the limitations of silicon chip based GCs One tenth the size of conventional GCs 30 lbs vs 300 lbs One tenth the power of conventional GCs 300 watts vs 3000 watts Analysis times times faster than conventional GCs Fixed gases and Hydrocarbons up to C50 Using resistively heated steel capillary column modules eliminating air bath ovens 433 AEI Drive Lewisburg, WV

4 MUST have all the major attributes of conventional GCs Split/splitless injector with a variety of sampling options Manual syringes as well as syringe based autosamplers Fully automated gas & liquid sample valves Range of sample pretreatment options: traps, headspace, pyrolysis and Process sample systems for automated process analysis & control even NeSSI 433 AEI Drive Lewisburg, WV

5 MUST have all the major attributes of conventional GCs Programmed temperature and/or isothermal columns Up to 2 modules, each having 1 and up to 8 meters of stainless steel capillary GC columns Independently controlled from 5 o C above ambient to the limit of the column type or 400 o C whichever is lower Can include one column switching valve NO air bath oven! 433 AEI Drive Lewisburg, WV

6 MUST have all the major attributes of conventional GCs Detectors Thermal Conductivity Flame Ionization Flame Photometric Dielectric Barrier Discharge Electron Capture for halogens Photo Ionization for aromatics & olefins Helium Ionization for everything Even High Pressure Mass Spec Detector 433 AEI Drive Lewisburg, WV

7 AND has modern software and communications technology to match the analytical and automation requirements Sensor rich GC system & firmware Chromperfect Ethernet/PC based data system Application modules to fit Process analyzer HMI TC/PIP communications MODBUS via Ethernet BTU calculations Links to other Windows applications 433 AEI Drive Lewisburg, WV

8 AND has modern software and communications technology to match the analytical and automation requirements Simulated Distillation applications Infometrix chemometric applications LineUp for retention time alignment InStep for runtime chemometric models PCA PLS & other Pirouette apps 433 AEI Drive Lewisburg, WV

9 Falcon Calidus Intellectual Property Fast Micro Gas Chromatograph System US Patent Trans-Configurable Modular Chromatographic Assembly US Patent AEI Drive Lewisburg, WV

10 Modular Calidus GC Single Injections Models are made of modules Currently there are 7 Calidus models are available 101, single column & detector 201, dual serial columns, single detector 301, dual parallel columns & detectors CS, dual columns & detectors Heartcut Trap/bypass Backflush GS & GS-T for environmental MT for transportable fraud detection * * Dielectric Barrier Discharge Detector 433 AEI Drive Lewisburg, WV

11 Modules Make Instruments Instruments Make Analyzers Analyzers plus Sample Systems Make Solutions One Solution 433 AEI Drive Lewisburg, WV

12 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 AEI Drive Lewisburg, WV

13 FalconFAST Analytical Solutions and the Promise of NeSSi Easy to use: Sophisticated instrument/analyzer pairs employed with intelligence, agility and transparency to the user - thereby unifying the measurement results from the laboratory, at-line, on-line or in the field Laboratories Field Ultrafast gas chromatography instrumentation with applications technology designed to perform the job combined with NeSSI sampling, Advanced data processing and Enlightened interpretation Customers need and want the answers Not the hassles associated with analytical chemistry! Parker NeSSI Sampling Process Falcon Fast GC Loading Dock Infometrix Chemometrics Chromperfect Data System 433 AEI Drive Lewisburg, WV

14 Modularity Modularity Modularity Modularity from the analytical elements to the entirety of the system Calidus Process Enclosure NeSSI Modular Fluid Delivery Systems Even software Calidus firmware Chromperfect Engine Chromperfect Apps Pirouette Engine LineUp InStep Pirouette models From sample probe to the DCS connection modularity makes jobs easier 433 AEI Drive Lewisburg, WV

15 Just because one can use NeSSi doesn t necessarily mean one should use NeSSi. Sample systems STILL need the right fundamental engineering design must be done Temperature, pressure and flow rate Preconditioning for particulate or condensate or, or, or must be properly done Transport distance and mechanism Sample stability and materials in contact And all the others What follows are some examples in FalconFast experience. 433 AEI Drive Lewisburg, WV

16 The Right Stuff full scale plant system 3 Calidus Process Analyzers 3 Single Stream Parker Intraflow systems with autocal Chromperfect operational controls and data system & communications Infometrix retention time alignment for rock solid stability 3 process streams: dimer, trimer & tetramers of propylene 433 AEI Drive Lewisburg, WV

17 What about Stability? Single System Example at the End of the 1 st Quarter 101 seconds Q 1 Visit: part of last run showing 60 to 140 seconds 433 AEI Drive Lewisburg, WV

18 Single System Example at the End of the 1 st and 2 nd Quarter Overlaid 101 seconds Q 1 & 2 Visits Overlaid: part of last run showing 60 to 140 seconds 433 AEI Drive Lewisburg, WV

19 Single System Example at the End of the 1 st,2 nd and 3 rd Quarter Overlaid 101 seconds Q 1, 2 & 3 Visits Overlaid: part of last run showing 60 to 140 seconds 433 AEI Drive Lewisburg, WV

20 Single System Example after a Whole Year! End of the 1 st,2 nd,3 rd and 4 th Quarter Visits Overlaid 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 0.6 seconds for a WHOLE YEAR!!! 4 th chromatogram is after > 175,000 runs with ZERO downtime, no sample valve rotor nor column change nor detector maintenance ZIP Q 1, 2, 3 & 4 Visits Overlaid: part of last run showing 60 to 140 seconds 433 AEI Drive Lewisburg, WV

21 Works OK after rework Pilot plant operations The measurement goal: help find optimum processing conditions Somewhat reactive samples Analysis is for ppm level impurities in product Process development campaigns mean different compositions at different times The issues: Very small process volume Sample system rework to return analyzer loop to the process WITHOUT contamination (disturbing the process) 433 AEI Drive Lewisburg, WV

22 Works Just Fine but should it have been done? 8 Small Bioreactors Off gas analysis for the product concentration Indicates performance of the microbes and nutrient and air feed rate requirements Heat tracing absolutely required to get the C 10 product through the tubing to the sample system & GC sample valve 433 AEI Drive Lewisburg, WV

23 Why the Second Guessing? LOST ORDERS! Small reactors Probably should have used a rotary selector valve Small diameter tubing would have fit in a single heated bundle Biological culture not really in tune with our industrial culture It all works great BUT it isn t really a good fit in this lab Well they said they would ultimately put it on very large fermentors 433 AEI Drive Lewisburg, WV

24 The Next Big Thing not NeSSI Highly reactive monomer production Sample must be kept above 200 C or polymer fills the tubing and sets like concrete! Sample system components become a disposable item We will see how this works out soon 433 AEI Drive Lewisburg, WV

25 Have you been listening? No one asks Falcon to do C 1 /C 2 ratios. IFPAC 2016, NeSSi 433 AEI Drive Lewisburg, WV

26 Old School Propylene Purity Application Single Oven Ethylene purity would be very similar to this application. methanizer ppm MeOH ppm C0, C02 SBFV SBFV SEL SBFV SBFV FID TCD Ref. Low ppm H2 Mea. % C3H8 26

27 New School, Ethylene Purity Application CALIDUD CS, Dual Column, TCD & FID FID TCD Column 1 MXT-U-Bond Column 2 MXT-Molesieve 5A 27

28 All Leads to Data Equivalency 433 AEI Drive Lewisburg, WV

29 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 433 AEI Drive Lewisburg, WV