6th Annual micro & Fast Gas Chromatography Symposium

January 07, 2018

The Ever Expanding Application of Fast Chromatography and Hyphenated Chromatography

Gulf Coast Conference

Wednesday, January 17, 2018, 10:30 AM, Room 381-A

George R. Brown Convention Center, Houston, Texas, USA


The Ever Expanding Application of Fast Chromatography and Hyphenated Chromatography

10:30 - 10:40 AM

Moderated by Dr. Carl Rechsteiner - CRechsteiner Consulting

Recent Advances: An Overview of Fast GC, Sensitive GC and Even Simply Faster GC than the Traditional

10:40 AM - 11:00 AM

John Crandall - presenter, Ned Roques, Joe Perron, Matt Holliday, Derrick Saul, Ken Melda – Falcon Analytical

Fast gas chromatography has been deployed “from the winery to the refinery to the wellhead” as previously reported at GCC. The value of rapid response has been demonstrated in the lab, at-line, online and even by the roadside. However, recent applications expand the technology even more to include product purity at the 99.99% plus levels. Environmental applications using both direct injection and pre-concentration trapping have been used to achieve limits of detection downwards from the parts per million level to parts per billion and even parts per trillion. Also, demand for higher resolution capability have been met with longer column possibilities up to 16 meters for a total of 32 meters with two modules. This paper will be a visual overview of the expanded capabilities of fast GC since Gulf Coast Conference 2016.

Resolving the Conflict between Lab and Process Data

11:00 AM - 11:20 AM

Carl Rechsteiner – presenter - CRechsteiner Consulting

Joe Perron, Steve Bostic, Ned Roques - Falcon Analytical

The conflict between lab and process data has always existed because the process data doesn’t always match the lab data. The lab’s primary function is to validate and certify products and it is therefore the adjudicator should discrepancies in data arise. Consequently, if the two sources of information do not conform, the process side is required to make the necessary changes, corrections, and adjustments; hence the conflict.

This paper explores data results for petroleum fraction samples ranging up to C44 or 535 ºC end boiling point on a lab and a process gas chromatograph (GC) wherein the same hardware and methods were used. The two GC’s differ only in their sample introduction method. The paper will discuss the operational parameters and the differences in results from liquid syringe autosampler based inlets used in laboratories to rotary valve based inlets required in the process all leading to a fluid free calibration of the process GC.

Recent Advances for Chromatography Data Systems in Fast GC: Control, Data Fusion, Automation

11:20 AM - 11:40 AM

George Schreiner – Chromperfect (Justice Laboratory Software, Inc.)

Modern gas chromatography continues to advance not only from speed and the need for higher data rates but also to the use of more and new detectors. Integration of analog and digital data from outside sources, sometimes called data fusion is also required. And there is an ever increasing desire to automate operations, system suitability and even automated assessment of results. The suite of software including Chromperfect the basic chromatography data system, Chromperfect Process Control the process GC automation and human/machine interface system and the Chromperfect Marker Trace application and of course communications to process control systems exemplifies response to these new market requirements. Use of these tools and their interaction with other data and programs like Infometrix LineUp and InStep make the applications possible in the hands of the intended end users.

True Plug-and-Play Chromatography

11:40 - 12:00 PM

Brian Rohrback - presenter and Scott Ramos - Infometrix, Inc.

In applications like simulated distillation, multiple instruments can run the same method but slight differences in column and flow conditions make chromatograms not match the time axis from instrument to instrument. Normally, this would require separate calibrations or even slightly separate methods for each instrument. With chemometric alignment, these minor variations can be compensated for and identical methods be used, potentially even skipping the calibration step. The idea is very powerful: that a small amount of software can be added to a chromatograph and have that addition open a true Plug-and-Play capability for the instrument/application. Ostensibly, a company could keep a cold spare chromatograph in inventory. When a process or lab unit goes down for any reason, the storage unit would be placed on-line and have its data be completely comparable to all previous runs on its very first injection without ever running a calibration step. Alignment can also apply this procedure to the historical chromatographic data assembly, giving a consistent database ready to be mined. Of course, this conclusion holds for situations where the column and the method conditions are very similar. But if this is the case, it may be possible to think of a chromatograph with the same supply and repair mindset more often reserved for temperature and flow sensors.


Roadside Ultrafast GC Analysis of Chemical Markers for Fuel Fraud Enforcement Campaign in the UK and Ireland

1:00 - 1:20 PM

Jeremy Reyes, presenter, Bill Winniford, Molly Price, Analytical Sciences, The Dow Chemical Company, Freeport, TX

Brian Jazdzewski, Warren Smith, Zahid Asif, Nathan Wilmot, Dow Industrial Solutions, The Dow Chemical Company, Freeport, TX

John Crandall, Ned Roques, Joe Perron, Matt Holliday, Falcon Analytical

ACCUTRACE™ fuel marking technology is entering its second year of use in the UK and Ireland. The award-winning system, including the ACCUTRACE™ S10 marker and the CALIDUS™ MT roadside detector, has “virtually eliminated fuel laundering” in the UK according to the UK press. It is also reported that as much as $1 billion in road use taxes have been collected due to the deterrent provided by the marking and detection systems. At low parts per million treat rates, this marker technology is highly cost-effective and is resistant to laundering methods practiced by criminals to launder low taxation fuels intended for farming, fishing, domestic heating, and construction.

The ultrafast CALIDUS™ gas chromatograph (GC) is utilized as a roadside analyzer and offers advantages in speed, sensitivity and transportability. Configured with two column modules, a heartcut valve, and dual FID detectors, separation via 2D GC delivers detectability down to low parts per billion (ppb). In the UK and Ireland, this marker and detection technology led to a reduction in laundering plants discovered, a decline in illegal use of subsidized fuels, and a drop in waste products associated with fuel laundering. In summary, this work will show the instrument performance and capability for analyzing ppb concentrations of chemical markers in fuel using a transportable, fast GC.

Identifying Authentic and Fraudulent Diesel Fuel by Fast GC Using Chemometrics

1:20 - 1:40 PM

Brian Rohrback - presenter - Infometrix, Inc.

Joe Perron – Falcon Analytical

Fraudulent use of off-road fuel can take many forms and is becoming a global problem. One way of avoiding road use tax is laundering markers from off-road diesel as just reported. A more subtle one is adulteration of fuel and labeling it as something that is not fuel. For example, biodiesel levels can be used as a diluent or base oils added or even high boiling fatty acids have been detected. Before delivery to retail outlets, product certificates are switched to label the material as diesel. The economic impact is not only tax loss but over time these materials can have a very negative impact on the consumers’ engines.

This paper will show how ultrafast GC coupled with chemometric techniques are an effective roadside detection and deterrent system for this criminal activity. The GC, the software and the database functions will be discussed as an economically and technically viable fast roadside solution to end this kind of fraud.

Fast Gas Chromatography High Pressure Mass Spectrometry (GC-HPMS) Technique, Software and Applications

1:40 - 2:00 PM

Graham Shelver and James Roush - 908 Devices

As user demand for analytical chemistry instrumentation continues the march towards easier to operate and simpler to service devices, Fast GC-HPMS brings real world capability to a broad range of hydrocarbon processing applications. GC/MS no longer need be restricted to the domain of the expert users and pristine laboratory settings. Exciting application areas include crude characterization, BTEX, other aromatics and a number of other applications not previously considered possible with complicated, high power, high-vacuum based conventional GC/MS systems.

Optimizing the Interface between Supercritical Fluid Chromatography and Electrospray Ionization Mass Spectrometry

2:00 - 2:20 PM

Michael O. Fogwill, Principal Research Chemist, Separations Research, Waters Corporation

Supercritical fluid chromatography (SFC) employs a compressible carbon dioxide-based mobile phase. Since the solvating power of the SFC mobile phase is directly related to pressure, there is a dramatic difference in mobile phase properties from the point of sample introduction to the point of detection in a SFC system coupled with mass spectrometry (MS). In order to maintain excellent peak shape and maximize sensitivity, both instrument design and method development must be optimized to account for this change in mobile phase solvating power. When properly optimized, SFC-MS provides a very sensitive and robust interface with performance on par with liquid chromatography mass spectrometry. This presentation will outline optimization of the instrumentation and the tuning parameters for the SFC-MS interface. Troubleshooting techniques specific to SFC-MS will be discussed with application examples.

Fast Gas Chromatography using Heated Headspace Gas Autosampling Techniques: Polyethylene Pellets, Product Purity Analysis

2:20 - 2:40 PM

Derrick Saul - Falcon Analytical

Sampling is often the most difficult part of an analytical method even for micro and Fast Gas Chromatography. In some cases the analytes of interest cannot be separated and measured with a column system that can survive the balance of the sample matrix. Purity analysis of Polyethylene Pellets is an excellent example. The solution is to heat the pellets and drive the target analytes into the headspace gas. The autosampler using a gas tight syringe can then sample and introduce the resultant sample into the GC. This paper will describe the system and the methods developed for this analysis.