Prepare and Analyze a Plant Extract by GC

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   |image      = PolymerTwinGC.png
   |image      = PolymerTwinGC.png
   |type        = Sample Prep and Inject
   |type        = Sample Prep and Inject
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   |id          = Polymers1001
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   |id          = Plant1001
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   |description = Polymer Analysis
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   |description = Analyzing a Plant Extract
}}
}}
=== Overview ===
=== Overview ===
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Chemical analysis of polymers, as well as other forms of analysis such as viscosity and other tests are a necessary part of polymer development, as well as QC processes during manufacture.  Polymers are generally solids when in the final product, and thus are not amenable to such analysis unless they can be first liquefied. Preparation for analysis requires multiple stages of treatment frequently with heated reaction and cooling steps prior to introduction into a detector such as a GC.  Such processes are lengthy, time-critical and labor intensive to perform manually. They frequently involve handling of caustic or toxic reagents. There is a strong case therefore, for automation of such processes.
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This GC Twin PAL application analyzes plant extract material. The application is to take a vial containing a plant material, add solvent, heat & agitator, filter, and then analyze on a 6890 GC.  This application may be applicable to any customer who wants to do filtration providing the liquid can be pushed thru the filter plate with a low pressure inert gas thru the headspace syringe.
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LEAP has broken new ground in one such application, where the complexities of this type of sample preparation have been fully automated using an HTX2H in the configuration shown below:
 
=== Significant Markets  ===
=== Significant Markets  ===
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* Polymer Manufactures
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Elements of this application can be applied to labs requiring any type of filtration of a sample while maximizing throughput.
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* Biodiesel Blenders
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'''What is a Plant Extract experiment?'''<br/>
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The sample prep procedure is quite simple with the exception of the final sample needing to not contain any of the plant material when it gets to the analysis procedure. The samples are incubated in a heated agitator, and then allowed to settle. The sample solvent, possible containing small pieces of plant material, is injected onto a 96 well filter plate in the top of a SPE drawer with a 19ga headspace syringe using the Combi PAL, the needle guide is locked, and then flushed (purged) with a stream of inert gas (e.g. Helium) forcing the solvent through the filter plate into the receiving plate below. The other PAL then makes the liquid injection from the receiving plate into the GC.
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* Polymer Distributors
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* Polymer End Users
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'''What is a Polymer experiment?'''<br/>
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The sample preparation process involves 2 heated reactions with cooldown steps in between. The first hydrolyses the solid polymer in a mixture with an internal standard at high temperature in Agitator 1. The pellets dissolve and after a quenching reaction and cooldown period, a derivitizing reagent is added followed by another heated incubation at lower temperature. The reactants are then injected onto a GC for analysis.
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A balance is used to check that a minimum weight of product is in the original vial. If not, the sample is skipped. The samples are barcoded at the time the sample list is set up. At runtime the scanned barcode is compared to the expected barcode and if there is a mis-match then the sample is also skipped. .
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LEAP Shell handles the sample scheduling of each of the 5 stages of the process, overlapping them all and filling up both agitators according to the available time between operations. It also handles barcode and weight validation as well as data logging.  
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'''LEAPS Approach'''<br/>
'''LEAPS Approach'''<br/>
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• Twin PAL control using a single sample list in LEAP Shell.<br/>
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The GC Twin PAL in combination with the cycle composer makes a very effective and flexible workstation. We were able to design and provide a solution which met the following challenges from the customer:<br/>  
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• Two heated zones for different temperature reactions.<br/>
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1. Provide the necessary filtration to have clean samples to analyze. In order to get good blow-out of the liquid through the filter, it was determined that the filter plate should be sealed and have a small nozzle on the underside to ensure accurate collection without crossover to adjacent collection vials.<br/>
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• Direct injection to either of two GCs.<br/>
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2. Throughput. By using a Twin PAL we are able to take advantage of having one PAL do the preparation while the other does the sample injections.<br/>
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• Balance integration for weighing of solid product and internal standard.<br/>
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3. Spatial concerns. Provide a way to get everything that was required to fit. <br/>
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• Up to 8 reactant vessels, and 32 sample vial capacity.<br/>
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• Overlapped staggered processing of all samples for high throughput.<br/>
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• Barcode checking, mismatched vials are not processed.<br/>
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• Weight checking, over or under weight vials are skipped.<br/>
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• Data reporting to log files.<br/>
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• GC failsafe mode – if GC goes down during a run, samples are still processed.<br/>
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• Integrated with Chemstation.<br/>
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<br/>
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'''Market potential:'''<br/>
 
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The success of this initial installation shows LEAP’s capability to solve complex automation challenges in areas which have previously been out of our reach. The polymer industry presents opportunities to expand these types of sales, not only for these complex sample preparation applications for solids, but for simpler applications such as viscosity testing or sample prep for NMR.<br/>
 
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In more general terms, this application illustrates the power of LEAP Shell and the new capabilities it provides which can be applied much more widely. Consideration should be given to the following opportunities:<br/>
 
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• Handling of single or multiple overlapped incubations e.g. Headspace or SPME.<br/>
 
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• Extensive customization of the Sample list.<br/>
 
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• Open access – walk-up addition of samples during a run.<br/>
 
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• Extensive use of the “IF” statement to manage error conditions and determine criteria for sample processing or not.<br/>
 
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• Output of data to log files for record keeping or for integration with data systems.<br/>
 
= Photos =
= Photos =

Revision as of 16:51, 9 February 2009

Plant Extract
Application Type
  Sample Prep and Inject
Application ID
  Plant1001
Description
  Analyzing a Plant Extract

Overview

This GC Twin PAL application analyzes plant extract material. The application is to take a vial containing a plant material, add solvent, heat & agitator, filter, and then analyze on a 6890 GC. This application may be applicable to any customer who wants to do filtration providing the liquid can be pushed thru the filter plate with a low pressure inert gas thru the headspace syringe.


Significant Markets

Elements of this application can be applied to labs requiring any type of filtration of a sample while maximizing throughput.

What is a Plant Extract experiment?
The sample prep procedure is quite simple with the exception of the final sample needing to not contain any of the plant material when it gets to the analysis procedure. The samples are incubated in a heated agitator, and then allowed to settle. The sample solvent, possible containing small pieces of plant material, is injected onto a 96 well filter plate in the top of a SPE drawer with a 19ga headspace syringe using the Combi PAL, the needle guide is locked, and then flushed (purged) with a stream of inert gas (e.g. Helium) forcing the solvent through the filter plate into the receiving plate below. The other PAL then makes the liquid injection from the receiving plate into the GC.

LEAPS Approach
The GC Twin PAL in combination with the cycle composer makes a very effective and flexible workstation. We were able to design and provide a solution which met the following challenges from the customer:
1. Provide the necessary filtration to have clean samples to analyze. In order to get good blow-out of the liquid through the filter, it was determined that the filter plate should be sealed and have a small nozzle on the underside to ensure accurate collection without crossover to adjacent collection vials.
2. Throughput. By using a Twin PAL we are able to take advantage of having one PAL do the preparation while the other does the sample injections.
3. Spatial concerns. Provide a way to get everything that was required to fit.


Photos

LEAP TWIN PAL for Polymers

Keywords: plant extract, sample prep, headspace syringe for liquid transfer, heating, shaking

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