Rugged FTIR to study bio-renewable (fermentation) processes

Authors: Dr. Jonathon Speed & Mr. Dan Wood

Poster Presentation: IFPAC 2017

28 Feb 28 – 02 March 2017N. Bethesda, Maryland, USA

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Rugged FTIR to study bio-renewable (fermentation) processesAuthors: Jonathon Speed, Dan WoodKeit Ltd., R71, Rutherford Appleton Laboratory, Harwell Campus, Didcot, OX11 0QXEmail: jonathon.speed@keit.co.uk

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Process Analytics for Bio-renewablesBio-renewables processes (such as fermentation) are often analysed usingoff-line techniques such as HPLC coupled with a suitable detector. This canresult in substantial delays in reporting, and in some cases can result inmissed opportunities to fix failed batches.

A simple fermentation processThis fermentation involves the consumption of a feedstock, which producesone of two intermediates and finally one of three products.

Feedstock

Intermediate 1

Intermediate 2

Key Product By-product

Secondary Product

Data acquisition and model buildingSpectra were acquired every 2 min for several days during the fermentation.Separately samples were removed for HPLC measurements. A PLS (partialleast squares) model was built using the spectra and HPLC data as inputs.

PredictionsEvery spectrum gathered during the fermentation (approximately 1600) was fedthrough the model and a prediction made on the feedstock, intermediates, andkey, secondary and by-products. These results were compared to the HPLCdata, with the results shown below.

The concentration profiles from prediction are in good agreementwith the HPLC reference data. It should also be noted that theconcentrations of the constituents range from 0.1 to 40 g L-1.

ConclusionThe Keit IRmadillo spectrometer can is capable of monitoring anindustrial fermentation process and by combining with chemometricscan accurately predict the concentration of various reactionconstituents over a wide range of concentration.

AbstractAn industrial fermentation process is monitored using a novel vibration resistant FTIR spectrometer. Spectra are gathered through the fermentation process and correlated to HPLC reference data using partial least squaresmethodology.

IntroductionBio-renewables and biotechnology are rapidly developing areas, and industrialfermentations can be 1,000,000 L in volume. It is imperative that theseprocesses can be properly controlled, and process analytical technology is a keypart of this. Industrial settings contain many hazards not present in the lab:vibrating reactors, vehicles, and in some cases extreme temperature changesand poor weather. Here we present a spectrometer that can withstand vibrationand is inherently rugged – perfect for an industrial setting.

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Food and drink

Suitable industries for FTIR monitored

fermentation

PharmaceuticalsRenewable fuels

Sagnac interferometers have no movingparts, making them highly resistant tovibration. Recent developments in detectortechnology coupled with development work atKeit, mean that the use of Sagnacinterferometry is no longer purely academicand can be extended to industrial settings.

This means that IRmadillo is inherentlyvibration resistant and there is also no needfor frequent baseline scans as there is almostno change inside the spectrometer withrespect to time or operating environment.

Sample

Infrared source

(emitter)

Beam splitter

Detector array

Curved mirror

Curved mirror

Michelson interferometers use amoving mirror to create a differencein path length of the light. The movingmirror needs to move smoothly inorder to provide reliable data. Thismakes the instrument extremelysensitive to vibration.

The common solution to this involvesusing a fibre optic probe to place theinstrument far away from theprocess. Unfortunately these are alsoaffected by vibration, and aresufficiently robust for industrialprocesses.

Sample

Detector

Fixed mirror

Beam splitter Moving

mirror

Infrared source

(emitter)

Conventional FTIRMichelson Interferometer

IRmadilloTM FTIRSagnac Interferometer

The techniques demonstrated in this work are directly applicable tothe industries shown above. From monitoring the production ofethanol in commercial brewing through to the production of APIs inbiosynthesis of drug molecules.

The combination of robust, rugged FTIR with chemometrics enablesreal time monitoring of a variety of industrial processes, improvingproductivity and reducing waste and cost.

Rugged FTIR SpectrometerFor Manufacturing Environments

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