Poster PresentationPittcon 2016, Atlanta, GA

From Mars to Mission Critical Process Control

Dan Wood ǀ www.keit.co.uk ǀ enquiries@keit.co.uk

Calibration and Long-Term Stability of a Rugged FTIR Spectrometer

Keit Poster - Pittcon 2016: Page 2

Background & Industry ChallengeFourier Transform Infrared (FTIR) spectroscopy is a powerful analytical tool. It can help manufacturing industries understand the chemistry of their reactions early on in the development process. However, standard FTIR analytical instruments are highly sensitive to vibration —making it a challenge to use in a production environment.

In addition, some chemical processes can only be controlled if the reaction state is known in real time. Key parts of reactions may remain unknown and uncontrolled. This frequently leads to poor quality and waste.

Objective Keit Spectrometers set out to prove that improvements to a novel optical design in an FTIR spectrometer based on the Sagnac model, originally developed for use on a satellite mission to Mars, can be successfully applied for use in manufacturing industries.

Figure 1, Sagnac: Interior layout of the

microFTS®, an FTIR spectrometer based on the Sagnac spectroscopy model. The novel optical design eliminates moving parts making the instrument highly vibration tolerant, eliminates the need for fibre optic cables and reduces need for frequent calibration.

Figure 2, Michelson: Interior layout of an industry standard FTIR spectrometer based on the Michelson spectroscopy model. This design requires the use of a moving arm making the instrument prone to vibration, requiring use of fibre optic cables and frequent calibration.

© HL Studios

© HL Studios

Keit Poster - Pittcon 2016: Page 3

Agri-Chemical Test Case StudyMajor agri-chemical provider stated experiencing up to 20% waste of production batches because they were unable to monitor real-time reactions with standard FTIR spectrometers that could not handle the vibration or the ambient conditions of the outdoor production environment.

SolutionKeit provided a mciroFTS® FTIR spectrometer that could monitor the process at a key stage of the reaction. The agri-chemical company tested the microFTS®’s suitability for measuring the progress of a production reaction involving a mixture of Acetonitrile (ACN), Tri-

ethylamine (TEA) and Heptane. Samples were run over a 2½ month

period (Nov 2015-Jan 2016).Positive study results included equivalent calibration models to existing bench-top FTIR and far greater long-term repeatability (See Figures 3 - 6).

Keit Poster - Pittcon 2016: Page 4

Built Rugged & Shock ResistantKeit’s dependable microFTS® spectrometer excels in the production environment. As the microFTS® was originally developed for use in satellites, the Sagnac-based design makes it inherently compact, rugged and able to take on the stresses of space flight. Keit is proving that innovative technology can be applied in other industries.

Keit Spectrometer’s goal is to help people make decisions on the production floor through better process monitoring technology — for better yields and process optimization in the pharmaceutical, chemical, oil & gas, and food & beverage manufacturing businesses. The microFTS® can help improve quality, reduce waste and improve facility utilisation using a more robust and stable instrument.

Better Process Monitoring and ControlKeit’s FTIR spectrometer, the microFTS®, is connected directly to production equipment to provide in-line process monitoring and eliminates the need for remote sampling or fibre optic cables. Keit cN help chemical engineering and production managers tell what is going right in their production process at the time of the reaction.

Keit’s microFTS®, a shock-resistant FTIR spectrometer

Keit Poster - Pittcon 2016: Page 5

RESULTS

Calibration ModelsCalibration curves developed for the 3 components had correlation of R2 = 99.94, 99.78 and 99.61 over the full range of concentration, thereby out-performing the reference spectrometer.

Figure 3: Keit’s microFTS® FTIR spectrometer. Calibration curve TEA (%).

Figure 4: Keit’s microFTS® FTIR spectrometer. Calibration curve ACN (%).

Figure 5: Keit’s microFTS® FTIR spectrometer. Calibration curve Heptane (%).

Keit Poster - Pittcon 2016: Page 6

RESULTS (Con’t)

RepeatabilityA further test was carried out to determine the repeatability of the spectra over time. The same spectrum was recorded on 17th November 2015 and then re-taken on each day between the 25th and 29th January 2016. When overlaid, the spectra were indistinguishable. The spectrometer had been moved around the lab between measurements and showed no signal drift over this 2½ month period.

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Figure 6: Keit’s microFTS® FTIR spectrometer. 5 overlay spectra run over 2½ months demonstrating repeatability.

Rugged FTIR SpectrometerFor the Production

Environment

www.keit.co.uk ǀ enquiries@keit.co.uk