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FT-NIR and Process Optimisation November 2019 Dr. Mark Whatton Technical Projects Manager QuadraChem Laboratories Ltd [email protected]

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Page 1: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

FT-NIR and Process Optimisation

November 2019

Dr. Mark Whatton

Technical Projects Manager

QuadraChem Laboratories Ltd

[email protected]

Page 2: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Contents

Infrared Spectroscopy Overview

Process Optimisation Cases

•Butter / Spreads

•Dairy Liquids

FT-NIR

FT-NIR Hardware For Process Optimisation

Making Optimisation Work

Summary

Page 3: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Infrared

Page 4: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Infrared Spectroscopy

Carbon, Hydrogen, Nitrogen, Oxygen, etc. atoms bonded to form molecules

Molecule bonds absorb IR light

The amount of IR absorbed at different wavelengths is measured

The amount of IR absorbed equal to the amount of molecule present

The analyser calculates the composition of different components

Beer-Lambert Law

A = alc

Page 5: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Infrared Spectrum

In MID IR individual components can be observed in the spectrum absorbing infrared light in proportion to their concentration

Fat B 2850cm-1

Fat A 1750cm-1

Protein 1547cm-1

Lactose 1040cm-1

(water)

Page 6: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

MIR Spectrum Changes

Fat B C-H Fat A

C=O

Changing FAT Level The Fat A should be applied for milk products whereas Fat B is applied at measurement of individual cow samples or samples containing free fatty acids (FFA).

Page 7: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

NIR Spectrum Changes

It is possible to observe changes in NIR spectra relating to components in some cases

NIR systems use calibration models to calculate component properties

However overlapping bands and shifting peaks make this haphazard

Page 8: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Then Why Use NIR?

NIR Absorptions are “Forbidden”

• In theory they shouldn’t happen

In Reality “occasionally”

they do

• NIR Waves travel through matter until absorbed

NIR reflected back from

matter

• Missing absorbed NIR seen in spectrum

NO SPECTROSCOPIC

SAMPLE PREPARATION!

Page 9: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

FT-NIR

9

Wavelength Accuracy

Signal to

Noise

Long Term

Stability Water vapour !

Page 10: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Salt Analysis

Salt is a Crystalline solid and therefore does not absorb IR light

However Salt does dissolve, surrounding water molecules altering the H-O bond

This is seen as a very small water peak change, which with FT-NIR can be accurately quantified (+/- 0.05% Salt)

Page 11: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Factory Process Optimisation

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Different requirements for the applications in lab versus in factory

Accurate information presented to Operators in clear way that can be used to affect change

Factory has capability to tune process to achieve optimisation

Page 12: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Butter Process Optimisation

ROI – Butter Production - Moisture max 16%

Before Inline Optimisation Optimisation

Production Optimisation

Analyser Variation

Old Method +/- 0.6 More Accurate Method +/- 0.15

Page 13: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Milk Process Optimisation

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Raw Milk Cream

Skim

Cream

Semi Skim

Semi Skim >1.50% FAT

Illegal Excellent Real Poor

Page 14: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Process Optimisation

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Fast trim at start-up and after production stop

Production closer to target

Warning about production drift outside targets

Page 15: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

FT-NIR Hardware for Optimisation

• Factory Suitable – Vibration, Protection, etc.

• Food Safe

• CIP/SIP Compatible

• SCADA / OPC Integration

• Useful To Operators

• No Down Time

15

Diffuse Reflectance Sampling

Spoon Probe Sampling

Backscatter Sampling

Transmission Probe Sampling

Transmission Cell Sampling

Page 16: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Production Integration

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Page 17: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Factory Spectrometer

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Isolated from plant vibration

Page 18: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Factory Operator Terminal

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+ SCADA Integration

Page 19: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Achieving Optimisation with FT-NIR

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Useful Results

Calibration Support

Reference Analysis

Sampling Error

Process Understanding

Expectations

Page 20: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

In-Line Accuracy Potential

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Liquid WPC Butter & Spreads

Lab Analyser

Lab Analyser

Page 21: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Dairy Liquids and FT-NIR

• Starter Calibrations – FT-NIR Bench-top Platform –no

pumping system, no cell ware wear, no maintenance, no ongoing calibration

– Models directly transferred to In-Line System

– Rapid commissioning

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Page 22: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

Technical Support

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Maintaining Accuracy

Solving Problems

New Products

Changing Processes

Page 23: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

FT-NIR & Optimisation

Know the Problem

Expectations Fit For Purpose NIR Hardware

High Quality Reference Analysis

Technical Support

Factory Engagement

Page 24: FT-NIR and Process Optimisation - QCL · 2019. 11. 20. · Dairy Liquids and FT-NIR •Starter Calibrations –FT-NIR Bench-top Platform –no pumping system, no cell ware wear, no

For More Information

Riverside, Forest Row, East Sussex, RH18 5DW

01342 820 820

Twitter - @qclscientific

@

www.qclscientific.com

[email protected]