Keit’s microFTS® FTIR Spectrometer

Bringing Power of FTIR Spectroscopy

to the Field and Factory

Slides 1-10, Presented at PEFTEC 2015 (18-19 November 2015), Antwerp, BelgiumKeit Ltd. ǀ www.keit.co.uk ǀ enquiries@keit.co.uk

Summary• Keit, spin-out from Rutherford Appleton Laboratory (RAL)

Space in Harwell, England• VC backed• Commercialising a rugged FTIR, originally designed for

space mission- small- light- rugged- low power (7W)

• The interferometer uses static optics and is thus inherently robust – this is not “ruggedized”, it is “born rugged”

• Targeting in-line process measurement (PAT)• microFTS® versus the Michelson – What’s the advantage?

Process FTIR overview• FTIR has grown in use for process analysis for various reasons

- very accurate, quantitative results- non-destructive- good for complex mixtures- fast (approx. 1 minute to result)

• But in production processes it is limited by- lack of robustness- calibration issues/creep- complications of ATEX compliance- problems and cost of fibre optic couplers

• In-process FTIR is seen as a fragile lab instrument dressed up to operate in the field, not as a rugged, reliable concentration-meter

Michelson and fragility

• The resulting ATEX-compliant FTIR is large and heavy

• Long fibre connectors are required which can also change spectral response during operation if moving

• Very expensive

Michelson schematicTo scale

• Precision moving mirror creates the interferogram

• Reliability and stability requires absolute repeatability and ruggedness of the mirror movement – very difficult to achieve

microFTS® - simple and rugged

• The resulting ATEX-compliant FTIR is small and requires minimal recalibration or maintenance

• Due to ruggedness, it is directly coupled to the reaction vessel or pipe - no fibre optics required

Keit schematicTo scale

• Interferogram is created by a patented arrangement of static mirrors and a VGA detector array

• No repeatability issues, no creep

Technology Advantages – RuggedNext slide to play video

Advantages

• Real-time readings

• Removes cost and delay of sampling

• Tolerant of thermal changes

• Can be directly attached to a vibrating test location

• Indoors or out

• No expensive (and breakable) IR fibre connectors

• Can be directly coupled to the plant control system

• Battery/solar power possibilities

microFTS® unique attributes address a wide range of field and factory applications

Pharma/Chemical Reaction Monitoring Food and drink quality control

Oil & Gas Product Measurement

Engine Monitoring Gas analytics

….and many more

Timeline2014 2015 June 2016 Sept 2016

• In-house testing and development

• IP67 rated• Suitable for non-FDA

regulated, non-ATEX monitoring

Proof of Principle

Beta Prototype

• In-house testing and development

• Academic research- 1 US, 2 UK

• Customer trials- 3 pharma- 2 chemical- more in discussion

Product #1

??

Now

• ATEX-rated• FDA compliant• Suitable for all

monitoring

Product #2(indicative image)

Sample Interfaces

• Sample interfaces include- ATR Dip probes (25mm o/d, 110 or 250mm long)- flow cells (ml to high volume)- transmission cells (cell gap 25 to 100 microns)

• Several ATR crystal materials are available

Material Hardness(Kgmm2)

pH range Cm-1 rangeRefractive

index

Diamond 7000 1-14 4000-30 2.4

ZnSe 137 6.5-9.5 5000-650 2.4

Germanium 550 1-14 5000-700 4.0

Chalcogenideglass

170 1-10 5000-840 2.5

Performance Data (Dec 2015)

Appendix

Ethanol in WaterEthanol in Water

0

5

10

15

0.08 0.1 0.12 0.14 0.16 0.18 0.2

Absorbance at 1043cm-1

(AU)

%w

/w E

tha

no

l

Data Value

R2 of linear regression 0.997

Limit of Detection (LoD) 0.1% w/w ethanol

Limit of Quantification (LoQ) 0.3% w/w ethanol*

* LoQ likely to approach LoD through use of non-linear modelling

Acetone in Water

Data Value

R2 of linear regression 0.999

Limit of Detection (LoD) 0.3% w/w acetone

Limit of Quantification (LoQ) 0.4% w/w acetone*

* LoQ likely to approach LoD through use of non-linear modelling

FTIR Spectra of Acetone in Water

0

0.1

0.2

0.3

0.4

0.5

80090010001100120013001400150016001700180019002000

Wavenumber (cm-1

)

Ab

so

rban

ce (

AU

)

0%w/w Acetone 0.39%w/w Acetone

0.78%w/w Acetone 1.17%w/w Acetone

1.56%w/w Acetone 1.94%w/w Acetone

2.32%w/w Acetone 2.69%w/w Acetone

3.07%w/w Acetone 3.44%w/w Acetone

3.8%w/w Acetone 4.53%w/w Acetone

5.25%w/w Acetone 5.95%w/w Acetone

6.65%w/w Acetone 7.33%w/w Acetone

10.61%w/w Acetone 13.66%w/w Acetone

Acetone in Water

0

5

10

15

0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08

Absorbance at 1369cm-1

vs 1296cm-1

(AU)

%w

/w A

ceto

ne

n-Butanol in Water

Data Value

R2 of linear regression 0.9825

Limit of Detection (LoD) 0.4% w/w acetone

Limit of Quantification (LoQ) 0.4% w/w acetone

FTIR Spectra of n-Butanol in Water

0

0.1

0.2

0.3

0.4

0.5

80090010001100120013001400150016001700180019002000

Wavenumber (cm-1

)

Ab

so

rban

ce (

AU

)

0%w/w n-Butanol 0.4%w/w n-Butanol

0.8%w/w n-Butanol 1.2%w/w n-Butanol

1.59%w/w n-Butanol 1.98%w/w n-Butanol

2.37%w/w n-Butanol 2.76%w/w n-Butanol

3.14%w/w n-Butanol 3.52%w/w n-Butanol

3.89%w/w n-Butanol 4.63%w/w n-Butanol

5.37%w/w n-Butanol 6.09%w/w n-Butanol

6.79%w/w n-Butanol

n-Butanol in Water

0

1

2

3

4

5

6

7

0 0.005 0.01 0.015 0.02 0.025

Absorbance at 1068cm-1

vs 1164cm-1

(AU)

%w

/w n

-Bu

tan

ol

Acetone in Toluene

Data Value

R2 of linear regression 0.997

Limit of Detection (LoD) 0.5% w/w acetone

Limit of Quantification (LoQ) 0.9% w/w acetone*

* LoQ likely to approach LoD through use of non-linear modelling

FTIR Spectra of Acetone in Toluene

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

80090010001100120013001400150016001700180019002000

Wavenumber (cm-1)

Ab

so

rban

ce (

AU

)

0%w/w Acetone 0.45%w/w Acetone

0.9%w/w Acetone 1.35%w/w Acetone

1.79%w/w Acetone 2.23%w/w Acetone

2.66%w/w Acetone 3.09%w/w Acetone

3.52%w/w Acetone 3.94%w/w Acetone

4.36%w/w Acetone 5.19%w/w Acetone

6%w/w Acetone 6.8%w/w Acetone

7.59%w/w Acetone 8.36%w/w Acetone

12.04%w/w Acetone 15.43%w/w Acetone

Acetone in Toluene

0

2

4

6

8

10

12

14

16

0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.16

Absorbance at 1719cm-1

(AU)

%w

/w A

ceto

ne

Paracetamol in Acetone

Data Value

R2 of linear regression 0.998

Limit of Detection (LoD) 0.2% w/w acetone

Limit of Quantification (LoQ) 0.2% w/w acetone

FTIR Spectra of Paracetamol in Acetone

0

0.2

0.4

0.6

80090010001100120013001400150016001700180019002000

Wavenumber (cm-1)

Ab

so

rban

ce (

AU

)

0%w/w Paracetamol

0.09%w/w Paracetamol

0.18%w/w Paracetamol

0.43%w/w Paracetamol

0.81%w/w Paracetamol

1.48%w/w Paracetamol

2.52%w/w Paracetamol

3.59%w/w Paracetamol

4.32%w/w Paracetamol

8.28%w/w Paracetamol

Paracetamol in Acetone

0

2

4

6

8

10

0 0.02 0.04 0.06 0.08 0.1

Absorbance at 1515cm-1

(AU)

%w

/w P

ara

ceta

mo

l

Keit’s microFTS® FTIR Spectrometer

Bringing Power of FTIR Spectroscopy

to the Field and Factory

Keit Ltd. ǀ www.keit.co.uk ǀ enquiries@keit.co.uk