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, Belgium Keit Ltd. ǀ www.keit.co.uk ǀ [email protected]
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 [email protected]
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 [email protected]