use of a nir mini spectrometer for polyamides ...€¦ · raman spectroscopy very discriminant...
TRANSCRIPT
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Use of a NIR mini spectrometer for polyamides discrimination on a
production unit
LOCATION HelioSPIRNAME Perrine HebertDATE 2018/11/28
Hebert Perrine 1, Montagnier Safia 1, Guilment Jean 1Lallemand Jordane 2 et Roussel Sylvie 2
1 ARKEMA - CERDATO / Laboratoire d'Étude des Matériaux (LEM) - Route du Rilsan, 27470 Serquigny – France [email protected]
2 Ondalys - 4 rue Georges Besse, 34830 Clapiers, France - [email protected]
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WHO ARE WE ? WHAT ARE OUR NEEDS?
WHAT TECHNOLOGY CHOICE FOR OUR NEEDS ?
WHAT RESULTS DID WE OBTAIN ?
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WHO ARE WE ?
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ARKEMA TODAY
4 P. HEBERT
sales19,000 Worldwide
presence€7.7 bnemployeesworldwide
136 3 R&Dindustrial sites and innovation
geographical hubsin 50 countries
34%of sales
Europe59 production sites
10,400 employees
38%of sales
28%of sales
North America38 production sites
3,600 employees
Asia and rest of the world39 production sites
5,000 employees
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SERQUIGNY’S PLATFORM : A PLANT + A RESEARCH AND DEVELOPMENT CENTER
Manufacturing, research and development of high performance polymers● Long chain alliphatic Polyamides Rilsan, Rilsamid● High temperature Polyamides● Transparent Polyamides● Pebax
7 P. HEBERT
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WHAT ARE OUR NEEDS?
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WHAT ARE OUR NEEDS?
7 P. HEBERT
Operational excellence
Fast quantitative measurements
Discrimination between product bases
Improved Return On Investment
Avoiding errors
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WHAT TECHNOLOGY CHOICE FOR OURNEEDS ?
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WHAT TECHNOLOGY CHOICE FOR OUR NEEDS ?
Raman spectroscopy
● Very discriminant technology● Not applicable to the entire range of applications (fluorescence)● Miniaturization of instrumentation started● High cost
NIR spectroscopy
● Validated for most of the insdustrial applications on FT-NIR instrumentation (except black samples)● Reasonable cost for « big » applications● Miniaturization of instrumentation started at very low cost● Performances to be assessed
X-Ray Fluorescence
● Validated for the insdustrial applications on ED or WD laboratory instrumentation● Needs disminative elements● Reasonable cost for « big » applications● Allows to work on black samples● Miniaturization of instrumentation started● Medium cost● Performances to be assessed
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WHAT TECHNOLOGY CHOICE FOR OUR NEEDS ?
Min
iNIR
Sens
or • 2-5000€• Recent on the market• Technology : Fabry Pérot• Limited spectral range• Performances to be
assessed
FTN
IR
• 50 000€• Widely used in the industry• Technology : Fourrier Transform• Wide spectral range• Qualitative and quantitative
analysis
P. HEBERT11
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FABRY PEROT TECHNOLOGY
Wavelength range ● 1.35 – 1.65 μm (NIRONE1.7)● 1.55 – 1.95 μm (NIRONE2.0)● 1.75 – 2.15 μm (NIRONE2.2)● 1.95 – 2.45 μm (NIRONE2.5)Detector type Single element extended InGaAsWavelength points Minimum step 0.1 nm,up to 512 in totalSNR (typical, w/o averaging) > 10,000Size (W x L x H) 60 x 53 x 27 mm3
12 P. HEBERT
Wavelength resolution (FWHM)● 14 – 18 nm (NIRONE1.7)● 16 – 22 nm (NIRONE2.0)● 20 – 26 nm (NIRONE2.2)● Not availble (NIRONE2.5)Illumination source 2 tungsten vacuum lamps Bulb life > 40,000 hrsWavelength switching time 1 msWavelength temperature response (max.) 0.1 nm/°CWeight 90g
Fabry Perot Interferometer● 1 λ for one cavity length● Cavity length controlled with MEMS (Microelectromechanical systems)
SPECIFICATIONS VALUEs
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WHAT ARE YOURS NEEDS ?
Analysis time = Integration time * Number of Scans * Number of points
Parameters: Integration time = 0.1ms / step Number of points (Range (1550 – 1950 nm) / Step size (1, 2 or 10nm))
Goal: Analysis time around of 20 secondes
20%50%
100%
Analysis of the 100% line as a function of Lamp intensity
Analysis of the 100% line as a functionof lamp stabilization time
1st Day2nd Day3th Day
P. HEBERT18
Full range = 2.10-3
Green range ~ 10-5
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FTNIR VS SENSOR NIR
P. HEBERT13
0.97
0.98
0.99
1
1.01
1.02
1.03
1.04
1.05
1.06
1.07
0.4
0.6
0.8
1
1.2
1.4
1.6
800 1000 1200 1400 1600 1800 2000 2200 2400
Abso
rban
ce S
enso
rNIR
Abso
rban
ce F
TNIR
Wavelength in nm
Spectrum FTNIR vs sensor NIR
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RESOLUTION : FTNIR VS SENSOR NIR
20nm
19 P. HEBERT
NIR Sensor 1 nm stepsNIR Sensor 5 nm stepsFTNIR
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20 P. HEBERT
DERIVATION
2nd dérivative – Sensor NIR 1nm steps2nd dérivation – Sensor NIR 5nm stepsFTNIR
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WHAT RESULTS DO WE HAVE OBTAIN ?
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DISCRIMINATION BETWEEN PRODUCT BASES AND /OR QUANTIFICATION
Plasticized products● Separation of plasticized (PA11 P20, PA11 P40) versus not plasticized (PA11,
PA12)● Separation of plascized products as a function of the plasticizer level (PA11,
PA11 P20, PA11 P40)● Prediction of the amount of plasticizer
Nature of products● Separation of PA11 versus PA12 vs other polyamides
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PLS-DA
P. HEBERT15
PA11 P40 vs all
PA11 vs all
Other PA vs all
PA11 P20 vs all
PA12 vs all
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PLS ON THE PLASTICIZER CONTENT
P. HEBERT16
Quantitative analysis ispossible
PA11PA11 P20PA11 P40
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CONCLUSION
Mini NIR spectrometer allows to discriminate between our products
● Plasticized vs un plasticized Easy● PA11 vs PA12 more challenging
Mini NIR spectrometer allows to quantify plasticized content
● Obvious patern● Strong concentration variations (%)
Necessory to develop
● Sampling interface● Computer interface● Chemometric interface
20 P. HEBERT
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THANK YOU FOR YOUR ATTENTION