trends and needs for on line micro analysis for r&d innoval: … · 2012-11-27 · 0.8505...
TRANSCRIPT
Renewable energies | Eco-friendly production | Innovative transport | Eco-efficient processes | Sustainable resources
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Trends and Needs for on Line Micro Analysis for R&D
INnovAL: Innovative Project for Micro Process
Analytical Technology
Dr. Franck BACO-ANTONIALI IFP Energies nouvelles BP3, 69360 Solaize, FRANCE [email protected]
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Agenda
Introduction
Trends and needs for R&D on line micro analysis
INNOVAL Project
Technologic platform AXEL'ONE : An collaborative platform
Conclusions and outlooks
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L’analyse des procédés: un enjeu pour l'industrie chimique
PRODUCTION
Products Quality
Safety of employees
and neighborhood
Environment protection (pollution)
R&D
Reduction of costs
Process intensification
ANALYSIS = PROCESS CONDITIONS CONTROLS
Objective
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Evolution of needs in term of analyzers in R&D
µ Pilots HTE Pilots Process Intensification
Reducing of sample volume
"Classical" analyzers
µ Analyzers
µCaptors
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• Employ more compact analyzers to be able to analyze in the heart of process "bring the analyzer to the sample" • Reduce time of experimentation - Increase the number of tests in the same time we need Smart analyzers to follow process stabilization, product quality, process control , ...
•Excellent repeatability, accurate systems, good accordance with
standard methods, ...
Needs for R&D and Process Intensification
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Next generation of analyzers: - compacts (micro analyzers, micro captors) - coupling with sampling microsystems - directly integrated in the process
>> Analysis at the closest of the reaction New Standard (SP76) NeSSI TM New Sampling and Sensor Initiative from CPAC
PROBLEMATIC
> Difficulties of direct implementation on industrial sites and R&D laboratories
- Unsatisfactory accordance between analyzers and industrials and R&D needs
- Some laboratories techniques are not always available for in situ application
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Needs
Need to employ more compact analyzers to be able to
analyze "in the heart of process"
Properties Molecular Properties Molecular
Analysis in liquids Analysis in gases Elementary analysis
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Elementary Analysis In situ analysis of elements in industrial liquids
traces of S, Ni & V in petroleum products traces analysis of contaminants in ex biomass and chemical products, ... traces analysis of contaminants in water following of corrosion (traces of metals) ...
Laser Induced Breakdown Spectroscopy
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Analysis in liquids - Properties
In situ analysis of elements in industrial liquids
in situ density, viscosity analysis of liquids with µsystems in situ refractive index analysis with µsystems particles analysis in liquid (solid, catalyst, macromolecules, ...) calculation of other properties using µspectrometers
Adaptation in function of specific needs Specific developments
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Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter Repeatability
Densité en ligne - Gazole
P=Patm, Qv = 2 ml/min
22
22.5
23
23.5
24
24.5
25
28/1/08 23:16 29/1/08 0:28 29/1/08 1:40 29/1/08 2:52 29/1/08 4:04 29/1/08 5:16 29/1/08 6:28 29/1/08 7:40
Time
Tem
pera
ture
(°C)
0.8435
0.8445
0.8455
0.8465
0.8475
0.8485
0.8495
0.8505
0.8515
dens
ity
(g/c
m3 )
T captor (°C)direct densityCorrected density at 15°C
Products
Numbers of measures
MV average g/cm3
St. Deviation g/cm3
Reapitability g/cm3
Gasoil
740
0,8509
1,96.10-5
5,49 10-5
Repeatability for diesel
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Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter Response to a periodic feed change
less than 30s – Flow 2ml/min
23
23.5
24
24.5
25
25.5
26
26.5
27
31/1/08 11:15 31/1/08 11:18 31/1/08 11:21 31/1/08 11:24 31/1/08 11:26 31/1/08 11:29 31/1/08 11:32 31/1/08 11:35 31/1/08 11:38 31/1/08 11:41
Time
Tem
pera
ture
(°C)
0.8405
0.8415
0.8425
0.8435
0.8445
0.8455
0.8465
0.8475
0.8485
0.8495
0.8505
dens
ity
(g/c
m3 )
T captor (°C)
Raw density
Corrected density
Gasoil A Gasoil A Gasoil A
Gasoil B Gasoil B
difference (A-B) 0.0006 g/cm3
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Analysis in liquids - Properties Example of In situ density with Excalibur µdensimeter µpilot test : gasoline + dissolved gas
0.7105
0.7155
0.7205
0.7255
0.7305
0.7355
0.7405
0.7455
0.7505
3/9/08 0:00 5/9/08 0:00 7/9/08 0:00 9/9/08 0:00 11/9/08 0:00 13/9/08 0:00 15/9/08 0:00 17/9/08 0:00
Date & Hour
Den
sity
(g/
cm3)
15.00
25.00
35.00
45.00
55.00
65.00
75.00
Tem
pera
ture
(°C
)
Corrected density at 15°CLaboratory analysis 15°CTemperature Captor (°C)
Better results with on line analysis
Lost of gas phase
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In situ analysis in different industrial liquids
in situ analysis with µspectrometric methods (miniaturized systems), using in situ probes Development and performance optimization
in situ analysis of dissolved gases (traces) in hydrocarbons (H2, O2, ...)
optimization of liquid injection systems for on line GC analysis
in situ analysis of liquid by µGC (at the moment only used
for gas analysis) ...
Analysis in liquids- Molecular Analysis
min0 20 40 60 80 100
pA
10
15
20
25
30
35
40
45
FID1 A, (D:\DOCUMENTS AND SETTINGS\JACQUINE\BUREAU\ETUDE HPLIS\DATA\P20BARS\001F0101.D)
PIC
1
PIC
2
PIC
3
PIC
4
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In situ analysis in different industrial gases
in situ analysis with µspectrometric methods using in situ probes Development en optimization of performances
Optimization of Tunable Diode Laser for specific applications Optimization of sensors
Density, moisture, H2, ... Analysis in corrosive environments (HF, HCl, ...)
Analysis in gases - Properties and Molecular Analysis
TDL
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Analysis in gases - Properties Example of in situ density in gas phase in µPilot: total gas flow 1l/h
density 1200
0
200
400
600
800
1000
1200
1400
23/0413:12
23/0418:00
23/0422:48
24/0403:36
24/0408:24
24/0413:12
24/0418:00
24/0422:48
25/0403:36
25/0408:24
25/0413:12
25/0418:00
25/0422:48
26/0403:36
26/0408:24
26/0413:12
26/0418:00
26/0422:48
27/0403:36
27/0408:24
27/0413:12
27/0418:00
27/0422:48
28/0403:36
28/0408:24
28/0413:12
28/0418:00
28/0422:48
29/0403:36
29/0408:24
29/0413:12
29/0418:00
29/0422:48
30/0403:36
30/0408:24
30/0413:12
30/0418:00
Date & Hour
Den
sity
(g/m
3)
GC analysisDensity (g/m3) at 15°C
CPG analysis for calculate gas density
Put to atmospheric presure of gas/liquid pot duringliquid sampling
No flow - Pilot's problem
Start Pilot
We are able to follow the "real life" of process Better knowledge for R&D development
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How to answer to the needs for Micro Analysis?
Micro Analysis Needs Collaborative project
USERS Request - Validation
LABORATORIES Research
INSTRUMENTALISTS Development & Industrialization
INNovAL Project
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Targets: -Development of new in situ on line analyzers in accordance with industrial and R&D needs > On the cutting edge of technology -Optimization available technologies presents on the market -Development of new and innovating solutions
INNovAL Project (AXELERA) "L'Analyse en Ligne au cœur du procédé"
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5 Skids on NeSSI platforms (Astute, Intraflow) for development of on-line applications – Evaluation in real conditions (P, T, ...)
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INNovAL – Main Actors
USERS Request - Validation
LABORATORIES Research
INSTRUMENTALISTS Development & Industrialization
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First innovative collaborative technological platforms in Lyon
INDEED (2013)
INNovAL – A structuring project
USERS Request - Validation
LABORATORIES Research
INSTRUMENTALISTS Development & Industrialization
INNovAL INDEED
Specific platform for industrial analysis in INDEED
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INDEED An innovative collaborative platform
Clean processes
UPSTREAM Factory of the futur
PROCESS ECO-DESIGN & ECO-
EFFICIENCY Technological
development, steering, diversification of raw
materials, demonstrations, training
TEST BENCHES Pilots, On line analysis, technological development
MODELING Simulation,
process control
INNovAL
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Conclusion & outlooks In R&D we need µanalyzers to intensify and optimize research
productivity and results quality Increase the links between industrials, academic laboratories and
instrumentalists to develop new analytical solutions in accordance with real industrial needs
INNOVAL project
Need to employ an innovative collaborative platform in order to develop & evaluate analytical instruments : pre industrialization before implementation on site
Platform Industrial Analysis in INDEED
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Lyon : Center of Excellence for "Industrial Analysis" in INDEED
Academics laboratories in UCBL Laboratories in CNRS/SCA Ecole des Mînes de St. Etienne
in all laboratories : teams, evaluation benches analyzers, ....
In INDEED platform laboratories for industrial experimentations, pilots, ...
Industrial users (Industrial partners : INnovAL, others)
Project of training in UCBL (Master) specialized in "Industrial
Analysis"
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Lyon : Center of Excellence for "Industrial Analysis" in INDEED Reseach laboratories – Industrial laboratories - Training
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Thank you
Dr. Franck BACO-ANTONIALI IFP Energies nouvelles BP3, 69360 Solaize, FRANCE [email protected]