Instruments for Monitoring Experimental Reactions

The study of the dynamic behavior of materials is complex, since it often requires several instrumental techniques to understand the physical and chemical processes. With complex and not understood systems, the concept of reproducibility is important. The number of parameters, controlled or not, is often too large. This means that several measurement instruments, including X-ray diffraction, will be set up around a single cell sample, to be followed in real time the evolution of structural modifications. The effects of changing various parameters (pressure, temperature, gas flow...) will then be directly recorded by all instruments.

Operando XRD-DRIFT : Catalyst characterization by Fischer-Tropsch process for clean fuel production
nCo + 2(n+1)H2 CnH(2n+2) +nH2O

INEL has designed a transmission mode diffractometer with a curved position sensitive detector associated to a DRIFT spectrometer. The system includes an environmental cell that allows X-ray and IR analysis at high pressure and high temperature.
Thanks to V. Moizan-Baslé, L. Braconnier, I. Clémençon, C. Legens, B. Rebours, L. Lemaitre, IFP-Lyon, BP 3, 69360 Solaize Cedex, France

XRD specifications
• Transmission mode with a Mo tube (lambda = 0,709 Å - E = 18 keV)
• Inel CPS120 curved detector, acquisition in real time over 120° 2
θ
• Focusing optic
• Debye-Scherrer geometry

DRIFT specifications
• IRcube OEM FT-IR spectrometer
• Set of parabolic and plane mirrors

 

Cell specifications

• Gaseous reactants flow through the reaction cell through a fix sample
• Heavy products collected in a condenser cooled at 15°C
• Operating conditions (T/P) : up to 600°C / up to 30 bars
• Specific windows for each experimental equipment

→  Connected to a gas chromatrograph for on-line analysis


Innovative system for the in situ investigation of hydrothermal reactions by X-ray diffraction


Specific instrumental device
• A purpose-built capillary reaction vessel which allows close emulation of the conditions present in mineral processing plants
• Transmission mode with the Mo K radiation, to ensure that the X-ray beam penetrates through the capillary
• An Inel CPS120 position-sensitive detector, to enable simultaneous collection of a wide range (120° 2
θ) of diffraction data


A : beam stop
B : sample holder (including the Swagelock settings to allow the application of gas pressure) and capillary reaction vessel
C : nozzle of the heater                                             
       Capillary mounted on a head goniometer
D : pressure line                                      
E : the incident-beam slit holder                                Heat zone : heating hot jet - T up to 750°C

                                                                                                     Pressure applied with a sweep gas
A close-up view of the sample configuration            (CO2, N2, H2, O2, Ar, etc.) - Up to 50 bars

Thanks to Ian C. Madsen,CSIRO Minerals, Box 312, Clayton South, Victoria, 3169, Australia

SAXS WAXS experiments combined with a Raman spectrometer for thermal studies


Proteins are essential components of all living organisms. Involved in many biological processes, they may be therapeutic targets and as potential drugs. One way to characterize them would be to develop innovative systems using Raman spectroscopy (or FTIR) coupled with X-ray scattering to study in situ the structure of proteins in solution (emulsion) or solid state (lyophilized powder) while having the ability to optimize the operating conditions (P, T, pH, ...).

Specific instrumental device :

• Transmission Mode with a Cu tube (lambda = 1,54 Å - E = 8 keV)
• An Inel CPS120 curved detector for WAXS measurement +
     a 2D detector or an Inel linear detector for SAXS measurement 
• In situ reaction with a heating hot jet or/and heating cold jet
 
Set up for combined SAXS / WAXS / Raman spectroscopy

Ask us to help you to configure a system as per your needs.

Download documentation

Please feel free to contact us and describe your project.

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Inel Inc, PO Box 147,
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T 001 603 778 9161 - F 001 603 778 9171